LGO Hydrotreating Unit Operating Manual
LGO Hydrotreating Unit Operating Manual
Operating Manual
LGO Hydrotreating unit Revision : R – 1
Date : 19/03/2020
(Unit 15) Page : 1 of 185
Operating Manual
LGO Hydrotreating unit
(Unit 15)
Chapter 5 Material and Heat Balances with Physical and Thermal Properties of the Streams
The hydrotreater is designed to process 17,000 BPSD (112.7m3/hr) of light gas oil from
the crude unit 11. ( currently the unit is running above design capacity by 10% more after
simulation calculations confirmed equipment capability).
Light gas oil feed properties are shown on Table 1. Hydrogen makeup properties are also
shown on Table 1. Hydrogen makeup will normally be supplied from the Naphtha
Hydrotreater Unit 12.
The hydrotreater will process LGO from the crude unit during crude runs on blends
ranging from 50/50 to 80/20 Dukham D/Dukham C respectively. For design, the gas oil
feed volume is the same for both cases.
The hydrotreater is designed for start of run (SOR) and end of run (EOR) modes of
operation charging gas oil from the 50/50 blend crude. All equipment designed for this
case will be capable of processing 80/20 blend gas oil.
Operating conditions are shown in the Haldor Topsoe Basis for Design, Hydrotreating
Unit 15.
Onstream factor is 90% (330 days per year). All equipment has been specified to enable
operation at 50% of normal flow.
TABLE 1
Makeup Gas
Feed
Vol. Percent
Case 50/50 80/20 50/50 80/20
Feed Rate, BPSD 17000 17000 H2O 0 0.27
Feed Rate, Std M3/H 112.6 112.6 H2S 0.53 0.19
H2 82 84.65
Std Process(SG) 0.857 0.853 C1 5.3 3.32
Cetane Index (from Assay) 50.8 57.7 C2 5.12 3.85
Sulphur, WT% 1.2 1.05 C3 4.4 3.99
Nitrogen, WT PPM 28 30 IC4 0.64 0.61
Aromatics, Liq Vol% NC4 1.35 1.73
Mono-Aromatics Note (1) 16.5 13.5 IC5 0.32 0.39
Di-Aromatics Note (1) 6.5 5.5 NC5 0.34 0.51
Tri-Aromatics Note (1) 4.5 3.5 C6+ 0 0.49
TOTAL 27.5 22.5 TOTAL 100 100
VISC. CST @ 50C 2.5 2.5
ASTM D-86 C Vol %
1 182 184
5 234 235
10 247 247
30 266 262
50 277 279
70 309 304
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90 330 335
95 343 344
EP 350 349
Note (1) The aromatics analysis has been estimated by Haldor-Topsoe from typical laboratory data.
It has not been derived by Parsons from the Assay.
TABLE 2
Distillation deg. C
IBP 147 133 170 168
10% 239 232 242 236
30% 260 254 257 252
50% 274 269 274 268
70% 304 300 299 293
90% 330 325 329 324
FBP 347 340 349 344
Note: 1. 50/50 case properties calculated from Pro2 simulation, except sulphur and
nitrogen data from Haldor Topsoe. 80/20 case properties from Haldor
Topsoe except flash point estimated.
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TABLE 3
TABLE 4
Note: For the detail of the battery limit conditions, refer to the attached sheet No.1.
The principal desulfurization catalyst for this unit is 1.3 mm three-lobed TK-554. This
catalyst will be sock loaded in both reactors. In addition,a graded bed system is utilized
at the top of the new reactor’s first bed to provide protection against fouling. The graded
bed system incorporates a 150 mm topping layer of high void inert 16 x 11 mm tableted
TK-10, a 300 mm layer of 5 mm ring shaped TK-550 catalyst and a 300 mm layer of 3
mm ring shaped TK-550. The high void inert 16 x 11 mm tableted TK-10 is also used
for a 150 mm topping layer on the catalyst bed in the existing reactor.
The following presents the overall catalyst requirements for this unit:
Each of the catalyst beds of The TK-554 is supported by a system of inert designed to
provide a stable support with minimum pressure drop. Most of the bottom head of
each reactor is filled with 19 mm inerts. That is topped with a 75 mm layer of 6 mm
inerts and a 3 mm inerts. The minimum distance from the top of the outlet cover at
the bottom of the reactor to the bottom of the 6 mm inert layer is 150 mm. The catalyst
can be loaded into the head as long as the cross sectional area of the catalyst is not less
than 80 percent of the shell cross sectional area.
Provide 11,600 kilograms of Dimethyl Disulfide for use as a catalyst sulfiding agent
during start-up.
The quantity of sulfiding agent specified represents an amount sufficient for the initial
start-up sulfiding operation. An equivalent amount should be ordered prior to the
process unit shutdown for catalyst regeneration or catalyst change out.
Caustics
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Provide 266,000 kilograms of 15 oBe caustic to neutralize reactor effluent gases for
the regeneration of the catalyst.
Provide 3,500 kilograms of soda ash (Na2CO3) with 500 ppm by weight maximum
chloride content, and 350 kilograms of sodium nitrate (NaNO3).
Corrosion Inhibitor
TABLE 5
Catalysts
Consumption
Initial Life
Cont.
Filling Time 3
Service Type per year /Batc Remarks
months
h
[m3] [years] [m3] [m3]
Catalyst 1)
1.8 - - Batch Sock loading
TK-10 Inert
(1501D & 1551D)
16x11mm tablet
Catalyst 1)
TK-550 3/16”&1/8” 4.24 - - Batch Sock loading
(1551D) rings, CoMo
Catalyst 1)
TK-554 82.4 - - Batch Sock loading
(1501D & 1551D) 1.3mm(1/20inch)
three lobe
1) Minimum 2 years for the 1st cycle life and 4 years for the ultimate life.
Chemicals
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Consumption
Initial Life
Cont.
Filling Time 3
Service Type per year /Batc Remarks
months
h
[m3] [years] [kg] [kg]
Catalyst Sulfiding 1) 1) 1)
DMDS Batch
Agent
Corrosion inhibitor Nalco EC1021A 1.0 2) 230 57 Cont.
(Filming)
Neutralizing Agent 4) 4)
Soda Ash (Na2CO3) - Batch
Neutralizing Agent 4) 4)
Sodium Nitrate - Batch
(NaNO3)
1) 11,600 kg of DMDS for catalyst sulfiding during start-up and after catalyst regeneration.
2) 1.8kg/day of corrosion inhibitor diluted with LGO. It is injected to 1501E on 1 to 40ppm. Chemical type and cons
umption is preliminary and to be finalized according to the vendor’s information.
3) 266,000 kg of pure caustic to neutralize reactor effluent gases for the regeneration of the catalyst.
4) 3,500 kilograms of soda ash (Na2CO3) and 350 kilograms of sodium nitrate (NaNO3) for neutralizing of the auste
nitic stainless steel lining in the reactor section.
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TABLE 6
Unit 15 Remarks
Revamp of Unit 15
Subject to conditions
1. The Gas oil feed shall be substantially as Feedstock maximum specified by Haldor-Topsoe
follows:
Composition
Vol%
1 182 184
5 234 235
10 247 247
30 266 262
50 277 279
70 309 304
90 330 335
Water 0 0.27
Haxane 0 0.49
Nitrogen wt ppm 28 30
Cetane index ASTM D-976-80 Shall not be less than the Cetane index of the feed
Yield wt% 93.9 94.3 Of the similar TBP fraction in the feed
Start of Run Pressure Drop for new reator (bar) 1.1 (max.)
5. Catalyst Guarantees :
( Table 6. continued)
Unit 15 Remarks
The above table lists the unit capacities, composition and properties guaranteed by open art unit
process designer.
TABLE 7-1
UTILITY SUMMARY (NORMAL)
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Exchangers
1501C1 Reactor 13.7
1503C1 Stripper 9.53
1506C Stripper Off 0.295 -29.7
1507C Reactor 1.21
Air Coolers
1502C Reactor 10.76 - 15x4
1504C Gas Oil Trim 1.435 -11x2 15x2
1504C1 Gas Oil Trim 1.435 - 5.5x2
1505C Stripper 0.844 -6x2 7.5x2
Pumps
1503J Gas Oil Feed -308 345
1503JA Spare for (- (345)
1504J Wash Water -15.4 30
1504JA Spare for (- (30)
1505J Stripper -8.5 11
1505JA Spare for (-8.5) (11)
1506J Gas Oil -102 132 -2.7
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TABLE 7-2
UTILITY SUMMARY (MAX)
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Exchangers
1501C1 Reactor 13.7
1503C1 Stripper 9.53
1506C Stripper Off 0.325 -32.7
1507C Reactor 1.21
Air Coolers
1502C Reactor 10.76 - 15x4
1504C Gas Oil Trim 1.435 -11x2 15x2
1504C1 Gas Oil Trim 1.435 - 5.5x
1505C Stripper 0.844 -6x2 7.5x
Pumps
1503J Gas Oil Feed -308 345
1503JA Spare for (- (345)
1504J Wash Water -15.4 30
1504JA Spare for (- (30)
1505J Stripper -8.5 11
1505JA Spare for (-8.5) (11)
1506J Gas Oil -102 132 -2.7
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( ) Indicates spare service, not included in totals. (*1) : The sum of possible simultaneous consumption
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3.2.1 Introduction
The main hydrodesulphurisation purpose is to eliminate the major amount of sulfur components
contained in the charge, and to improve the product qualities by taking into account pollution,
corrosion and odour specifications.
The nitrogen compounds are hydrogenated, and the catalyst retains the metallic components.
The reactions are exothermic, and aid in release of hydrogen sulphide and ammonia. A hydrogen
gas recycle limits the coke deposits on the catalyst.
3.2.2 Reactions
2) Aromatics: Aromatic hydrocarbons are more difficult to saturate owing to the presence
of sulphur. The reaction depends on the hydrogen partial pressure, and takes place
preferentially on polynuclear aromatics that have an olefinic character. This reaction is
highly exothermic, and improves the product quality.
R-NAPHTALENE
R
+ 2H2
Not available
R-TETRALIN
R
+ 3H2
Not available
The reaction of hydrogen with the aromatic compounds present in the feed is reversible. At
higher temperatures or at lower hydrogen partial pressure, the rate of the reverse
(dehydrogenation) reaction increases relative to the hydrogenation reaction. The amount of
conversion of aromatics decreases as the reactor temperature is increased above
approximately 675F. At the end of run, the amount of di and tri-aromatics in the product
will be greater than at the start of run.
The types of reactions that occur in the reactor that involve sulphur compounds include
reactions of mercaptans, sluphides, disulphides, thiophenes, benzo-thiophenes and di-
benzothiophenes. Hydrogen sulphide is formed in the reactor as a result of these reactions.
An example of these reactions is shown below:
HDS :
DI-BENZOTHIOPHENE DI-PHENYL
BENZOTHIOPHENE ETHYLBENZENE
All of these reactions consume hydrogen and are highly exothermic. The amount of hydrogen
consumed per weight percent of sulphur in the feed is dependent on the types of sulphur
species that are present.
Only the most difficult to remove sulphur compounds remain thiophenes that have an alkyl
group attached to the carbon atom or atoms adjacent to the sulphur atom. Two of these
compounds are 4-methyl di-benzo-thiophene and 4,6 di-methyl-di-benzo-thiophene.
[Link] Hydrodenitrification Reaction
Nitrogen is contained essentially in heterocyclic compounds. Hydrodenitrification is a more
difficult reaction than hydrodesulphurization.
Part of the nitrogen and oxygen containing organic compounds that are present in the feed to
the unit is converted in the reactor, producing ammonia and water as a by-product. The
content of nitrogen and oxygen compound is very small for the design feed. Very little
hydrogen is consumed by these reactions. The importance of the denitrogenation reactions to
form ammonia is that the ammonia formed can react with hydrogen sulphide or any chlorides
present in the makeup gas or feed to from solid deposits in the colder equipment in the unit.
These deposits are controlled by the addition of wash water.
Examples of the types of denitrogenation reactions occurring in the reactor are shown belows:
HDS :
INDOLE ETHYLBENZENE Heat of reaction at 25C (kcal/mol) :
C8H7H C8H10
CARBAZOLE DI-PHENYL
H
H
C12H8H C12H10
Although hydrocracking reactions occur in the reactor, the amount of hydrogen consumed by
these reactions is small. These hydrocracking reactions are also exothermic and result in a
temperature increase across the reactor.
At the start of the run, when the reactor average temperature is low, very little hydrocracking
takes place. As the reactor temperature is increased, the rate of hydrocracking also increases.
The net result is an increase in light gas (methane, ethane, propane, butane) and naphtha
formation as the catalyst ages. The average boiling point of the desulphurised distillate also
decreases from the start to the end of the catalyst cycle.
The principal operating variables of the hydrogenation reactions are the following
Temperature,
Pressure,
Space velocity,
Charge quality.
3.3.1 Temperature
Every increase in temperature increases the hydrogenation reaction speed. However, the coke
deposit also increases on the catalyst. So, it is necessary to find a balance between a catalyst
life and complete hydrogenation.
3.3.2 Pressure
The pressure is normally maintained at a maximum compatible with the equipment. This
pressure has a favourable effect limiting the coke deposit on the catalyst (increase of the
hydrogen partial pressure), and promotes the hydrogenation of nitrogen compounds.
The secondary reactions (saturation and hydrocracking) increase with the pressure, and
increase the hydrogen consumption.
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The space velocity is the residence time of the feed on the catalyst. It indicates the hourly
flow rate of liquid fresh feed in a ratio to the volume of catalyst, and provides indications on
the severity of the operation.
In general, a low space velocity will improve the reactions. As the volume of catalyst is
fixed, only changing the feed rate may vary the space velocity.
A decrease of the feed flow rate (a decrease of the space velocity will promote the reactions
and permit reduction in the temperature to the reactor. In the inverse case, an increase of the
feed flow rate requires an increase of temperature.
This ratio is defined by the number of hydrogen moles divided by the number of hydrocarbon
moles in the reaction section. The greater this ratio is the smaller the coke deposit on the
catalyst, thereby improving the hydrogenation reactions. This is why the quantity of hydrogen
introduced in the reaction section includes the quantity needed for the hydrogenation reactions
and a quantity going through the reactor without reacting, which increases the partial pressure
of hydrogen. The recycled volume is greater than the one reacting.
The operating conditions vary according to the quality of the feeds. They will have a greater
severity for feeds with a high end point of distillation and/or which have a greater content of
impurities.
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Cold feed at 25C from storage enters under flow control to the coalescer 1503L for water removal
and then enters the feed surge drum 1501F. Hot feed to the LGO hydrotreater flows directly from
the crude unit 11 light gas oil stripper and arrives hot (149C) at the battery limit under flow control
in unit 11 and enters the feed surge drum 1501F. The design is based on 90% hot feed, 10% cold
feed. Pressure on the surge drum is maintained with a fuel gas blanket. Feed from the surge drum
is charged to the unit under level control using the gas oil feed pump suction line close to the vessel
to allow vessel isolation during a pump seal failure and/or plant fire.
Feed is preheated in the gas oil feed/reactor effluent exchanger 1501C1~4 and splits into two equal
streams, the split controlled by a proportioning circuit on the feed level control loop. Each stream is
mixed with treat gas which has been preheated in reactor feed gas/effluent exchanger 1507C and
which also has been divided into two equal streams upstream on the mixing tee under proportioning
flow control. The combined feed and treat gas is heated to reactor inlet temperature in the reactor
charge furnace 1501B. Each half of the combined feed uses one heater pass. The hot charge from
each heater pass enters desulphurisation reactor 1551D, then passes through 1501D.
Cooled effluent is separated into hydrocarbon liquid, sour water, and vapour phases in the HP flash
drum 1502F. Hydrocarbon liquid is dropped in pressure under level control and enters the LP flash
drum 1503F. Sour water is sent by level controller 15-LV-036 to the sour water-stripping unit for
removal of hydrogen sulphide and ammonia. Disposition of the HP flash drum vapour is described
in paragraph 4.3.
A pressure control on the HP flash drum maintains the hydrotreater unit pressrue by adjusting the
exiting purge gas (paragraph 4.3).
Hydrocarbons entering the LP flash drum are separated into hydrocarbon liquid, sour gas, and a
small amount of sour water. The sour gas is directed to the amine treating Unit16. Pressure control
on the LP flash drum is maintained by adjusting sour gas flow. Sour water is sent to the sour water
stripping unit. Flash drum liquids are charged to the light gas-oil product stripper 1501E as
described in paragraph 4.4
4.4 AMINE TREATING, PURGE, MAKEUP AND RECYCLE GAS COMPRESSION, AND
TREAT GAS
HP flash drum vapour phase from 1502F is washed with monoethanol amine (MEA) in the recycle
gas H2S scrubber 1502E to remove hydrogen sulphide. MEA is supplied to the battery limits at
adequate pressure to enter 1502E without further pumping. A portion of the washed gas is purged
to control the build-up of light hydrocarbons, the remainder of the gas enters the recycle gas
compressor 1501J2 or 1501JA2 via the recycle gas K.O. drum 1507F.
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The emergency depressuring station is provided on the knockout drum overhead line. The
depressuring orifice is sized for an initial depressuring rate of 6.9 bar per minute. The depressuring
station is provided with an 15-Hs-030A which can be opened from the control room.
Recycle gas from 1501J2/JA2 is mixed with makeup hydrogen discharging from the makeup gas
compressor 1501J1/JA1. The makeup gas compressor takes suction from the hydrogen header
which normally draws gas from the naphtha hydrotreater unit 12. Mixed recycle and makeup gas
(treat gas) is preheated, and enters the reactor inlet as previously described in paragraph 4.1.
LP flash drum 1503F liquid (stripper feed) is dropped in pressure through a flow Controlled valve
reset by 1503F level control. Stripper feed is heated to stripper inlet temperature in the stripper
feed/effluent (stripper bottoms) exchanger 1503C.
Feed enters the product stripper 1501E. Supplemental energy for stripping is provided by stripper
reboiler 1502B. Stripper overhead is condensed in the stripper overhead condenser 1505C,
combined with a small stream of condensate from the compressed gas K.O. drum 1506F (described
below), and enters the stripper reflux drum 1504F. The hydrocarbon liquid from this drum is
pumped with stripper reflux pump 1505J/JA back to 1501E as reflux with a small portion of the
pump discharge drawn off to the crude distillation unit 11 as wild naphtha. Alternatively to
condensate distillation unit 61.
Sour water from drum 1504F is directed to the sour water stripper in unit 11. via new drum 1516F
and new pump 1510J. PCR(15-10-001).
Sour gas from 1504F passes through stripper off-gas K.O. drum 1505F, is compressed with sour gas
compressor 1502J/JA to sour fuel gas pressure, cooled in the stripper off-gas cooler 1506C, and
passes through compressed gas K.O. drum 1506F. A small amount of condensate is removed from
1506F as wild naphtha to unit 11 or 61. The compressed sour gas combines with the sour off-gas
from the LP flash drum (paragrpah 4.2), and is directed to the amine-treating unit 16. Stripper
pressure is controlled by adjusting the recycle gas on the sour-gas compressor.
Stripper bottoms are product light gas oil. The product is pumped with the gas oil product pump
1506J/JA under stripper level control and cooled by heat exchange with the stripper feed in stripper
feed/effluent (stripper bottoms) exchanger 1503C1~6, and gas oil trim cooler 1504C/C1.
A line is provided from the discharge of pump 1506J/JA for recirculation of product back to the
feed drum. This is useful for start-up and also when battery limit feed is tempeorarily unavailable.
Corrosion inhibitor is added via corrosion inhibitor tank 1502LF and pump 1502LJ into the stripper
overhead line. This reduces the potential for corrosion in this sour service.
6.4 REGENERATION
During regeneration, the unit is charged with nitrogen and circulation maintain with make-up and
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the recycle gas compressors. The make-up and recycle gas compressors 1501J1/J2 or 1501J2/JA2
may be used to maximse regeneration gas flow. The H2S scrubber 1502E is bypassed during the
procedure. During the burning phase, air is introduced into the compressor suction with a portable
compressor and closely monitored so that the oxygen concentration in the gas to the reactors is
about 1~2%.
Compressor discharge flows through the reactor feed gas/effluent exchangers 1507C and the reactor
furnace 1501B and is heated to the reactor inlet temperature required for sustaining the catalyst
burn. Flue gases from the reactor pass through the reactor effluent heat excahgners 1501C1~4 and
1507C. Sodium hydroxide (caustic soda) solution is injected into the flue gas stream and the
mixture cooled in the effluent cooler 1502C. The caustic neutralises sulphur dioxide and a portion
of the carbon dioxide formed in the reactor to prevent corrosion of the air cooler and downstream
piping.
Caustic is separated from the flue gases in the HP flash drum 1502F. Caustic is normally
recirculated by caustic circulation pump, 1507J and blowdown stream of spent caustic removed. A
portion of the flue gas is purged from the system to prevent build-up of carbon dioxide in the
recirculating nitrogen. Fresh nitrogen is added to maintain the system pressure.
Contact of oil with hydrogen gas takes place in the presence of a catalyst in the reactors. Under the
appropriate operating conditions of temperature, pressure, and time over the catalyst; the
desulphurisation reaction takes place. Sulphur in the feed combines with hydrogen and enters the
gas phase as hydrogen sulphide(H2S) which can readily be separated downstream of the reactor
from the product oil. The gas oil is cleaned of sulphur to levels below 0.05% weight.
Two reactors are required for holding sufficient catalyst to provide a liquid hourly space velocity of
2.5 needed to achieve gas oil desulphurisation to 0.05% weight maximum in the product gas oil.
The existing reactor 1501D is designed to contain 27m3. With addition of the new reator 1551D,
the total catalyst volume will be nominally 60m3. The new reactor will be added upstream in series
with the existing reactor. Placing the reactor in this position provides greater flexibility for adding
reactor internals which may be required for installation of the distributor, distirbutor tray, and other
equipment which may be necessary for provision of the graded catalyst bed.
6.2 COMPRESSORS
The make-up compressor supplies the hydrotreater with hydrogen from the naphtha hydrotreater
hydrogen product header. The recycle gas compressor circulartes the gas which has been separated
from the treated oil back to the reactor. The recycle gas is separated from oil in the HP flash drum
and passes through the amine contactor in which the generated H2S is removed. The gas passes
through the recycle gas compressor, mixes with the fresh hydrogen, is heated to reactor inlet
temperature and contacted with oil in the reactor, is then cooled and finally separated from the oil to
complete the loop.
Both the make-up and recycle gas compressors are new for handling the operating conditions
required for the revamped hydrotreater. The recycle compressor will be required to circulate
nitrogen during startup, presulphiding, and regeneration and appropriate notes have been added to
the compressor data sheets.
Installation of flange with valve for chemical cleaning /steaming facilities for de-plugging Cooling
system for both compressor of unit 15 during normal operation and shutdown to avoid higher
temperature. PCR No (15-11-005). In case of higher gas temperature of compressor, these facilities
can be used for de-plugging the cooling water line via high pressure water / steam during normal
operation.
The sour gas compressor increases the pressure of the off-gas from the product stripper to sour fuel
gas header pressure upstream of the amine treating unit 16. Because of increased gas rates, two new
compressors are required.
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The reactor effluent exchangers conserve energy by warming the treat gas (incoming hydrogen plus
recycle gas) and fresh gas oil with hot reactor effluent. As much heat as possible is removed from
the reactor effluent stream to conserve fired heat required in the heater.
Four new shells are required for the gas oil feed/reactor effluent service 1501C1~4 replacing the
existing three shells. This permits a greater temperature cross and reduces the heat duty of reactor
charge furnace 1501B. The existing shells in the reactor feed gas/effluent exchanger 1507C are too
small to handle the increased reactor effluent flow and were replaced by one new shell.
The reactor charge furnace 1501B heats reactor feed to the requird reactor inlet temperature. The
existing heater was checked and found to be adequate for the new service.
NODCO inspection reports (1993 and 1995) indicate that the airCooled reactor effluent cooler
1502C is severely fouled and may required major repairs or replacement. Until this is confirmed, it
is assumed that a new air cooler is required.
6.4 DRUMS
All drums in the unit are adequate for the new service. Surge times in the predominantly liquid
holding drums are as follows:
Minutes
Feed surge drum 18
HP Flash drum 7
LP Flash drum 7
Stripper reflux drum 12
Other drums are adequate to handle the required gas flows and to separate entraind liquids.
A gas-blanketed wash water drum has been added. The feed surge drum, stripper reflux drum, and
stripper off-gas drum require increased nozzle sizes.
New knockout drum (1515F) installed during 2013 to improve consistent refinery wide fuel gas
heating value, remove impurities, and stabilize supply pressure and improving burner reliability.
The product stripper removes H2S and light hydrocarbons from the hydrotreated gas oil. Removal of
the light hydrocarbons ensures that the flash point is within specification.
The product stripper is adequately sized for the new service and calculations indicate that the trays
will be satisfactory. However, tray loads will be forwarded to the tray vendors for their check, as the
vendors will provide a guarantee and may wish to perform tray modifications.
No. of tray : 6 16
No. of passes : 1 2
Material : 410S
In the H2S scrubber 1502E, sour gas from the HP flash drum is washed with monoethanol amine
(MEA) to remove hydrogen sulphide and ammonia. The column is adequately sized to handle the
gas and increased liquid flow in the revamped unit, but the packing will require change to a type
with lower pressure drop such as pall rings.
The objective of ESD/PSD system is to prevent undesirable event and minimize their consequences.
It is activated in a critical situation in the unit to prevent the unit to go out of control and in case of
leakage, fire and accidents. The system is designed to limit damages on environment and to
minimize the risks on personnel.
The levels of shutdown depend on the severity of the event and are configured to ensure safe and
effective shutdown of the equipment/plant in a controlled manner.
The shutdown levels comprise of 3 levels, which are according to the increasing levels of hazard.
They are:
Note: Level 3 shutdown is the most severe and is activated only if Level 2 shutdown is active. Level
3 shutdown is activated manually only.
The objective is to protect facilities and personnel in the event of serious process malfunction.
The operator is responsible for taking the decision to activate this level of shutdown.
In order to enable a quick restart in case of rectification of the problem within a reasonable
length of time, no blowdown facilities are included.
The objective is to minimize risk and to protect environment and personnel under upset
conditions/emergencies.
Operating Manual 2500-15-00-80-001
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The operator is responsible for taking the decision to activate this level of shutdown.
Level 3 shall only be activated if the facility has reached a Level 2 status. This is activated
manually by a blowdown push button located on the CCR DCS console.
7.2 DESCRIPTION
No.2 GO Hydrotreater (Unit 15) is provided with three levels of shutdown, Level 1, Level2 and
Level3.
This is detailed in the Cause & Effect Table in P&ID (Chapter 24) Drawing No. 7J48N-15-00-
30-005
This is activated by 15-HS-001A and 001B. 15-HS-001A is located in the CCR while 15-HS-
001B is in the field.
Separate SIL study done for unit (15) as details report available.
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The start-up is represented on the following preliminary precommissioning and start-up schedule.
This schedule shows approximately when the successive operations should be carried out and the
duration of these operations, from the checking of the unit until the performance test.
This schedule may be modified following the local conditions and particularly buyer's
requirements.
For the first start-up, it is necessary that several items be taken care of before the unit can be
considered ready for oil. Most of these items might be considered as construction details, in as
much as subsequent plant start-ups will not require the repetition of all of them. Such items
may be summarized in action as follows
The lines and equipment should be divided into convenient sections for hydrotesting. In any
given section the pressure test applied should be equal to the allowable test pressure of the
lowest rated equipment in the circuit.
In hydrotesting sections which include heat exchangers, special care must be exercised to
avoid exceeding the design differential pressure across the tube bundles, especially for
exchangers in the reactor system. A temporary connection may have to be installed to ensure
that both sides of the exchangers are pressured to the same level. Before the pressure test is
concluded, exchangers must be tested at the design differential pressure to ensure that no
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leakage exists.
The test pressure must be held until it is certain that the section being tested is tight, and all
leaks have been eliminated. In addition to process lines, utility lines (steam, air, etc.,) should
also be tested. The contractor and refinery personnel responsible for such tests must witness
all pressure tests.
In general operating staff is not involved in hydrostatic pressure tests that are carried out at
the end of the construction period.
4) Plant Inspection
The equipment must be checked to see that it conforms to the detailed P&I drawings and the
Project Specifications. Attention should be given to the location of vents, drains, gauge
glasses, pressure gauges, sample points, etc., to ensure that they are accessible.
5) There should be sufficient room for expansion when the unit is heated. Particular attention
Break-in compressors
6) Service and calibrate instruments.
7) Pressure test equipment.
Following construction, the various utilities such as steam, cooling water, air, etc., must be
put in service. The various lines must be tested for leakage and should be washed free of
debris and construction trash. This latter may be done by water flushing and air blowing to
atmosphere. Fuel gas lines must be steamed out or N2 purged to remove air before admitting
gas. Steam lines should be warmed up slowly to prevent damage by water hammer. All steam
traps and control valves in the system should be placed in service and tested. Likewise,
control systems in the air, water, and fuel systems should be tested for operability.
a) Steam networks
Networks shall be blown through completely from battery limit with a strong steam flow
in order to clean the lines. The following steps are recommended.
open slightly battery limit valve and let the temperature rise in the header, slowly and
steadily,
when the line is hot, blow it through completely with a strong steam flow,
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When the blowing is satisfactory, reconnect all the equipment and remount the stream
traps.
Note:
To drain the low points of lines during the heating period of the collectors in order to
avoid water accumulation which causes water hammer, this also checks that the lines
to steam traps are not plugged.
To open the vents during all the cooling periods to prevent creating a vacuum.
Networks shall be cleaned with water from battery limit with strong water flow.
c) Cooling water
Networks shall be cleaned from battery limit with a strong water flow. All the equipments
will be disconnected at the inlet and reconnected when lines are cleaned. When the
systems have been washed out, pressurize the lines to the operating pressure.
Note :
To open the vents at high points in order to evacuate the air contained in the
equipment and the piping.
Networks shall be blown through completely from battery limit with a strong air flow in
order to clean and dry the lines.
The instrument air system shall be tested pneumatically with dry air.
All joints and connections shall be checked for tightness with soapy water solution.
Heater and branch lines shall be blown through with a high flow rate of air. During all
these tests, the instruments, supplied with air, shall be carefully isolated from the system.
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Networks shall be blown through from battery limit with a strong steam flow for fuel-oil
and a strong air flow for fuel gas in order to clean the lines.
During this operation, the orifice plates and control valves shall be removed.
f) Sewers
Sewer system is the first system to be prepared and placed in service, ready to receive the
various discharges.
It is very important that the internals of the hydrotreating reactor be inspected very carefully.
The hydrotreating reactor internals should be checked for holes and/or damage and repaired
as required. The catalyst support basket and unloading sleeve should be checked to insure
correct fit in the nozzles.
The product separator should be checked carefully to be sure the cement lining is installed
well, and that the mesh blankets is securely fastened to the support ring. There should be no
gaps in the mesh blanket, which can occur at seams between sections or between the blanket
and the vessel shel1.
In pressure testing equipment, particularly in cold weather, care should be taken that the
testing of the vessels is not carried out at temperature levels so low that the metal becomes
brittle. As metal temperatures decrease, the tendency for brittleness increases. Temperatures
above 17℃ (60℉) are considered satisfactory for testing to eliminate the possibility of cold
fracturing of equipment. Such temperatures can be attained by warming the testing medium.
If the unit contains any austenitic stainless steel, the chloride content of the test water must be
less than 50 ppm. If this is not possible, then the test water should have 0.5% wt. sodium
nitrate added to it.
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It will not be practical to test all of the equipment together. Thus, the unit will be divided into
sections as governed by the location of the various items of equipment and the test pressures
to which each item will be subjected. Suitable blanks must be made up for insertion on
nozzles and between flanges to isolate the various sections of equipment as required.
Normally, the exchangers, receivers, etc., for the various towers will be tested together with
the main vessels. Test pressures will be determined from the pressure vessel summary for the
unit. During pressure testing, all safety valves must be blinded off, since their normal
relieving pressure will be exceeded.
It may be convenient to test the heaters and reactors in one group. A field hydrostatic test on
the gas compressor after installation could result in damage to the internals, so the
compressors must be isolated from the reactor system. As the heaters are normally tested at a
higher pressure than the reactors, it would be simplest to blind off the heaters, Test them first,
then Test the entire system at the reactor test pressure. Blanks can be provided with
connections for introduction of water for testing and for venting of air as the system is filled
with water. It may be necessary to use thermowall connections and pressure taps for
additional vents in the reactor system. At the completion of the hydrostatic test, all water
should be removed from the equipment. Where necessary, flanges may be broken to drain low
points and the equipment air blown to remove as much water as possible before flanging up.
After the hydrostatic pressure test has been completed on any vessel with its connected
piping, receivers, exchangers, etc., required blanks are pulled and water is circulated for the
purpose of removing any dirt, scale, etc. Much of the dirt is picked up in the pump screens,
where it is taken from the system by removing and cleaning the screen.
A1l possible lines and pumps should be used during the washing procedure for complete
clean-up of the system. Of course, no water circulation should be carried out in the gas
sections of the Unit.
All towers and drums should be manually cleaned before flushing. The fire water system
should be flushed first and can be used to supply water for flushing the rest of the plant.
Before flushing, open overhead vents on vessels (to avoid vacuum), disconnect pump
suctions and discharges, cover pump nozzles, and "drop out" or "roll" control valves and
orifice plates. Open compressor headers and blank off compressors.
Fill vessels with water and flush lines away from vessels or drums, especially if equipped
with internals that could be fouled. All lines not flushed by vessel drainage must be
flushed independently.
Lines connected to exchangers should not be flushed into exchangers but the joint should be
disconnected and the exchanger flange covered with a piece of sheet metal.
After sufficient flushing, the line can be reconnected and water flushed through the
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Reconnect pump suction lines after initial flushing and insert 20 mesh or 30 mesh screen
linings in pump strainer and continue flushing, changing to spare pump and cleaning
strainers when plugged. This operation should continue until no debris is collected on the
strainers.
Any equipment flushed into should be opened and cleaned manually. Block valves or other
valves not "rolled" or “dropped out" should be checked for closure and rolled out for
cleaning as required.
All equipment blinds not necessary during start-up should be removed during or after the
flushing operation.
All control valves and orifices should be installed when line flushing is completed.
Prior to unit start-up, all centrifugal pumps should be thoroughly checked and run-in
properly (after pressure testing and water flushing) as indicated in the following outline.
Caution: Many high head pumps are not designed to pump water. To do so can result in
damage to the pump internals. Check the Vendor's specifications before attempting to run-in
pumps with water.
a) Check to see that all necessary water piping has been made to stuffing boxes, bearing
jackets, pedestals and quench-glands. Make sure that all necessary lube all piping is
installed, and that this piping is not mistakenly connected to the water system.
b) Check arrangements to vent the pump for priming if the pump is not self-venting. See
that special connections such as bleeds and drains are properly installed.
c) Check strainers in pump suction lines. Strainers must be installed before aligning
pumps. A three to six mesh strainer is provided for each pump suction line during start-
up. To avoid pump damage during flushing with water, the strainers should temporarily
be lined with 20 mesh or 30 mesh screen.
Remove this screen after water flushing is completed. All strainers should be flagged,
and a list similar to the blind list should be kept, so as to prevent a "lost" screen from
plugging and upsetting unit operation later on.
d) Check that power or steam is available for running-in the pump. Check that: pressure
gauges and any special instrumentation are in working order.
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Water circulation on motor driven hydrocarbon pumps can result in motor overloading
if the full pumping capacity is used. In this type of equipment, the capacity must be
reduced by throttling the discharge during such periods. An ammeter can be used to
determine the required throttling.
e) Before lubricating oil-lubricated bearings, check bearing chamber in pumps to see that
no slush compounds or shipping grease is left in the chamber.
f) Mechanical type seals should be flushed with water prior to pump operation so no dirt
gets into the seal and scores the seal faces.
g) It is extremely important that the proper type and viscosity all and proper grade of
grease is used to lubricate the equipment. Refer to manufacturer's instructions and
refinery lubricating schedule for this information.
h) See that the driver rotates the pump in the direction indicated by the arrow on the pump
casing. Rotate the pump by hand to see that it is clear before starting.
i) Couple up and align the pumps, then check for cooling water availability and start flow
of cooling water to the pumps requiring external cooling, before they are run in.
j) Open pump suction valve and close discharge valve (crack discharge valve for high
capacity, high head pumps). Make sure the pump is full of liquid.
k) Start the pump. As the pump is motor driven, the pump will come up to speed.
Immediately check discharge pressure gauge. If no pressure is shown, stop the pump
and find the cause. If the discharge pressure is satisfactory, slowly open the discharge
valve to give the desired flow rate. Check the amperage of the motor. Do not run the
pump with the discharge block valve closed, except for a very short time. Note any
unusual vibration or operating condition.
l) Check bearings of pumps and drivers for signs of heating. Recheck all oil levels.
m) Run the pump for approximately one hour, then shut off to make any adjustment
necessary and check parts for tightness. Since it is not possible to run the pump at
operating temperature, a final check of alignment must be made during normal
operation by switching to the spare pump.
o) Shut the pump down and pull the strainer. Clean the strainer and replace it in the suction
line. Remove the temporary fine mesh liner from the strainer after water flushing is
completed.
On a new unit, the screens are sometimes left in service for the first run on all locations
where spare pumps have been provided.
Water circulation with motordriven hydrocarbon pumps can result in motor overloading, if
the full pumping capacity is used on water. In this type of equipment, the capacity must be
reduced by throttling the discharge during such periods. When water is used for pressure
testing and washing, it is sometimes better to have packing in the pumps for a seal to
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Of course, no water circulation should be carried out through the gas compressors. It is
important that the catalyst and the compressors are not exposed to excessive moisture.
As with the pumps the compressors should be run-in as soon as construction permits to find
and correct problems early. The initial run-in of all compressors should be carried out under
the supervision of the manufacturer's representatives. Before running any of the machines, the
operators should familiarize themselves with the pertinent operating instructions including
1ubricating, cooling and safety requirements.
The compressors will be run-in on air according to maker's instructions. Before operation of
the compressors, the following items should be completed:
2) If portion of make-up and recycle system were acidized they should be under a nitrogen
blanket since the completion of the acid cleaning.
5) It is extremely important that all instrumentation on the compressor and its associated
equipment be thoroughly checked to ensure proper installation and function. All alarms
must be tested. All shut down alarms must be tested.
Before running any of the reciprocating compressors, the cooling and lubrication system must
be placed into service. Before loading any compressor, be certain that all liquid has been
drained from the lines, snubbers, etc.
The charge heater dry-out can be performed by itself or it can be coupled with the run-in of
the recycle compressors and the dry-out of the reactor system. Although it is probably
preferable to combine all three operations, the charge heater may be ready for dry-out before
the reactor and compressor system. It that case it may be desirable to do the heater dry-out by
itself. The heater manufacturer's procedure for refractory dry-out should be consulted and
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incorporated into either method used. See Chapter 14 for the dry-out procedure.
The recycle compressor will be run in on air at maximum flow through the reaction section, if
possible, according to the manufacturer's instructions. All possible low points will be open to
remove the water still remaining in the system after the flushing of the equipment.
During this operation the make up compressor may be run at 0% capacity by unloading the
valves.
Caution : Recycle cylinder should not be operated at 0 % capacity for more than 20 minutes.
Make-up cylinder can run permanently at 0% capacity. When running unloaded, the cylinders
do not compress and the same gas is always recycled in the suction valves. Excessive
overheating can occur causing damages of the wearing parts. See manufacturer's instructions.
When this operation has been completed and vessels inspected for cleanliness, catalyst can be
loaded into the reactor and packing into the gas absorber. Demister pads, orifice plates and
restriction orifices can be installed and a check made on all instrumentation for correct
installation and operation.
As the recycle gas scrubber 1502 E needs degreasing before start-up it will be included in the
unit 16 washing operation for the circulation of the cleaning solution. Refer Unit16 Operation
Manual Chapter 14, chemical cleaning of the unit.
Prior to starting the air coolers, the motor-driven fans are run-in for at least four hours. The
auto variable blade will be adjusted, so that the amperage on the driver is near the maximum.
Before start, the following checking must be done:
Coupling.
1) Check the entire plant to ensure that all vents and drains are closed, and that the unit process
lines are blinded off at battery limits. Pressure tests are now carried out on the unit using
plant air tied in at suitable points, to ensure that no major leaks exist due to omissions of
vessel test plugs, gaskets, etc.
All flanges and manholes should be checked for leaks using tape and soap solution.
The reactor and the stripper sections will be tested at different pressures.
c) Test the equipment at 7 barg. Finally vent the system. Use the low points to drain any
remaining water left in the system.
Block off all pumps and test the system at 1.75 barg.
APPENDIX I
PUMP OPERATION
The following procedures are presented to outline the most important steps involved in pump operation.
Any modification of these procedures due to particular installation peculiarities should conform to good
engineering practice.
Suction Conditions
Sometimes the suction conditions imposed on a centrifugal pump are extremely unfavorable and lead to a
complete breakdown of the operation of the pump. The suction head or pressure should be kept within the
limitation for which the pump was sold. If the original operating conditions must be change for any reason,
consult your nearest Worthington specialist.
Care should be exercised to keep the suction piping air tight and sealed against leakage.
Preliminary instructions
Test the driver for rotation with the coupling bolts removed. An arrow shows rotation on the pump casing
Starting Pumps
Refer to the lubricator section and be sure that the bearings have been properly lubricated. Before starting
the pump initially, turn the rotor over several times by hand to lubricate the bearings.
If cooling water is required by the operating conditions, open the valves in the cooling liquid line. Once the
pump is in operation regulate the cooling liquid to prevent condensation inside the bearing housing.
Eliminating visible condensation on the outside of the housing can do this.
The valves on the liquid line to the stuffing box should now be opened. This step is imperative whether the
pump has a packed box with a seal cage, or a mechanical seal requiring flushing. The amount of fluid
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circulated to the stuffing box must be controlled at all times during operation. Operating experience will
indicate the proper procedure to be followed.
Open the suction valve and any vents or gauge connections in the system which will allow the air in the
casing to escape. Turn the rotor over by hand ; if it is bound, do not operate the pump until the cause of the
trouble is found. Start the driver according to driver manufacturer's instructions. Open the discharge valve
slowly as soon as the pump attains full speed.
If the discharge pressure gauge does not immediately register when the rotor is revolving at or near rated-
speed, immediately shut down and make a careful check of the suction line for obstructions in the line which
could interfere with the liquid flow to the pump. During the routine operation of the pump, the bearings
should be occasionally checked for proper lubrication and oil level. Check stuffing box operation.
Stopping Pumps
Normally, there should be a check valve and a gate valve in the discharge line. In such cases, stopping the
driver according to the driver manufacturer’s instructions can shut down the pump. The remaining valves are
then normally closed in the following order : discharge, suction, cooling liquid supply, and sealing liquid
supply. (In some services, the sealing liquid is left on continually to protect seals against the formation of
solid or crystals etc.).
In some installations the use of a check valve is not feasible due to the creation of pressure surges or water
hammer as a result of the sudden closing of the valve under high discharge pressure. In such cases the
discharge valve should be closed slowly prior to stopping the driver to eliminate the possibility of water
hammer.
A pump will partly drain through the glands if left standing for long periods of time. For this reason it is
recommended that the pump always be primed before start-up.
LUBRICATION
Oil used for lubricating ball or roller bearings should be a high quality, well-refined mineral oil which will not
readily oxidize or gum. Vegetable or animal oils should not be used. The oil should be certified to be free
from deleterious substances which would harm the bearings at any operating temperature.
1 - Drain the bearing bracket and flush it with a light oil, install the constant level oiler.
3 - Fill the bottle through the stem, replace and allow all to flow into reservoir. It may be necessary
to fill the bottle several times before the oil ceases to run into the reservoir, indicating that the oil
is up to the proper level.
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Caution
The constant level oil control maintains a constant level of oil in the reservoir. The control feeds only enough
oil to maintain the required level. It operates on the liquid seal principal, feeding only when the level in the
reservoir is low enough to break the liquid seal at the end of the shank, thus permitting air to enter the
bottle. It will cease to feed when there is sufficient all in the reservoir to cover the hole in the end of the
shank.
The oil fingers maintain circulation of the oil in the reservoir. It is recommended that the lubricating oil be
kept between 40℃ and 70℃, preferably above 50℃.
Bearing cooling water may be eliminated, when desired, for suction pressures up to 20 bar g when the
pumping temperature is below 50℃ In specific cases higher pumping temperatures are possible without
cooling up to 100℃ maximum with considerably lowered suction pressure. The bearing oil temperature
Oil Change
Operating conditions and severity of service will determine the intervals between oil changes. In general
higher oil temperatures will require more frequent oil change. If the bearings maintain their normal
temperature and there has been no contamination of the oil, the interval between changes may be
prolonged. Generally the oil should be changed every six months. If the bearing temperature increases, check
immediately for improper lubrication or a faulty bearing.
LOCATING TROUBLES
The troubles which may occur with your pump and their causes are listed below. The operator can often
avoid unnecessary expense by careful consideration of the points outlined.
a) Insufficient speed.
b) Discharge head too high (greater than that for which the pump is rated).
Insufficient Capacity
e) Insufficient NPSH.
f) Mechanical defects
- Impeller damaged.
b) Air in liquid.
c) Mechanical defects :
b) Liquid pumped of different specific gravity and viscosity than that for which pump is rated.
c) Mechanical defects.
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Pump Vibrates
a) Misalignment.
d) Mechanical defects :
- Bent shaft.
- Worn bearings.
e) Insufficient NPSH.
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The start-up procedure contained in this manual describes in general terms the steps to be followed
for placing the unit on stream. The following steps must be completed before charging oil to the
reactors.
The reactor and stripper section are treated separately. The reactor section is first placed under
vacuum and then filled with pure nitrogen whereas the stripper section is purged with steam
that is subsequently replaced by fuel gas. Appropriate blinds should be removed before the
purging operation.
After venting to atmosphere, the vents are closed and the section is placed under
vacuum by means of the steam jet ejector 1501L which is connected to the recycle
compressor section line so that the vacuum will be pulled in the normal direction of
flow. It is emphasized that whenever flow is established through the reactor, be it for
vacuum or pressuring, it must always be in the normal direction that is downward
through the catalyst bed.
Make sure that instrument connections are isolated to prevent damage when a vacuum
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of 600 mm Hg approximately has been reached, the ejector is first blocked off and then
shut down.
The pressure rise over a period of one hour is recorded and if it is greater than 25 mm-
Hg/hr the system is not sufficiently tight and should be retested under positive air
pressure to find the leaks.
Note: Open the 1 1/2 inch H2 pressurizing line between the make-up compressor
section and discharge in order to include the make-up gas K.O. drum 1508F in
the reaction section. When the system is sufficiently tight, the vacuum is
broken using nitrogen which is introduced downstream of the recycle gas
compressor and allow pressure to build up to 0.3 barg. Then the ejector is
restarted to remove the nitrogen.
Repeat this process two or more times until the oxygen content of the system, sampled
at the ejector, is less than 0.5% by volume.
Once purging is complete the reactor section is held at a nitrogen pressure of about 0.3
barg.
At the same time that the reactor circuit is evacuated, the compressors must be
thoroughly purged with nitrogen before admitting hydrogen into the unit. Do not pull a
vacuum on the compressors but leave them blocked in during the reaction section
purging phase.
With the suction and discharge block valves closed and the by-pass open, introduce
nitrogen via the nitrogen connection provided at each head. When the system is at the
nitrogen supply pressure or at least 3.5 bar g, shut off the nitrogen supply, bar over the
compressor and then vent off the nitrogen.
Repeat the above operation two or more times or until the oxygen content is less than
0.5% by volume.
This procedure applies for the recycle and make-up gas compressors 1501J1/J2, 1501
JA1/JA2 as well as the product stripper overhead sour gas compressors 1502J/JA.
The product stripper section, the feed coalescer 1503L, the feed surge drum 1501F, and
the LP flash drum 1503F are first purged by steam to displace air in the system, then the
steam is replaced by fuel gas.
g) Start steam purging, introducing steam through steam hoses and into steam-out
connections. When a steady continuous flow of steam has been issuing from the high
point vents for a minimum of one hour, fuel gas may be brought into the unit.
h) Close vents and steam purging connections. Close drains.
i) Slowly introduce fuel gas along the start-up connection. (2" line connected on the
product stripper 1501E).
j) Slowly bring the product stripper, the stripper overhead drum 1504F and the overhead
compressor K.O. drum 1505F to a pressure of 0.3 bar g. bring the rest of the system up
to gas pressure. Commission the 15-PIC-005 on the overhead drum.
k) Slowly bring fuel gas into the feed surge drum 1501F and commission the 15-PIC-001.
m) Establish a liquid seal of lean amine solution in the base of the H2S scrubber 1502E.
9.1.3 Circulation on start-up bypass - The stripper section - Cold oil circulation
The start-up bypass lines installed in the unit should be used to run-in the charge pumps, to
remove scale from the lines, and to inventory the stripper with oil. In order to avoid rapid
expansion of the pumps and lines due to the high temperature of the raw gas oil from the
crude distillation unit should this plant be running, the feed surge drum wi11 be fed using the
6" recycle line located downstream of the stripper bottom air cooler 1504C/C1.
a) Open the oil feed block valves on the 6” recycle line. Establish a normal working level in
the feed surge drum and leave the drum floating under controlled pressure from the fuel
gas system (15-PIC-001). During cold-circulation, the feed coalescer, 1503L should be
blocked
c) Line up the feed charge pump 1503J/JA via the 6" start-up line to the stripper 1501E and
establish the following circulation route: from the stripper 1501E through the bottom
pump 1506J/JA, product stripper feed/bottoms exchangers 1503C1/C2/C3/C4/ C5/C6,
gas oil trim coolers 1504C/C1 and the recycle line back to the surge drum 1501F, or to
storage if the crude unit is shut down. 15-FIC-016 at the liquid outlet of LP flash drum
1503F will have to be opened from the control room using 15-FIC-016, as there is no
product in the LP flash drum 1503F.
d) Start the feed pump 1503J/JA at a flow of 55m3/h (minimum flow allowed by the
manufacturer) using 15-HCV-001 on the 6” start up line. Establish a level in the product
stripper 1501E. Prime and start the stripper bottom pump 1506J/JA. It would be to
establish the flow to the stripper reboiler furnace 1502B first as close to design as
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possible. Control valves, 15-FV-025/026 at the inlet to the two passes are used to split the
flow equally.
f) During these operations and until the complete loop has been established it is advisable
that an operator keep watching the feed surge drum level and keep it normal by throttling
on the 6" recycle line feeding this drum.
g) During the cold oil circulation step it is assumed that the crude distillation unit will be
running only at 50% of design as both recycled stripper bottoms and raw light gas oil
from crude unit will be flowing through the gas oil trim cooler 1504C/C1, the split
between the two streams being made downstream the latter.
Drying of the fresh or regenerated catalyst prior to activation is preferably carried out using
treat gas, nitrogen or air. If hydrogen or gases containing large amounts of hydrogen (e.g.
recycle gas) are used, the reactor temperature must be kept below 200C (400F). Contact of
hydrogen with fresh or regenerated catalyst in the absence of sulfur particularly at higher
temperature will reduce the efficiency of the sulfiding treatment and the catalyst performance.
This is due to the risk of reducing the catalyst oxides to free metals that would be extremely
harmful to the catalyst activity. Therefore the heating up of the catalyst is carried out with
nitrogen at reduced flowrate.
Please note that ex-situ presulphided catalyst should not be dried out before activation.
a) IF hydrogen containing the reactor must be purged with nitrogen so that the oxygen
content of the reactor is less than 0.5 volume percent before introducing the hydrogen
containing gas.
c) Be sure that the nitrogen circulation loop is isolated from cold circulation in stripping
section, block valve in 6''-P-15-105-0-GA02 closed.
Check that block valves are closed in:
e) Light the reactor charge furnace 1501B according manufacturer's instruction. Start to
raise the reactor temperature to 150℃ (300F) over a 4 to 5 hour period. The
recommended maximum rate for heating up of the catalyst is 30℃/hr (50F/hr) to
minimize chances for leaks due to thermal expansion.
f) Maximize cooling of the effluent by 1502C. Check and drain water from the high-
pressure separator 1502F. When no more water is accumulated in the high-pressure
separator 1502F, the drying out of the catalyst is complete.
g) Stop the burner of the reactor charge furnace 1501B. Stop the make-up and the recycle
compressor 1501J1/J2or 1501JA1/JA2. Depressurize the loop.
h) If air is used for the above procedure, nitrogen purge must now be used in order to reduce
oxygen level in the reactor to less than 0.5 volume percent prior to the activation step.
Hydroprocessing catalyst can be delivered ex-situ presulphided. The ex-situ presulphiding is done
by impregnating the catalyst pore system with a sulphur-containing component dissolved in an
organic solvent or with elemental sulphur followed by a soaking of the catalyst in a paraffinic
hydrocarbon. When the catalyst is heated under hydrogen pressure, this sulphur-containing
component will decompose and release the sulphur in the form of H2S for the sulphiding of the
catalyst. Irrespective of type, ex-situ presulphided catalysts are dark gray with a slight small of the
organic solvent.
Hydroprocessing catalysts are very porous, having surface areas of 150-250 square meters/gram.
This is an important feature of the catalyst. Such porous catalyst is hygroscopic, i.e. water or
moisture is readily absorbed. As delivered, the catalyst will contain some water, normally about 1-
2 percent of the catalyst weight.
Furthermore, the catalyst may absorb some moisture during the loading. Therefore, the catalyst
must be dried before the activation is carried out. Please note that ex-situ presulphided catalyst
does not require drying before activation because this has already been done at the company doing
the ex-situ presulphiding.
Hydroprocessing catalysts including ex-situ presulphided catalyst must be activated before use.
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During the activation and the cobalt/molybdenum are converted to sulphides, which is the active
form of the catalyst.
The activation is very important for the subsequent performance of the catalyst charge and
therefore requires careful monitoring. During the activation, the catalyst will pick up 6-13 weight
percent sulphur depending on the level of active metal present in the catalyst.
There are several methods available for sulphiding the catalyst. The method recommended by
HALDOR TOPSOE is the doped feed method using an easily decomposable sulphur compound
mixed with the oil.
If other methods are considered, such as native sulphur or ex-situ presulphided, HALDOR
TOPSOE should be consulted in each case for advice.
In this procedure, a start-up feed is used with additional sulphur being provided by doping the
feedstock to about 1-2 weight percent sulphur with a sulphiding chemical. The startup feed is
a light straight-run petroleum fraction (e.g. kerosene or diesel) that is not higher boiling than
the normal feedstock. The start-up feed should have a maximum ASTM end point of 370℃
(700F).
A number of options are available for sulphiding chemical. The procedure as written is based
on using dimethyl-disulphide, DMDS. DMDS is the most commonly used sulphiding
chemical currently being used in the refining industry. If other sulphiding chemicals are
applied, adjustments to the procedure below may be needed and HALDOR TOPSOE should
be consulted. It is advisable to do a sulphur balance as a check on the level of sulphiding by
measuring DMDS added the organic sulphur in the feed and duct streams and the H2S
content in the gas product streams. Normally we recommend having an excess of 25 percent
available of the sulphiding chemical.
DMDS will be supplied from 4603LJ1 at Unit46.
n) The reactor must be dried out and purged with nitrogen, so that the oxygen level is less
than 0.5 volume percent. The temperature at the start of the procedure is maintained at
approximately 150℃ (300F) to minimize catalyst reduction.
o) Set the high-pressure flash drum pressure controller 15-PIC-003 to 4.2 barg.
p) Crack open the 6'' make-up hydrogen line to unit15 & 17 in unit12 and allow the reaction
section pressure to rise to 4.2 barg using the 1 1/2 inch pressurizing line. Check the
system for leaks. If the system is tight at this pressure, raise the pressure in 7 barg steps
using the HP flash drum pressure, controller 15-PIC-003, each time checking for leaks
until the make-up gas mains pressure is reached.
NOTE: During start-up of unit 15, natural gas will be used for the pressure control of
1701F
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r) Pressurize the reactor to normal operating pressure (unless limited by the ductile-brittle
transition temperatures of the reactor and equipment)
t) While pressurizing the unit, start the make-up and recycle gas compressor and establish
recirculation of process gas at normal flow rate. In order to conserve H2S the recycle gas
scrubber should be by-passed or the amine recirculation stopped during the sulphiding.
u) Line up the recycle and make-up compressors to discharge through 1507C to the charge
heater 1501B, reactors 1551D & 1501D, through feed/effluent exchangers 1501
C1/C2/C3/C4 and 1507C, through air cooler 1502C to the high pressure flash drum
1502F, through the 6" start up line by passing the recycle gas scrubber 1502E, to the
recycle gas to drum 1507F & 1508F and back to the make-up and recycle gas compressor.
The two valves on the 6” start up line are locked open during bypassing the recycle gas
scrubber 1502E.
v) Open the block valve in feed line 6"-P-15-105-0-GA02 and start to feed the reaction
section through the furnace by increasing the set point of 15-FRC-001, closing
progressively 15-HCV-001 in reaction section by-pass line. Make this change gently. Do
not allow reactor temperature to drop significant1y during the change.
w) Start flow of start-oil at normal feed flow rate. Adjust both 15-FRC-006 (H2) and 15-
FRC-001 (oil feed) for design flow-rate. This must be done gently to prevent thermal
shock
x) After stabilizing of flows, temperatures and pressures in the unit, the start-up oil can be
recirculated from the stripper, 1501E, if desired. This reduces the quantity of start-up oil
needed and may reduce off-specification material produced. Start-up oil recycle should
not be done through storage tanks because the unstripped start-up oil may contain H2S
that may accumulate in the storage tank.
y) Increase the reactor 1551D inlet temperature to 180℃ (360F) at a rate of (45F/hr).
aa) When the reactor inlet temperature is 180C (360F), start the sulphiding chemical
injection and adjust the rate to give 1-2 weight percent total sulphur in feed.
bb) Water is formed from the sulphiding reactions. Check the high-pressure separator, 1502F
at regular intervals for water accumulation and drain if necessary.
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cc) The reactor inlet temperature is increased to 225C (440F) at a rate of 25C/hr (45F/hr).
The catalyst is sulphided at this reactor of 1551D inlet temperature until breakthrough of
H2S. The reactor of 1501D outlet temperature during this period should not exceed 250C
(480F).
dd) In order to ascertain breakthrough of H2S, the high-pressure separator of 1502F off-gas
should be checked for H2S concentration at regular intervals. Breakthrough can be
defined as the point when consecutive stable measurement of H2S are above 5000 vppm
H2S. Breakthrough indicates completion of the first stage of the sulphiding.
ee) Raise the reactor inlet temperature to 350C (660F) at a rate of 15C/hr (30F/hr). Check
H2S levels at 1/2-hour intervals. Stop the heat-up rate if the H2S level drops below 3000
vppm. During this period, adjust the injection rate of the sulphiding chemical to keep the
recycle gas H2S content of 1-2 volume percent.
ff) Hold the reactor inlet temperature at 350C (660F). When all catalyst temperatures have
been at or above 330C (625F) for a minimum of 4 hours, the sulphiding phase is
considered completed.
gg) Lower the reactor inlet temperature at a rate of 30C/hr (50F/hr) to the temperature
specified as the start-of-run temperature(316C).
hh) Start normal straight-run feed (90wt% hot feed from unit 11 and 10wt% cold feed from
stroage) to the unit at design rate. 10wt% cold feed is fed after removing water by feed
coalescer 1503L and the cold-feed flow-rate is controlled by 15-FV-076. Start amine
circulation and put the recycle gas scrubber into service. If the startup oil is recirculated,
stop the circulation and begin flow to tankage. Typically this will be to off-spec storage
until laboratory analyses indicate the product meets design specifications
ii) Check operating conditions to ensure the design pressure, gas rates, recycle gas purity and
H2S removal specifications are being met. Adjust the operating temperature to meet
product specifications.
After on specification, LGO product will be routed to HT gas oil storage
tanks(2106FA/FB).
[Link] Sulphiding of Replacement Catalyst after Skimming and Reaction Section Start-up
In some cases, refiners have had to interrupt a run to skim off the top catalyst bed to alleviate
pressure drop problems or to replace contaminated catalyst. In these cases, new replacement
catalyst (or a layered graded bed) could be installed after the skimming. The bulk of the
catalyst is still in the sulphided state, so sulphiding is only required for the new top layers.
jj) The reactor must be dried out and purged with nitrogen, so that the oxygen level is less
than 0.5 volume percent. The temperature at the start of the procedure is maintained at
approximately 150℃ (300F) to minimize catalyst reduction.
kk) Set the high-pressure flash drum pressure controller 15-PIC-003 to 4.2 barg.
ll) Crack open the 6'' make-up hydrogen line to unit15 & 17 in unit12 and allow the
reaction section pressure to rise to 4.2 barg using the 1 1/2 inch pressurizing line.
Check the system for leaks. If the system is tight at this pressure, raise the pressure in 7
barg steps using the HP flash drum pressure, controller 15-PIC-003, each time
checking for leaks until the make-up gas mains pressure is reached.
NOTE: During start-up of unit 15, natural gas will be used for the pressure control of
1701F
nn) Pressurize the reactor to normal operating pressure (unless limited by the ductile-brittle
transition temperatures of the reactor and equipment)
oo) Prepare to start the make-up and recycle compressors, 1501J1/J2 or 1501JA1/JA2.
Commission 15-FIC-006 on recycle gas flow to charge heater 1501B. Commission 15-
PIC-003 pressure controller on the high pressure separator 1502F. Start the reactor
effluent condenser 1502C in reactor effluent line.
pp) While pressurizing the unit, start the make-up and recycle gas compressor and establish
recirculation of process gas at normal flow rate. In order to conserve H2S the recycle
gas scrubber should be by-passed or the amine recirculation stopped during the
sulphiding.
qq) Line up the recycle and make-up compressors to discharge through 1507C to the
charge heater 1501B, reactors 1551D & 1501D, through feed/effluent exchangers 1501
C1/C2/C3/C4 and 1507C, through air cooler 1502C to the high pressure flash drum
1502F, through the 6" start up line by passing the recycle gas scrubber 1502E, to the
recycle gas to drum 1507F & 1508F and back to the recycle gas compressor. The two
valves on the 6” start up line are locked open during bypassing the recycle gas scrubber
1502E.
rr) Open the block valve in feed line 6"-P-15-105-0-GA02 and start to feed the reaction
section through the furnace by increasing the set point of 15-FRC-001, closing
progressively 15-HCV-001 in reaction section by-pass line. Make this change gently.
Do not allow reactor temperature to drop significant1y during the change
ss) Introduce the feed at design rate. If the feed normally is a cracked stock or has cracked
components, use a straight-run feed in the same boiling range as the normal feed or the
straight-run components of the blend. The start-up feed must contain enough sulphur,
above 0.5 weight percent, to make this procedure effective
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tt) After stabilizing of flows, temperatures and pressures in the unit, the start-up oil can be
recirculated from the stripper if desired. This reduces the quantity of startup oil needed
and may reduce off-specification material produced. Startup oil recycle should not be
done through storage tanks because the unstripped startup oil may contain H2S which
may accumulate in the storage tank.
uu) If the new catalyst has been ex-situ presulphided, increase the inlet temperature
gradually, 10C/hr (15F/hr), until the exothermal begins. It is expected that at a
reactor inlet temperature of 150-180C (300-350 F) the conversion of the sulfur on the
ex-situ presulphided catalyst will start and a reactor exothermal will develop. When the
exothermal starts, pause the heat-up until the exothermal has stabilized
vv) If pressure was limited by ductile-brittle transition temperature, increase the pressure to
design level when all reactor wall temperatures exceed the transition temperature.
Minimize the recycle gas bleed to conserve H2S.
ww) Water is formed from the sulphiding reactions. Check the high-pressure separator,
1502F at regular intervals for water accumulation and drain if necessary
xx) Increase the reactor, 1551D inlet temperature at 30C/hr (50F/hr) until the
desulphurization reactions begin and an exothermal develops. Hold the inlet
temperature as needed to maintain the exothermal for a minimum of 2 hours.
yy) After the 2-hour hold, increase the inlet temperature to 350C (660F) at 30C/hr
(50F/hr).
zz) Hold the inlet temperature at 350C (660F) for 4 hours. The sulphiding of the replaced
catalyst is then considered completed.
aaa) Lower the reactor inlet temperature at a rate of 30C/hr (50F/hr) to the temperature
specified as the start-of-run temperature.
bbb) Start normal straight-run feed (90wt% hot feed from unit 11 and 10wt% cold feed
from stroage) to the unit at design rate. 10wt% cold feed is fed after removing water by
feed coalescer 1503L and the cold-feed flow-rate is controlled by 15-FV-076. Start
amine circulation and put the recycle gas scrubber into service. Also commission the
amine regenerator. If the startup oil is recirculated, stop the circulation and begin flow
to tankage. Typically this will be to off-spec storage until laboratory analyses indicate
the product meets design specifications.
ccc) Check operating conditions to ensure the design pressure, gas rates, recycle gas purity
and H2S adsorption specifications are being met. Adjust the operating temperature to
meet the product specifications.
1 After on specification, LGO product will be routed to HT gas oil storage
tanks(2106FA/FB).
ddd) At this step oil is flowing through the stripping section supplied from 1503F of LP
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eee) Start the reboiler 1502B according manufacturer's instructions and bring the
temperatures to operating conditions.
Note: The drying out of the furnace can be performed at this moment if not already
done.
fff) When a normal working liquid level is established in the stripper overhead drum
1504F, start the product stripper reflux pump 1505J/JA and commission the reflux flow
controller 15-FIC-021, the level controller 15-LIC-011 and the pressure controller 15-
PIC-005. The product stripper off-gas compressor 1502J/JA is to be started and the
start-up fuel gas supply can be shut-off.
ggg) Commission the compressed gas K.O. drum 1506F level controller 15-LIC-016 and
establish a normal working level in the drum, transferring excess liquid hydrocarbon to
the Unit11. If Unit11 is shutdown, excess liquid is transferred to the Unit61.
hhh) Sample the desulphurised product for quality and route product to desulphurised
storage 2106FA/FB when on specification.
This section is a start-up following a normal shutdown, were no changes have been made to
the state of the catalyst.
4) The high-pressure section is purged with nitrogen, so that the oxygen level is less than
0.5 volume percent. Keep the reactor inlet temperatures below 150C (300F) to
minimize catalyst reduction.
5) Set the high pressure separator 1502F pressure controller 15-PIC-003 to 4.2 barg. Crack
open the 6'' make-up hydrogen line to unit15 & 17 in unit12 and allow the reaction
section pressure to rise to 4.2 barg using the 1 1/2 inch pressurizing line. Check the
system for leaks. If the system is tight at this pressure, raise the pressure in 7 barg steps
using the HP flash drum pressure, controller 15-PIC-003, each time checking for leaks
until the make-up gas mains pressure is reached. Open fully the make-up gas valve in
unit12.
NOTE: During start-up of unit 15, natural gas will be used for the pressure control of
1701F.
6) Pressurize the reactor to normal operating pressure (unless limited by the ductile-brittle
transition temperatures of the reactor and equipment).
7) Prepare to start the make-up gas compressor 1501J1/J2 and recycle gas compressor
1501JA1/JA2. Commission 15-FIC-006 on recycle gas flow to charge heater 1501B.
Commission 15-PIC-003 pressure controller on the high pressure separator 1502F.
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8) While pressurizing the unit, start the make-up gas and recycle gas compressor according
to manufacturer’s instruction and establish recirculation of process gas at normal flow
rate. If the recycle gas is scrubbed to remove H2S, start amine circulation and put the
recycle gas amine scrubber into service.
9) Start increasing the heater outlet temperature at 30C/hr to 150C, when the right
hydrogen flow has been established.
10) When the heater outlet temperature has reached 150C, introduce the feed at 50% design
rate and raise it gradually to full design rate.
11) If pressure was limited by ductile-brittle transition temperature, increase the pressure to
design level when all reactor wall temperatures exceed the transition temperature.
12) After stabilizing of flows, temperatures and pressures in the unit, the start-up oil can be
recirculated from product fractionator if desired. This reduces the quantity of startup oil
needed and may reduce off-specification material produced. It shall however be assured
that some sulfur remain in the liquid feed to maintain the exotherm in the reactor and
prevent sulfur reduction of the catalyst. The preferred method of for checking this status
is to check that the high-pressure separator gas going to the scrubber remains above 0.05
mol% H2S. This can be checked with Drager tubes. Startup oil recycle should not be
done through storage tanks if the stripped startup oil may contain H2S, which may
accumulate in the storage tank.
13) The heater outlet temperature is raised at 30C/hr towards the desired operating
temperature. At no point in time must the heater outlet temperature be more than 100C
higher than any reactor temperature.
14) As the reactor temperatures approach the desired operating temperatures, stop any
product recirculation and start performing laboratory analysis for the desired
specifications.
15) Check operating conditions to ensure the design pressure, gas rates, recycle gas purity
and H2S removal specifications are being met. Adjust the operating temperature to meet
product specifications.
After on specification, LGO product will be routed to HT gas oil storage
tanks(2106FA/FB).
To start the unit after catalyst regeneration, follow in its entirety the procedure outlined
previously for fresh catalyst.
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The proper operation of the unit will depend on the judicious selection and control of the processing
conditions. As they are of utmost importance to the performance of the unit the following
discussion includes some of the steps that can be taken to maintain them within acceptable limits.
Each reactor inlet temperature is most easily and commonly controlled by the operator to
adjust the sulfur removed from the feed. The reactor 1501D-outlet temperature is a function
of the feed quality and cannot be easily varied except by changing the reactor inlet
temperature. The reactor 1551D-inlet temperature must always be controlled at the minimum
required to achieve the desired sulfur and/or nitrogen removal. Temperatures above this
minimum will only lead to higher rates of coke formation and reduced processing periods.
During the course of an operating cycle, the temperature required to obtain the desired
product quality will increase as a result of catalyst deactivation. The gradual loss in catalyst
activity can be compensated for by increasing reactor temperatures up to a limit of about
(428℃) maximum bed temperature, above which coke formation becomes very rapid and
little improvement in performance is obtained. Note that this temperature is the highest
temperature in the catalyst bed and is not necessarily the outlet temperature. The design
temperatures of the reactor and charge heater will also determine the maximum allowable
operating values. The temperature rise across the reactors must be monitored continuously in
order to ensure that the design limitation of the unit is not exceeded. This can be especially
important when changing feed stocks since olefin saturation results in considerably higher
heats of reaction.
The first reactor inlet temperature is controlled by 15-TIC-010 acting on the rate of fuel to the
reactor charge heater 1501B through 15-HS-005 which selects either fuel gas or fuel oil as
leading fuel, the remaining fuel being manually adjusted by 15-HIC-005. The second reactor
inlet temperature is controlled by 15-TV-016. Special care should be taken when operating
these devices as misoperation could lead to temperature upsets thus leading to coke formation
or improper desulphurization.
Reactor Temperature, oC
a The reactors are operated with equal bed outlet temperatures by adjustment of the quench
temperature setpoint
b Average bed temperature is weighted by catalyst volume and temperature profile in the
catalyst bed.
c The recycle gas hydrogen content has been calculated by simulation based on the yields and
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The amount of catalyst loaded into the reactors as well as other design parameters are based
on the quantity and quality of feedstock the unit is designed to process. While minor changes
in feed type and charge rate can be tolerated, wide variations should be avoided since they
will tend to reduce the useful life of the catalyst.
An increase in the charge rate will require higher reactor temperature to achieve a constant
desulphurization, as well as higher recycle gas rate to maintain a constant ratio of H2 to
hydrocarbon. The increased reactor temperatures will also lead to a fester rate of coke
formation which will reduce the period between regenerations. The reduced feed rate may
lead to bed flow distribution through the catalyst, such that higher temperatures will be
required to obtain good product quality. In order to minimize the effect of variations in charge
rate, it should be made common practice to reduce the reactor temperature before lowering
the feed rate, and conversely, to increase the feed rate before raising the reactor temperature.
The feed consists of 10wt% cold feed from Tank through 1503L and 90wt% hot feed from
Unit11.
The gas oil feed rate is controlled by 15-FIC-001 acting through a bias control on the flow
control valves 15-FV-001A/B thus ensuring an equal split between the two passes of the
heater l501B.
Its distillation range and API gravity best indicate the type of feed being processed. An
increase in the end point of the feed wil1 make sulfur and nitrogen removal more difficult,
thus requiring higher reactor temperatures which, in turn, accelerate coke formation. Coke
deposition is also accelerated by the fact that heavier feed contains more of the precursors that
favor coke formation.
In addition to the above, high boiling fractions also contain increased quantities of metals
which lead not only to higher reactor pressure drop, but also to rapid catalyst deactivation as
wel1. It must be remembered that regeneration will not restore the activity of a catalyst that
has been poisoned by excessive quantities of metals. Thus, it is seen that processing higher
than design end point feeds will, at best, reduce the length of the operating cycle, and under
extreme conditions, may lead to an irrecoverable loss of catalyst activity. Therefore, every
effort must be made to maintain the end point of the feed within the design limits by operating
the crude and other units such that an acceptable feed stock is obtained. Storage tanks used for
the accumulation of feed to the unit must be gas blanketed in order to minimize the formation
of coke producing materials.
10.1.4 Pressure
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The reactor section operating pressure is 15-PIC-003 controlled by the pressure maintained at
the high-pressure separator. This pressure, multiplied by the H2 purity of the recycle gas,
determines the partial pressure of H2 in the reactor. The hydrogen partial pressure required
for the operation of the unit is chosen based on the degree of sulfur (or nitrogen) removal that
most be achieved and is an economic optimum that balances initial investment and operating
costs against catalyst life. The operating pressure (i.e. the high pressure separator pressure)
most be held constant at the design value for the following reasons :
i) While higher than design operating-pressure directionally favors catalyst life and may
result in somewhat better catalyst activity, such operation would be detrimental since the
equipment (heaters, reactors, compressors, exchangers, safety valves, etc.,) has been
designed based on a fixed separator pressure. An increase in the separator pressure wil1
lead to accelerated wear on the equipment, and in extreme cases could result in costly and
dangerous equipment failures.
j) A reduction of the operating pressure below the design level will have a negative effect
on the activity of the catalyst and will accelerate catalyst deactivation due to coke
formation
These two terms are interchangeable since at a given system pressure the purity of the recycle
gas will determine the partial pressure of hydrogen in the reactor. At reduced hydrogen
purities (i.e. partial pressures) the reactions are not effectively completed and there is a greater
tendency for coke to be formed in the hydrogen deficient atmosphere. This is especially more
so as a result of the plant operator's reaction to raise the reactor temperatures to compensate
for the lower catalyst activity caused by reduced H2 purity. Catalyst deactivation rate can be
kept to a minimum by maintaining the recycle gas hydrogen purity as high as possible.
The large quantity of gas recycled from the high-pressure separator to the reactor serves the
following purposes :
k) Provides the excess hydrogen needed to ensure that the reactions are carried to
completion.
l) Absorbs some of the heat of reaction, thereby minimizing the catalyst bed temperatures.
m) Helps hold down charge heater and combined feed exchanger tube wall temperatures by
increasing the flow through the equipment, and the excess H2 prevents the formation of
coke as the charge is heated to reaction temperature.
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The charge heaters combined feed exchangers, compressors, etc., have been designed to allow
for the circulation of a minimum ratio of hydrogen to hydrocarbon charge. This ratio,
expressed as standard cubic meter of H2 per cubic meter of feed (Nm3/M3) is on the order of
209Nm3/M3. The H2/HC ratio is an economic optimum, balancing initial investment against
catalyst life.
If the unit is operated at less than the design H2/HC ratio, higher catalyst bed and charge
heater tube wall temperatures will result, leading to accelerated coke formation and
equipment wear. A complete loss of recycle gas can result in very serious damage to the
catalyst and equipment, therefore, a safety device is incorporated in all units to shut down the
charge heaters whenever the recycle gas flow drops to a predetermined minimum. Other steps
to be taken during such as emergency are more completely described in the Emergency
Procedures section of this manual.
As the amount of gas that can be circulated is a function of the compression ratio, a gradual
reduction in recycle gas rate will be observed during the course of an operating period as a
result of higher reactor system pressure drop. Such a reduction in the recycle gas rate is
acceptable as long as the calculated H2/HC ratio does not fall below the minimum value.
When it is no longer possible to maintain the minimum H2/HC ratio, the catalyst must be
regenerated and screened in order to reduce the reactor pressure drop. In all cases that result
in less than design H2/HC ratio due to pressure drop or mechanical difficulties, the raw oil
charge rate must be lowered in order to obtain the required H2/HC ratio. In the event of a
complete loss of recycle gas, immediate remedial action must be taken to protect the catalyst:
and equipment, as described in the Emergency Procedures section of this manual.
The effective completion of the hydrogenation reactions occurring over the catalyst requires
that a certain quantity of hydrogen be present at a minimum partial pressure. As noted
previously, both the quantity (H2/HC) and partial pressure are dependent upon the hydrogen
content, i.e. purity, of the recycle gas. Practical considerations, such as the cost of
compression, catalyst life, etc., limit the purity of the recycle gas to a normal value usually in
the range of 82 to 85 mol%. Lower hydrogen purities are detrimental to the performance of
the unit since higher temperatures must be used to achieve the desired product quality. The
purity of the recycle gas is determined by the following factors :
In most instances, the makeup gas H2 purity cannot be easily manipulated since it is fixed by
the operation of the platformer. The light hydrocarbons present in the recycle gas enter the
system with the make-up gas in addition to those being formed in the reactor, and must be
vented from the high pressure separator to prevent their accumulation in the recycle gas This
can be achieved by increasing the make-up gas rate thus venting more gas through 15-PIC-
003.
The H2S formed in the reactors can reach equilibrium values as high as 5-mol% in the recycle
gas. This concentration of H2S has a depressing effect on the activity of the catalyst,
therefore, it is desirable to remove the H2S from the recycle gas. The removal of H2S is
performed in a scrubber 1502E where the recycle gas in contacted with a monoethanolamine
(MEA) solution. In this manner, the H2S content of the recycle gas can be reduced to the part
per million range. The design flow of lean amine to 1502 E is 28543kg/hr or 28.6m2/hr at 15-
FIC-017.
10.1.9 Contaminants
The sulfur and nitrogen found in the feed can be considered contaminants to the extent that
they produce hydrogen sulfide and ammonia which can react to form ammonium sulfide. The
water injected into the reactor effluent dissolves the ammonium sulfide and prevents
exchanger fouling. Organic nitrogen in the feed, if present in amounts higher than expected,
will require higher reactor temperatures for processing, and will lead to a reduction in catalyst
life.
Alkaline metals are permanent catalyst poisons and must be completely excluded. Solid
material, such as corrosion products, wi11 lead to rapid fouling of the catalyst bed if allowed
to enter the reactor.
During the ignition and the gradual firing rate increase of the burners, check the outlet
temperature of the coils. If it does not rise, shut-off the heat, and look for the reason,
Increase progressively the heat, watching the flue gas temperature at the bridge wall. For
information, the temperature rise rate can be about 50℃/hr at this control point.
The firing rate must be brought up gradually. As a matter of fact, during this period, the
heat must be supplied both to the charge and to the furnace taken as a whole. A too fast
increase of the firing rate can cause an over heating of the tubes, and of the fluid to be
treated and crack the refractories.
In case of fluid circulation shut down, shut off immediately the burners. However, the
furnaces are provided with safety devices which shut off the fuels automatically in case
of loss of product through the coils.
Up to the half of the normal burners heat liberation, it will be better to adjust manually
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the burners. Then, it will be possible to operate with the automatic control-valve taking
care not to increase suddenly the fluid during the operation.
When the outlet temperature of the charge reaches its normal operating level, the swing
to automatic may be attempted.
Adjust the draft and excess air accordingly by means of the stack damper and burners
registers.
Combustion conditions:
Draft
7
The draft must be adjusted by means of the damper located in the flue gas outlet of the
furnace.
The draft should be periodically checked by means of draft gauges which are fitted on the
furnace.
A minimum draft should be obtained, without leaving the furnace under positive pressure.
Excess Air
A checking of the excess air must be carried out, The excess air adjustment depends on the
burners air registers opening.
Flames Aspect
The various burners should have flames as uniform in length and size as possible.
Under no circumstances should the flames be permitted to touch tubes or furnace walls.
Tubular Coils
The regular and periodical control of the combustion minimizes the external and internal
coating of the tubular coils : coke, ash, etc
Flame impingement on tube surface decreases their service life duration and can cause serious
damage.
At regular intervals and particularly after any change in load, make sure that the flame
impingement does not occur, and that no local hot spots are visible on the furnace walls.
10.3.3 After-burning
When the furnace is operating with insufficient combustion air, the flue gases are growing in
carbon monoxide and an after-burning may occur at the bottom or at the top of the stack,
according to the carbon monoxide content.
An after-burning causes a rapid increase in flue gas temperature in the stack, and deterioration
of the stack and of the structural steel may occur.
An after-burning is due to a bed combustion control, and to a lack of flue gas analysis.
A reduction or a shut down of the circulation in the tubular coils causes immediately an over
heating of the tubes and requires an immediate reduction of the heating or the emergency shut
down of the furnace.
Burners must be shut off when the fuel pressure reaches a value less than 10 % approximately
of the minimum operating value.
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In case of a complete failure independent of the unit operation, close the burners manual
valves, reduce the draft and close the combustion air registers, in order to avoid a quick
cooling of the furnace.
When it is possible to light burners again, proceed as indicated in the section describing
furnace start-up.
The gas burners may be extinguished for the following main reasons :
When the draft is too high,
When the combustion air is not correctly adjusted.
When the burners operate at too high or too low pressure, compared with those for
which they are designed,
When there are condensates in the gas feed pipe, particularly at high operating rate.
Consequently, the gas circuit must be carefully preheated and purged
When the firing rate is too rapidly reduced, without adjusting the draft and excess
air accordingly
Insufficient combustion air. The flame smokes, is irregular and tends to be unstable.
The combustion air registers must be properly adjusted,
Excessive firing: at a high rate, the flame is long and irregular. Reduce the firing
rate,
Obstruction of the burner orifices : the gas manifold must be dismantled and the
obstructed orifices cleaned,
Draft excess: when the draft is too high, flames begin to lift-off, relight and cause
smell explosions.
Draft failure: when there is no draft, the furnace begins to smoke and flames tend to
come out through the peepholes and registers. Reduce the firing rate and adjust
properly the stack damper.
10.3.7 Incidents With Fuel Oil Burners
s) Burners extinction
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Check that the oil tips are correctly positioned and, if necessary, adjust the all gun
higher.
Remove periodically all burners and clean them, after complete dismantling. The
frequency of this cleaning should depend on the fuel used.
During unit shut down, check the dimensions of the orifices of the oil tips and
atomizers. In addition :
The normal destinations and alternate destinations of off-spec products in case of start-up,
shut down or maloperation of the unit are listed below:
A normal shutdown a controlled cooling down and removal of the feed from the unit. The shut-
down can be a short term occurrence midway through the catalyst’s life cycle due to maintenance
requirements or due to shut-down of upstream or downstream units. In this case, it is expected that
the reactor will be restarted after the shutdown. A long-term shutdown will come at the end of the
catalyst life, cycle. In this case, the catalyst will either be replaced or regenerated.
1) Warn all units which may be affected, that shutdown of the unit is imminent (crude unit,
platformer, amine regeneration and off-sites).
2) Reduce heat input to the unit to cool the reactor at a maximum of 30C/hr (50F/hr).
3) Switch product run-down to off-spec storage. Gradually decrease feed rate to nominally 50
percent of design. If processing a cracked stock. Remove the cracked portions of the blend first.
Use suitable flushing oil to purge cracked material or high pour point gas oil from the system.
If the unit is fed from the crude unit do not close the battery limit block valve. Close the valve
at the inlet of the feed surge drum and reroute the raw gas oil from the crude unit to the inlet of
the stripper bottoms cooler 1504C/C1.
Caution: Do not forget to route the product stripper bottoms to slop or intermediate storage to
avoid pollution of the treated storage before carrying out the above-mentioned operation. Valve
15-LV-010 will have to be manually open to allow raw product to be sent to storage. As the
stripper reboiler 1502B is still in operation care will be taken not to lose the stripper bottoms
pump suction by closing the block valve on the 6" bottoms product to storage at the outlet of
the feed/bottoms exchanger 1503C1/C3.
u) Continue cooling with treat gas and flushing oil until the maximum reactor temperature
reach 175C (350F). If not involved in the shutdown maintenance, the reactor does not
need to be further cooled. The flushing oil can be put on recycle or stopped. Continue
recycle gas circulation.
v) Maintain the amine circulation and keep the amine regenerator hot unless the shutdown
will be for an extended period.
y) Cool the reactor at 30C/hr (50F/hr) with treat gas and flushing oil until the temperatures
reach 230C (450F).
z) When the reactor inlet temperature reaches 230C (450F), remove flushing oil
completely and shut down the amine system.
aa) Circulate recycle gas at the maximum rate and increase the reactor inlet temperature to
400C (750F). Hold the reactor inlet temperature to 400C (750F) for 2 hours.
bb) Begin cooling the reactor at 30C/hr (50F/hr) with recycle gas. Reduce the pressure
appropriately in the unit before cooling below the ductile-brittle transition temperature.
dd) Drain the feed surge drum 1501F, and then shut down the charge pump 1503J/JA (in
good time) just before it loses suction.
ff) Drain the reactor effluent separator 1502F into the stripper feed flash drum 1503F. When
no more liquid collects close the contro1 valve 15-FV-013.
gg) The hydrogen make-up must be shut off at battery limit, the make-up compressor
cylinder unloaded, and the cylinder by-pass opened.
hh) Open the 6" recycle gas scrubber by pass line and block the scrubber inlet.
Stop the MEA flow to the scrubber. Block the MEA inlet and outlet keeping a liquid seal
at the bottom
jj) When the reactor temperature is about 218℃, shut down the charge heater 1501B, shut
down the make-up and recycle compressor, and close suction and discharge valves.
kk) Pressure any remaining liquid in the reactor effluent separator 1502F and the LP flash
drum 1503F to the product stripper 1501E. Close block valve.
ll) Depressurize the reactor to flare via the depressing valve, 15-XV-030.
mm) If equipment is not to be opened, care must be taken to maintain a positive pressure
of about 0.35 barg.
nn) If equipment is to be opened, it should be drained, purged with nitrogen and blinded off
during shut down.
6) When the reactor feed is cut out, start reducing the firing of the stripper reboiler furnace. Once
the reactor effluent separator is drained, pressure the liquid contents of the stripper feed flash
1503F drum into the product stripper 1501E
7) When the stripper feed stops, cut out the firing of the stripper reboiler furnace 1502B. The
overheads will reduce rapidly in volume and the amount of off-gas leaving the product stripper
overhead drum will also diminish until the product stripper off-gas compressor 1502J has to be
shut down.
8) Stop the corrosion inhibitor injection. Shut down 1502LJ. However if units 12 and 14 are
running, the HC release drum 1602F may produce low pressure gas and depending upon the
amount, the stripper off-gas compressor 1502J/JA may have to be kept on line or acid gas may
be evacuated to the acid gas flare through 15-PV-005A.
9) When no more liquid collects in the product stripper overhead drum, 1504F, empty the drum
into the tower and then shut down the product stripper reflux pump 1505J/JA.
10) Shut off the gasoline to crude unit at battery limit then pressure out any liquid in the
compressed gas K.O. drum 1506F to 1504F.
11) When the stripper bottoms temperature is down to about 200℃, empty the product stripper to
slop or intermediate storage by manually opening the block valve on the 6" stripper bottom
line.
12) Block off the reactor system purge gas at the 15-PIC-003 control valve and close the valve in
the 6" gas scrubber by-pass line.
Depressurize the compressed gas K.O. drum 1506 F and the stripper feed flash drum 1503F
using the 1" vent to flare making sure that the battery limit valve is closed.
13) Depressurize the feed surge drum 1501F to flare via 15-PV-001B.
14) If towers or drums are not being opened, care must be taken to maintain a positive pressure of
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about 0.3 barg on the system using fuel gas via the start up connection.
15) If towers or drums are to be opened, they should be drained, steamed out, washed and blinded.
Reduce the heating gradually to lower temperature of the treated fluid following the
instructions of the operating manual and reduce the flue gas temperature which leaves the
radiant zone or arch by about 50℃/hr.
Keep a small steam flow for a few minutes to avoid oxidation of the burners tips,
Do not introduce too much purge steam too rapidly, otherwise burners go out too quickly
and unburnt fuel is ejected into the furnace,
If another start up is forecast immediately, close the combustion air registers and stack
damper, so that the furnace does not cool too rapidly,
Stop the circulation in the tubular coils.
Otherwise, ventilate the furnace by leaving the burners, registers and the stack damper wide
open.
It is advisable, when the stoppage is foreseeable, to introduce a drying agent into the fire
box.
After this operation, see part AFTER ASSEMBLY, refractories will remain dry and no
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At the furnace start up the temperature rise at the arch must exceed 27℃/hr with a
leveling off at 150℃ during about 12 hours.
Objective: Maintain hydrogen pressure to minimize cokes formation and cool the catalyst with
recycles gas.
The loss of normal feedstock may have different causes depending on the way the unit is fed.
Possibilities include:
17) Shut-down of the feed pump from intermediate storage if the crude unit is not on line,
Since the charge heater transfer temperatures will drop due to heater shutdown initiated through 15-
FALL-002, proceed as follows
d) Shut down the charge pump 1503J/JA if the failure is from an outside source.
e) Maintain water injection to the reactor effluent at the same rate as before the emergency. Take
special care to prevent water from entering the stripper.
g) Cool the catalyst bed to at least 200℃ with recycle gas before charging oil again to the reaction
section.
1501J/JA recycle and make-up compressors are provided with safety devices :
In case of recycle and make-up compressor failure, the following action is to be taken:
The charge heater 1501B will trip automatically through the safety device 15-FALL-007 low
recycle gas flow, then :
b) Put the spare compressor on line as quickly as possible after the fault has been cleared, if it is a
common fault, or immediately if it is a specific compressor fault.
d) Once the compressor has been restarted, cool the catalyst bed to at least 200℃ before restarting
the charge pump 1503J.
In the event of a failure of the hydrogen-rich make-up gas, due to shut-down of gas platformer for
example, and before the recycle and make-up compressor is tripped through low pressure make-up
compressor suction safety mechanism, cut the feed rate down to the minimum in order to reduce
hydrogen consumption and drop of reaction section pressure (to minimize coke formation). If the
failure is prolonged, stop the liquid feed and shut down the unit in the normal manner.
This is a serious situation which requires immediate attention. It can be brought about by equipment
or utility failures which result in a significant reduction in space velocity (this results in a reduction
of gas capability to remove the heat of reaction from catalyst), thereby overheating during a startup,
or it can even occur during normal operation. The period during startup before the catalyst has been
thoroughly sulphurated is perhaps the most critical time when very special care should be taken to
control the reactor temperatures, as outlined in the startup procedure.
During a temperature runaway, highly exothermic demethylation reactions can take place. It is not
necessary, however, to have demethylation occurring in order to have a temperature runaway.
When there is a significant increase in residence time of feedstock on the catalyst, and especially
when this is coupled with the loss or reduction of a large heat removal stream such as recycle gas,
excessive cracking reactions can take place, resulting in severe overheating. Catalyst temperatures
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can rise rapidly to well above thc reactor design temperature in such a situation, even though the
cracking has not progressed to the point of demethylation.
In order to sustain a temperature runaway, both hydrocarbons and hydrogen must be available.
Therefore, removing one or the other will cause the reactions to stop. The quickest way to achieve
this, and still maintain hydrogen pressure to minimize coke formation, is to remove the liquid
hydrocarbon feed from the reaction by stopping all feed, sweeping the catalyst with recycle gas
circulation, and providing maximum cooling to the catalyst. If the temperature rise cannot he
controlled, however, then the system should be rapidly depressurized to suppress the reactions and
to minimize the danger of damage to the reactor and other equipment.
Proceed as follows :
e) Stop the liquid feed by shutting down and blocking in the feed pump, and shut down the reactor
charge heater immediately.
g) Maximize cooling on air-fin coolers in the recycle gas circuit to provide the maximum amount
of cooling possible to the catalyst.
h) Maintain water injection to the reactor effluent at the same rate as before the emergency.
TAKE SPECIAL CARE TO PREVENT LIQUID WATER FROM ENTERING THE
STRIPPER.
Open the stack damper and all air registers to the full open position to establish the maximum
flow of cooling air through the heater fire-box.
i) Hold the system pressure at the normal level if the temperature rise in the reactor can be
brought under control. If the rate of temperature increase indicates the maximum allowable
operating temperature will be exceeded (at normal operating pressure) at any point, either on
the reactor itself or in the catalyst bed, then depressurize the reactor circuit to flare from the
recycle gas knock-out drum at a rate at least 50percent of the vessel’s design gauge pressure
within approximately 15minutes, utilizing 15-HS-030A/B. Continue depressurizing at this rate
until the plant pressure is reduced to 60 % of the normal operating pressure. Closely monitor all
catalyst and reactor outlet temperatures, and if any of these temperatures continue to rise
unchecked, then increase the depressurizing rate to the maximum possible and continue
depressurizing to as low a pressure as necessary to try to stop the temperature rise. If it appears
that any temperature point, either on the reactor itself or in the catalyst bed, will exceed the
reactor design temperature, do not stop depressurizing when the 60 % pressure level is reached,
bolt continue depressurizing at the maximum rate possible to minimize any danger of damage
to the reactor and other equipment. It should be noted that when depressurizing at accelerated
rates, it will most likely be necessary to provide maximum cooling to the reactor products
condenser to prevent overheating that exchanger. If temperatures remain high after the unit has
been depressurized, then begin purging the reactor with nitrogen at the maximum rate possible.
j) If recycle compressor operation can be maintained, continue maximum gas circulation and
make-up rate and cool all catalyst temperature points and the reactor outlets to 200℃.
k) If recycle compressor operations cannot be maintained, immediately shut down and block in all
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make-up gas compressors to cut off any additional supply of hydrogen to the reactions and to
allow for more rapid depressurizing of the system.
l) With all temperatures below 200℃, pressure the unit with make-up hydrogen.
m) If it was necessary to depressurize the unit to a very low level, necessitating shutting down the
recycle compressor, then the water injection system should be shut down also.
n) Put the recycle compressor on line and after it runs satisfactorily for one hour without difficulty
and all catalyst temperatures remain below 200℃, load the make-up compressor and pressure
to normal operating pressure with hydrogen.
oo) 415V half-board temporary failure. BUS BAR A or BUS BAR B and E.
After a delay of about three seconds due to automatic transfer, power will be again
available and the equipment fed from this helfboard and included in the reaccelerating
group will be automatically restarted.
In case of complete loss of power, the emergency generator will start and after a delay
of about 60 to 90 seconds the power will be restored to the emergency board. Motors
connected to the emergency board will then be reaccelerated following their
reaccelerating group. Motors with no reacceleration group will have to be restarted
manually. The pattern is as follows :
DELAYS
Bus Bar A B E Step (SECONDS) ROLE
TEMP. EM GEN
1502C 3 25 85/115 Reactor effluents cooler
1505C 1 15 75/105 Stripper overhead air cooler
1501
1 15 75/105 1505 J Oil pump
J1/J2 J2M
1501
1 15 1501 JA all pump
JA1/JA2 J2M
1505J 2 20 80/110 Product stripper reflux pump
1505JA 2 20 80/110 Product stripper reflux pump
Product stripper buttons pump
1506J 1 15
Product stripper buttons pump
1506JA 1 15
Bottoms product air cooler
1504C/C1A 1 15
In normal operation the emergency board is coupled with BUS BAR B. As the feed pumps
1503J/JA and the recycle and make-up compressors 1501J/JA are fed from the 3.3 kV board,
these equipments will not shut down in case of 415V medium voltage board failure. The charge
heater will keep running. On temporary failure, the effluent reactor cooler 1502C will
automatically restart after about 25 seconds. It might be safer to cut the charge rate down to 50%
to avoid overheating the HP flash drum 1502F. The stripper reboiler should not trip as the low
flow safety 15-FALL-022 cut off is fitted with a temporization and the spare pump starts
automatically through 15-FALL-023. The stripper overhead cooler 1505C will restart after 15
seconds and the reflux pump 1505J will restart after 20 seconds. The bottoms product air cooler
1504C will have to be restarted immediately and product routed to intermediate storage to avoid
pol1ution of the treated product storage tank.
In all cases when cutting back the charge rate to the reaction section, and if the crude unit is
running, the excess raw gas oil from U11 must be routed to 1504C and the blend raw gas oil
plus bottoms product sent to intermediate storage or slop.
In addition of the equipment above mentioned, the recycle and make-up gas compressor
1505J1/JA1/J2/JA2 and the charge pump 1503J/JA will trip.
On a full electrical failure the fire in the furnaces should be cut immediately, the unit shut down
as far as possible in the usual way, and the vessels left with liquid levels ready to he restarted
when the power returns.
The steam header pressure to Unit15 is indicated in the control room by 15-PI-117. A steam
failure will lead to loss of atomizing steam and snuffing steam for the furnaces 1501B and
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1502B.
To avoid damage to the rotating machinery it should be shut down as soon as possible unless
a temporary water supply can be made available (e.g. from hose connections).
The actions of the control valves are arranged so that a general instrument air failure will
leave the unit in a sate condition.
If possible, maintain the recycle gas circulation as long as possible while shutting down the
plant in the normal manner. A close check should be kept on the recycle loop pressure, any
excessive pressure being manually vented via the H.P. separator relief valve bypass.
The unit may be left with pressures and levels maintained in the vessels until the fault is
rectified.
In the event of a failure of the hydrogen rich make-up gas the feed rate must be cut as
necessary, probably by at least 50%. The firing must be adjusted accordingly.
If the failure is prolonged, the start-up circulation procedure should be maintained for as long
as possible and the unit then shut-down in the normal manner.
HIC/XV
15-HIC-001X 1501B Damper open
15-HIC-002X 1502B Damper open
15-XV-005 1501B Safety shut-off valve Fuel gas to main burners closed
15-XV-003 1501B Safety shut-off valve Pilot gas closed
15-XV-006 1501B Safety shut-off valve Fuel oil to main burners closed
15-XV-007 1502B Safety shut-off valve Fuel gas to main burners closed
15-XV-004 1502B Safety shut-off valve Pilot gas closed
15-XV-008 1502B Safety shut-off valve Fuel oil to main burners closed
15-XV-030 Emergency depressing valve open
PRESSURE
15-PV-001A Feed surge drum pressure control Fuel gas make-up closed
15-PV-001B Feed surge drum pressure control to flare closed
15-PV-003 HP flash drum 1502F Pressure control closed
15-PV-004 LP flash drum 1503F pressure control closed
L5 PV 05A Stripper reflux drum 1504F pressure control to flare closed
15-PV-005B Sour gas compressor 1502J/JA kick-back open
15-PV-006 Make-up gas knock-out drum 1508F pressure control during open
regeneration.
15-PV-007 1501 B F6 to main burners closed
15-PCV-024 1501 B Pilot gas control
15-PV-009 1501 B Fuel oil to main burners closed
15-PV-011 1501 B Atomizing steam open
15-PV-012 1502 B F6 to main burners closed
15-PCV-025 1502 B Pilot gas control
15-PV-014 1502 B Fuel oil to burners closed
15-PV-016 1502 B Atomizing steam open
TEMPERATURE
15-TV-016 Desulphurization Reactor 1501D temperature control open
Objective : Stop adding hydrogen and hydrocarbons to the fire in the heater box through the process
lines, purge with steam/nitrogen to the rupture to prevent air from entering the process lines and
equipment.
o) Shut down and block in all liquid feed pumps to the reactors.
p) Shut off all fuel supply and return lines to the heaters and open snuffing steam to the box.
s) Depressurize the unit to flare with 15-HS-030A/[Link] it has not already been depressurized into
the heater box.
t) After the system is depressurized, hook up steam hoses to both sides of the heater and purge
through to the rupture to prevent air from back-flowing through the rupture and forming an
explosive mixture with hydrocarbons in the system. If purging must pass through the reactor,
then the purging material should be nitrogen instead of steam.
Objective : Rapidly shut down the unit and depressurize (if necessary) to prevent further damage.
Be aware of the possibility that high temperatures could be generated rapidly in the catalyst bed,
and be prepared to take appropriate action per instructions in paragraph 4.
u) Shut down and block in the liquid feed pump to the reactors, 1503J/JA.
v) Shut off all fuel supply and return lines to heaters 1501B/1502B.
w) Unload make-up gas compressor, but maintain recycle gas compressor operation as long as
possible.
y) Shut down and block in the water injection pump after the catalyst has been cooled to 200℃,
but in any case before the recycle compressor is shut down.
In order to deal with other situations, same remote shutdown switches are provided :
Emergency shutdown switches located in the control room. These shut off all the fuels
including the pilot gas to the heaters 1501B/1502B.
17) 15-HS-007B/15-HS-008B
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These switches are located outside and at least 15m from furnace at grade. This has the
same action as 15-HS-007A/15-HS-008A above mentioned.
18) 15-HS-012A/15-HS-014A
Located in the control room. They shutdown the compressors (one switch for each
compressor) and close the associated motorized valves at the suction and discharge.
19) 15-HS-012B/15-HS-014B
These switches are located outside and at least 15m from the compressors
1501J1/JA1/J2/JA2. They shutdown the compressors (one switch for each compressor)
and close the associated motorized valves at the suction and discharge.
20) 15-HS-030A
Located in the control room. This provides a quick means for depressurizing the
reaction section if required.
21) 15-HS-030B
Located outside. This has the same action as 15-HS-030A above mentioned.
Emergency shutdowns may be caused by failures of various kinds. The action to be taken is
primarily dictated by personnel and equipment safety considerations.
However, in order to protect best the catalyst from damage, it should be kept in mind that the
catalyst may be damaged by:
aa) Hot hydrogen without hydrogen sulphide or oil: This will tend to strip sulphur from the
sulphided catalyst and at prolonged exposure to these conditions, there is a risk of reducing the
metals with to free metals with consequent permanent loss of activity.
bb) Hot oil without hydrogen: Operating with a hot oil on the catalyst without any hydrogen will
result in coke formation on the catalyst, leading to loss of catalyst activity and increased
pressure drop.
cc) Contact with water condensate: Exposing the catalyst to liquid water or high water vapor
concentrations at elevated temperatures can result in loss of catalyst strength. Therefore, any
slugs of water into the reactor inlet streams must be avoided.
dd) Back-flow: Back-flow through the reactor should be avoided due to the risk of lifting of the
catalyst bed and support.
With the above in mind, the following emergency procedures should be observed.
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ee) If the charge pump shuts down, the treat gas will continue. However, the heater will not
respond quickly to the sudden loss in flow. To prevent overheating, the heater should
automatically cut back to minimum fires or shut off the fuel to the main burners. Pilots can be
kept in service to facilitate return to normal service. If the pump cannot be started within 15
minutes, continue to cool the reactor at a rate of 30C/hr (50F/hr) to 230 (450F).
Stop the amine circulation in the scrubber. The recycle gas compressor should be kept at
maximum to maximize the cooling of the reactor.
ff) If the recycle gas compressor shuts down, the oil will stagnate in the reactor. The feed pump
should automatically shut down, the heater should cut back to minimum fires or shut off the
fuel to the main burners. The make-up gas compressor should be kept at maximum to sweep oil
from the heater tubes and catalyst.
gg) If the make-up gas compressor shuts down, the pressure will decay as the hydrogen is
consumed. If the make-up gas compressor cannot be restarted immediately, the feed should be
removed and the unit cooled down as described for normal short-term shutdown.
hh) If the amine supply is stopped, the H2S concentration in the recycle gas will increase and
inhibit catalyst activity. The unit can continue to operate for a short time although the product
may be off spec. Maximize recycle gas purge until limited by the make-up gas compressors’
ability to maintain loop pressure. Decrease feed rate to reduce the off spec. material and reduce
sulphur input. If the amine system cannot be restarted reasonably quickly and the shut down the
unit as described above for normal short-term shutdown.
ii) If the wash water injection pump shuts down, operations can continue but be aware that
ammonium salts may start to precipitate in the colder heat exchangers. Ammonia will be
absorbed in the amine solution and that could potentially upset a downstream sulphur plant.
The unit is equipped with an emergency depressurizing system and the unit is depressurized to meet
as following:
To drop pressure at a rate equivalent to 7 bar/min (100 psi/min) tar the first minute.
The emergency depressurizing system is connected to the normal flare and used to rapidly drop the
pressure in the unit in case of fire or other major emergency.
In case of significant disastrous situation, initiate unit shutdown by pushing the emergency
shutdown switch(15-HS-030A or 15-HS-030B), depend upon the desires of the supervisor.
Otherwise, do the following if possible.
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Notes: 1. In addition to the above, saturated high press. Steam is produced from sulfur unit.
2. LLP steam will be available only within 47/49 unit area.
13.1.3 Steam Condensate
Process Area
Temperature Two Phase
System Battery Limit
(C) (Unpumped) or
Identification Pressure (barg)
All Liquid (Pumped)
Normal Design Normal Design
At Condensate Tanks Inlet 1.0 9.3 65 to 100 130 Unpumped if possible.
To Users(for LP steam desuperheaters) 14.2 18.0 65 to 90 120 Pumped
To Users(for HP steam desuperheaters) 59.0 79.0 65 to 90 120 Pumped
To Users(for process water) 4.5 12.0 60 100 Pumped
Notes:
Notes: 1. The figures in parenthesis are required maximums in accordance with BS 2486 :
1978.
2. N.A : Not Applicable.
3. Above figures are estimated considering expected make up ratio of Dealkalized
water with Recovered Steam Condensate to produce Boiler Feed Water based on
Steam Balance. For LP/MP/HP Boilers, estimated make up ratio of Dealkalized
water are 100 / 0 / 22 % respectively and 5 % of blow down rate was applied.
Liquid Fuel
Data:
Maximum : - -
Normal : 120 50
Minimum : - -
Design : 150 150
Flow Rate (m3/hr) As required As required
Notes: 1. Expected Composition changes are due to blending and Refinery feed cases.
Gaseous Fuel
Properties:
H2 O - 1.15 0.1 -
O2 - - - -
N2 4.45 3.08 0.67 0.2~0.8
CO - - - -
CO2 2.19 - 0.33 0.1~0.4
H2 S 0.9 <0.005 0.14 0.01~0.1
H2 - 50.56 76.77 55~65
C1 87.86 14.13 14.88 6~11
C2= 4.5 4.25 - 6~10
C2 - 11.63 2.68 -
C3= 0.09 0.62 - 15~20
C3 - 9.69 1.95 -
C4= 0.01 0.1 - -
iC4 - 1.77 0.6 1~3
NC4 - 2.17 1.8 1~3
C5= - - - -
iC5 - 0.47 0.04 0.1~0.9
nC5 - 0.11 0.02 0.1~0.9
C6+ - 0.28 0.04 0.2~0.4
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Notes :
1. Case 1/2/3 shall be applied to heater design of the new condensate complex (unit 47/61/62/63
/64/65).
2. Case 1/2 shall be applied to heater design of the all other units (Refinery 1/2/RFCC complex)
3. Normal Existing Refinery Fuel Gas : Information only for vendor to evaluate the existing burner
s which were designed based on this fuel gas for the revamping unit heaters.
4. Case 1 is identical to Natural Gas.
Properties:
Case 1 Case 2 Case 3
Revamped Refinery Fuel Gas for Normal
Data Supplementary Fuel Gas Condensate Unit Existing Refinery
Fuel Gas Fuel Gas
Data Conditions
Flow Temperature (C)
Normal 40
Design 70
Flowing Pressure (barg)
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Normal 7.0
Design 10.0
Dew point = -5C (maximum) at 7.0 barg.
Plant Air
Data Conditions
Flow Temperature (C)
Normal 40
Design 70
Flowing Pressure (barg)
Normal 7.0
Design 10.0
Plant Air to be Oil free and Liquid water free
13.1.8 Nitrogen
Raw water delivered by the local authority is used as fire water, potable water, service water,
make-up for cooling water and for water treatment plant.
Normal Design
Pressure (barg) 3.1 to 4.5 7.0
Temperature (C) 30 to 43 75
Characteristics are:
Cations
(ppm wt)
Na 25 to 40
K 0.4 to 2
Ca 25 to 50
Mg 2 to 10
Fe 0.2 to 0.4
Anions
(ppm wt)
HCO3 80 to 110
SO4 4 to 6
CL 40 to 70
CO3 0 to 10
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NO3 0 to 0.1
NO2 -
SiO2 0.1 to 0.4
Chlorine 0 to 0.2
Phosphate 0.3 to 0.4
This is treated raw water, the feed to LP/MP Dealkalizer to remove hardness and alkalinity via
treatment plant.
Normal Design
Pressure (barg) 4.8 7.5
Temperature (C) 30 to 43 75
Characteristics are:
Dealkalized Water
This is raw water treated to remove TDS and alkalinity via a dealkalization unit. The only users
are as make-up to the BFW systems. BFW is expected to be a mixture of steam condensate and
dealkalized water.
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Normal Design
Pressure (barg) 3.3 5.6
Temperature (C) 30 to 43 75
Characteristics
Cl : 40 - 70
Oil : non detectable
pH : 8.5 - 9.5
Quality and conditions (including those at battery limit) are the same as raw water.
Conditions are:
Normal Design
Pressure (barg) 7 to 12 16
Temperature (C) 30 to 43 75
Conditions are:
Normal Design
Pressure (barg) 7 to 12 16
Temperature (C) 30 to 43 75
The cooling tower make up water will consist of a mixture of the two following streams:
uu) Treated Waste Water from EDR Unit in the Waste Water Treatment Plant.
The quality of this water will be similar to Raw Water except TDS, less than 210 ppm.
Refer to Engineering Design Brief 7J48N-00-16-17-051 “Electrical Power Systems” for further
details
Electrical power for the expansion project is supplied by three 33/11kV transformer feeders,
50Hz, three phase. Voltage levels used in the Refinery are 11kV, 3.3kV and 415V.
The electrical equipment is designed for operation on the systems listed below:
240 volts, single phase, 50 Hz derived from a medium voltage (415V), three phase, four wire
50 Hz earth neutral system.
Instruments
Refer Engineering Design Brief 7J48N-00-16-63-005 “Instrument Power Systems” for further
details.
or
24V dc as appropriate.
Note that all existing instrumentation systems are to be disconnected from their present power
supply and reconnected to the appropriate new system.
Socket Outlets
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Emergency Power
vv) Existing
Emergency power supplies for the existing plants are derived from two gas turbine driven
generators, each rated at 3.3kV, 1,450kW, 0.8 PF with facilities for automatic start in the
event of grid supply failure.
xx) LP Steam
Reactor Charge Furnace (1501B)
: Snuffing steam at startup and shutdown to purge out the furnace or for the decoking
or emergency situation like furnace tube rupture.
Stripper Reboiler (1502B)
: Snuffing steam at startup and shutdown to purge out the furnace or for emergency
situation like furnace tube rupture.
Ejector (1501L) : blanketing the system with nitrogen for air free.
Steam Tracing : Steam tracing for residue service or temperature conservation
Pump Quench Steam.
Utility Station.
zz) Pumps
For the cooling down the pump seal cooler as required pump seal plan. Following pumps
are required the cooling water.
Gas Oil Product Pumps (1506J/JA)
aaa) Compressors
For the cooling down the compressor and LO cooler Following compressors are required
the cooling water.
Make-up and Recycle Gas Compressors (1501J1/J2/JA1/JA2)
Sour Gas Compressor (1502J/JA)
13.2.6 Nitrogen
Compressed Gas Knock-out Drum (1508F) : Suppling during Regeneration.
Make-up and Recycle Gas Compressor (1501J1/J2/JA1/JA2) : Rod packing.
Sour Gas Compressor (1502J/JA) : Rod packing.
Nitrogen is supplied to utility station as required.
Correct installation and subsequent activation of the TK catalysts is extremely important to obtain
the optimum catalyst performance. These operations should therefore be carefully monitored. In
case of wet weather, the top of the reactor and the catalyst loading area have to be protected with
tarpaulins in order to keep water off the catalyst during the loading operation. If that is not possible,
catalyst loading must wait until it can be done without getting the catalyst wet.
When TK catalysts are ex-situ presulphided the loading should not be done in wet weather due to
the risk of SO2 formation.
In order to avoid uneven flow distribution (channeling,) in the catalyst bed, it is important that the
loading of the catalyst is done properly. Uneven flow distribution can have a significant influence
on the performance of the unit and in the worst case, the product specifications may not be met.
This can force an unscheduled shutdown for rectification of the situation.
It is equally important to properly install the reactor internals to prevent flow maldistribution. Each
level of internals must be properly assembled with gasketing where required to prevent leakage. In
multiple bed reactors, care should be taken to ensure internals parts are not intermixed.
The following sections discuss catalyst loading and internals installation in more detail.
The principal desulfurization catalyst for this unit15 is 1.3mm three-lobed TK-554. This
catalyst will be sock loaded in both reactors 1501D & 1551D. In addition, a graded bed
system is utilized at the top of the new reactor’s first bed to provide protection against
fouling. The graded bed system incorporates a 150-mm topping layer of high void inert
16x11-mm tableted TK-10, a 300-mm layer of 5-mm ring shaped TK-550 catalyst and a 300-
mm layer of 3-mm ring shaped TK-550 catalyst. The high void inert 16x11-mm tableted TK-
10 is also used for a 150-mm topping layer on the catalyst bed in the 1501D
Each of the catalyst beds of TK-554 is supported by a system of inert materials designed to
provide a stable support with minimum pressure drop. Most of the bottom head of each
reactor is filled with 18-mm inerts. That is topped with 75-mm layers of 6-mm inerts and 3-
mm inerts. The minimum distance from the top of the outlet cover at the bottom of the reactor
to the bottom of the 6-mm inert layer is 150mm. The catalyst canbe loaded into the head as
long as the cross sectional area of the catalyst is not less than 80 percent of the shell-cross
sectional area.
Prior to loading catalyst, the reactor should be checked to ensure all maintenance work is
complete, the internals are properly installed (with the exception of the manways) and the
reactor is clean and dry. Areas of particular importance are:
ddd) Ensure all contractor equipment and extraneous hardware have been removed.
eee) Verify that support beams are straight and level.
fff) Check that the screening on the support grids and outlet cover is clean and not corroded.
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ggg) Check that gaps between support grid sections and between grid sections and
reactor wall are sealed with ceramic fiber rope packing to prevent catalyst migration.
hhh) Check the outlet cover for gaps at the reactor head. Also check that all holes and
slots are clean.
iii) Check that the distribution beams and trays are flat and level. Tray sections should be
properly gasketed to minimize leakage. The trays should be clean and dry.
jjj) Check that all slots, holes and on the distribution tray chimneys or caps are not plugged
or fouled.
kkk) Check that the quench zone mixer is clean and dry.
lll) Check that the quench line nozzles are clean.
mmm) Check that the nozzles for thermocouples are clean and free from catalyst particles.
nnn) Check that the thermocouples are positioned correctly and firmly attached to their
supports.
Mark the wall and support beams at the top of each inert bed and catalyst bed layers. This will
facilitate catalyst loading and leveling.
Ceramic Inerts are used for catalyst support at the bottom of each catalyst bed. The support is
graded to prevent migration of the catalyst through gaps in the support grids and outlet cover.
The layer heights and inert sizes are specified in the reactor specification. The following
general guidelines are followed:
ooo) Inerts are loaded into the bottom of the reactor head so that the outlet cover is
totally overlaid to a depth as specified in the design manual. The minimum depth is
150mm (6 in). The diameter of the inerts should be larger than the width of the slots in
the outlet collector. A nominal 19-mm (3/4 in) ceramic inert or pellet is typically
specified.
ppp) If 1/8 inch catalyst is used the bottom layer on a grid support tray or the layer on
top of the 19 mm inerts is a nominal 6 mm (1/4 in) ceramic inerts. The depth of the layer
is 150mm (6 in).
qqq) If 1/16 inch or 1/20 inch catalyst is being used, two layers of inerts are used. A
75mm (3 in) layer of a nominal 1/8 inch is loaded on top of a 75 mm (3 inch) layer of a
nominal 1/4 inch inerts.
rrr) A hold-down layer of TK-10 is installed on top of the catalyst bed. The TK-10 is a high
void material that traps and holds scale and other contaminants as part of the catalyst
graded bed system. The TK-10 material also helps break down the liquid streams from
the chimney trays into multiple entry streams into the catalyst bed.
The principal desulfurization catalyst for this unit15 is 1.3mm three-lobed TK-554. This
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catalyst will be sock loaded in both reactors 1501D & 1551D. In addition, a graded bed system
is utilized at the top of the new reactor’s first bed to provide protection against fouling. The
graded bed system incorporates a 150-mm topping layer of high void inert 16x11-mm tableted
TK-10, a 300-mm layer of 5-mm ring shaped TK-550 catalyst and a 300-mm layer of 3-mm
ring shaped TK-550 catalyst. The high void inert 16x11-mm tableted TK-10 is also used for a
150-mm topping layer on the catalyst bed in the 1501D
Density. Kg/m3
TK-10 800
TK-550 3-mm and 5-mm rings 500
TK-554 1.3-mm three-lobed 700
Each of the catalyst beds of TK-554 is supported by a system of inert materials designed to
provide a stable support with minimum pressure drop. Most of the bottom head of each reactor
is filled with 18-mm inerts. That is topped with 75-mm layers of 6-mm inerts and 3-mm inerts.
The minimum distance from the top of the outlet cover at the bottom of the reactor to the
bottom of the 6-mm inert layer is 150mm. The catalyst canbe loaded into the head as long as
the cross sectional area of the catalyst is not less than 80 percent of the shell-cross sectional
area.
The Catalyst and Inerts Specification indicates which method is specified for each catalyst.
The sock loading is clone by using a vinyl or canvas hose attached to a hopper. The hopper is
placed on the inlet flange on top of the reactor with the hose extending from the button of the
hopper to the top of the catalyst bed. During the loading, the hose is shortened, so that it is
always close to the top of the catalyst bed. The catalyst should not be poured into a heap and
raked as this will result in segregation of particle sizes and improper catalyst particle
orientation. It is therefore necessary to have personnel inside the reactor to guide the loading
and ensure the top of the catalyst bed is kept reasonably level at all times. The personnel
inside the reactor should not step directly on the catalyst but use boards or “snow shoes” to
distribute the weight over a larger surface area.
The inerts and TK rings will always be sock loaded. When loading inerts, care should be
taken to prevent inerts from filling the hose. The weight of inerts may cause the hose to break
or separate from the hopper, thereby endangering the personnel inside the reactor.
Dense loading is done using a special dense loading apparatus. While there are various
designs for dense loaders, they all use the principle of dispersing the catalyst over the cross
sectional area of the reactor so the catalyst level rises evenly. Loading rate is controlled so
each catalyst particle comes to rest before being covered by another layer, thereby minimizing
bridging and particle size segregation.
The dense loading apparatus is mounted on the inlet flange of the reactor or in the manway
through the distribution tray in a multibed reactor. In the latter case. a vinyl or canvas hose
typically transfers the catalyst from a hopper above the reactor to the dense loader.
When using the dense loading technique, it is very important to periodically stop the loading
and check the level and density of the catalyst bed. Depending on the apparatus, there are
various adjustments that can be made to correct the loading patterns. If the bed density is low,
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the rate of loading must be reduced. If the bed density is high, it may be an indication that the
dense loader throws the catalyst particles at the reactor wall which cause breaking of the
particle. Furthermore, adjustments have to be made as the level of catalyst rises to maintain an
even distribution of the catalyst over the reactor cross sectional area.
After loading each catalyst layer, it is recommended to determine the depth of the catalyst bed
and the weight of catalyst loaded in order to check that required bulk density has been
achieved.
After a catalyst bed and topping layer have been loaded, reactor internals must be assembled
to close the access manway. At the top of the reactor, this will involve assembly of the liquid
distribution tray. In multi-bed reactors, there will be a quench section and catalyst support tray
to assemble.
The liquid distribution tray is installed to achieve an even distribution of both the liquid and
the gas over the entire cross section of the catalyst bed and thereby obtain optimal utilization
of the catalyst. It is extremely important that the tray is assembled correctly and is undamaged
and installed horizontally to meet the leakage specifications. In multibed reactors, the quench
zone mixer must be installed correctly to ensure the reactants are properly quenched and
remixed to achieve compositional thermal equilibrium between beds. The following items
should be checked when assembling the manway tray sections. If contract labor or the
contract catalyst loading personnel is assembling the internals, make sure they are well
supervised to be certain that the internals are properly assembled.
sss) Check that the distribution tray sections are undamaged and that no sections are bent or
severely corroded.
uuu) Check that the distribution tray is sealed tightly, both along the circumference and
between the different sections using ceramic fiber gasketing.
vvv) Check that the quench zone mixer is installed properly. Items a, b and c above also
apply to the mixer.
www) Check that the quench nozzle is installed properly with the correct orientation. The
connection of the nozzle to the quench line entering the reactor should be essentially leak
free.
xxx) Check that the manway catalyst support grid section is horizontal and fits well with
the other grid sections. Use ceramic fiber rope packing to seal gaps between grid sections.
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yyy) Check that the screens on top of the catalyst support grid sections are clean, non-
corroded and provide a gap free surface for catalyst loading.
All hydroprocessing catalysts will age and deactivate during use in the reactor. The deactivation
rate varies considerably, depending upon feedstock and operating severity. Straight-run naphtha
processing will cause a very low deactivation rate and resid processing will have a high activation
rate.
Some carbon will form on the catalyst during normal operation and as the run progresses these
carbon and other deposition like metals, silicon, et cetera will contribute to a loss of catalyst
activity. Normally, reactor temperature is increased to compensate for this effect and still maintain
product quality.
At some point in time, the inability to raise reactor temperature further or failure to meet product
sulfur specification will necessitate a plant turnaround. For the Kerosene/Gas Oil Hydrotreater, the
catalyst may be reused after it has been regenerated and reactivated. However, should any of the
catalyst in the top of reactor 6401D unexpectedly have been poisoned with silicon or metals, this
catalyst should be dumped separately and not to be reused. It must also be noted that the process of
burning off the carbon does not remove the metals that have been deposited on the catalyst.
If the catalyst is regenerated properly, in most cases it will regain almost the same activity as fresh
catalyst. However, if the catalyst is deactivated by metals and silicon, or by mal-operation that
causes sintering and loss of surface area, it will not regain the activity of fresh catalyst after
regeneration.
Dumping and screening of the catalyst following in-situ regeneration is recommended. The reason
for this is to remove particulates that have accumulated in the bed during normal operation and any
agglomerated catalyst formed during regeneration. (Iron sulfide that is deposited in the reactor
during normal operation will fuse catalyst pellets together during regeneration. This can result in a
high-pressure drop or hot spots inside the catalyst bed after start-up). The TK-10 inerts and TK-550
rings loaded on top of the bed of the 6401D should be replaced with fresh, and the reactor topped
with fresh catalyst to reach the original catalyst volume after reloading the regenerated catalyst.
After dumping, screening, and reloading, regenerated catalyst will normally have a lower
length/diameter ratio than fresh catalyst. This means that one can expect a slightly higher start-of-
run pressure drop as compared to fresh catalyst.
During regeneration, it is very important to maintain a good flow distribution of the regeneration
gas in the catalyst bed in order to avoid formation of localized hot spots. If the reason for the unit
shutdown was high pressure drop over the reactor, the risk of uneven flow distribution and hot spots
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during in-situ regeneration is particularly great. In those cases the reactor should be skimmed using
inert entry prior to regeneration.
For in-situ regeneration, it is necessary to have a number of thermocouples also in the middle of the
catalyst bed in order to follow the regeneration burning front.
Special precautions must be followed throughout the procedures if there is austenitic stainless steel
in the reactor section of the unit. Water in the liquid phase plus oxygen should never be allowed to
come in contact with austenitic stainless steel since there will be a light deposit of iron sulfide on
the metal. If water, oxygen, and sulfur come in contact with austenitic stainless steel, the areas of
stress, such as welds, could suffer from stress cracks. This hazard should at all times be considered
by the supervisor and operating personnel who will be conducting the regeneration.
NOTE: (Only for austenitic stainless steel) If, for any reason, it is necessary to open the reactor
system prior to regeneration, the unit must first be properly evacuated and purged with dry nitrogen.
The nitrogen blanket should then be maintained with a small nitrogen purge in the section to be
opened to prevent air and moisture from entering. Other sections should be blinded at this time.
NOTE: For the purpose of hydrotreating catalyst regeneration with austenitic stainless steel in the
reactor section, nitrogen containing 100 mol-ppm or less of oxygen must be used.
Process Description
The following is a procedure for regeneration of TK hydrotreating catalyst using recycle inert and
air. The catalyst is regenerated by circulating inert recycle gas in the normal recycle gas loop. Air
is metered into the inert gas through a block valve after the reactor has been pressured with
nitrogen. Throughout the regeneration, inert gas is recycled at the maximum rate possible while
maintaining the reactor inlet oxygen concentration.
Coke + O2 CO2 + H2 O
MeS + n O2 SO2 + MeO (Me = Co, Mo …)
SO2 + ½O2 SO3
A stream of dilute caustic is injected to the reactor effluent gas cooler during regeneration. The
caustic is required to scrub out the SO2 and SO3 formed during regeneration. The SO2 must be
completely removed from the gas returning to the reactor to prevent it from reacting with the carrier
to form aluminum sulfate. Sulfation of the alumina destroys the catalyst structure. The caustic in
the recirculation stream will neutralize all of the sulfur oxides and part of the carbon oxide
produced during combustion of the coked catalyst. If the sulfur trioxide is not neutralized, it will
condense out as concentrated sulfuric acid, causing corrosion of the effluent exchangers and piping.
The sulfuric acid dew point can be high as 250℃. The circulating caustic stream is therefore
injected at a point where the temperature is above the acid dew point.
The following reactions take place, when the recycle gas downstream the reactor is mixed with the
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circulating caustic:
The pH of the caustic solution must be in the range of 6.5-7.5 to ensure that all sulfur oxides are
neutralized. Higher pH will increase caustic consumption. The dilute caustic recirculation rate
should be high enough to cool the effluent gas and liquid mixture to below 100℃. The mixture is
then cooled in the reactor effluent condenser 6402C before going to high pressure separator 6402F
where the gas stream is separated from the caustic solution. A purge of the circulating liquid stream
is required to control dissolved solids. If not controlled, solids may precipitate and plug the lines
and exchangers, 6401C and 6402C. Make-up water and caustic are injected on a continuous basis
into the remaining circulating liquid stream before it is pumped back to the reactor effluent line.
The percentage of oxygen entering the reactor is the most important variable used to control
regeneration temperatures. Operators must be thoroughly familiar with its role in regeneration.
The oxygen concentration at the reactor inlet determines the temperature differential between
reactor inlet temperature and the highest average temperature in the catalyst bed in the reactor. As a
rule-of-thumb a concentration of 1.0 percent oxygen at the reactor inlet produces about a 55℃ rise
in reactor temperature if all the oxygen is consumed by burning.
For a given reactor inlet temperature and a given oxygen concentration, the highest temperature in
the catalyst bed can be predicted using the above rule-of-thumb. The maximum temperature will
occur in the burning zone, which moves down through the reactor temperature as coke is burned off
the catalyst.
For maximum restoration of activity, catalyst should not be heated above maximum peak
temperatures specified below. If any temperature in the reactor is rising so fast that the maximum
may be exceeds, reduce the air injection rate. In any emergency with high temperature, cut off all
air supply and ensure maximum gas recycle.
Because controlling the reactor inlet recycle gas oxygen concentration is so important, a continuous
oxygen analyzer is installed on this stream during regeneration.
Do not raise reactor inlet temperatures and recycle gas oxygen concentration at the same time.
Raising both at the same time makes it difficult to predict what will happen to peak burning
temperatures and may result in exceeding the maximum allowable temperature. Also, do not leave
the reactors with air in them without gas circulation. There is always the possibility that a small
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pocket of unburned coke may ignite and began to burn. Without gas circulation localized hot spots
can form.
During regeneration, it is very important to maintain a good flow distribution of the regeneration
gas in the catalyst bed in order to avoid formation of localized hot spots. If the reason for the unit
shutdown was high-pressure drop over the reactor, the risk of uneven flow distribution and hot
spots during in-situ regeneration is particularly great. In those cases the reactor should be skimmed
using inert entry prior to regeneration.
For in-situ regeneration, it is necessary to have a number of thermocouples in the catalyst bed in
order to follow the regeneration front.
The following is a procedure for regeneration of TK hydrotreating catalyst using recycle inert
gas and air. Circulating inert recycle gas in the normal recycle gas loop regenerates the
catalyst. Air is metered into the inert gas through a control valve after the reactors have been
pressured with nitrogen. Throughout the regeneration, inert gas is recycled at the maximum
rate possible while maintaining the required reactor inlet oxygen concentration.
A stream of dilute caustic is injected upstream of the reactor effluent air cooler during
regeneration. The caustic is required to scrub out the SO2 and SO3 formed during combustion.
The SO2 must be completely removed from the gas returning to the reactor to prevent it from
reacting with the carrier to form aluminum sulfate. Sulfating of the alumna destroys the
catalyst structure. The caustic in the recirculation stream will neutralize all of the sulphur
oxides and part of the carbon dioxide produced during combustion of the coke catalyst. If the
sulphur trioxide is not neutralized, it will condense out as concentrated sulfuric acid, causing
corrosion of the effluent exchangers and piping. The sulfuric acid dew point can be as high as
250C (482F). The circulating caustic stream has to be injected at a point where the
temperature is above the acid dew point.
The dilute caustic recirculation rate should be high enough to cool the effluent gas and liquid
mixture to about 100C (212F). The mixture is then cooled in the air cooler before going to
the high-pressure separator. A bleed of the liquid stream is required to control dissolved
solids. If not controlled, solids may precipitate and plug the air cooler Make-up water and
caustic are injected on a continuous basis into the remaining circulating liquid stream before it
is pumped back to the reactor effluent line.
The engineering contractor based on his design must check the gas circulation rate and the
process pressure drops during regeneration.
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The percent oxygen entering the reactor is the most important variable to control regeneration
temperatures. Operators must be thoroughly familiar with its role in regeneration. The oxygen
concentration at the reactor inlet fixes the difference between reactor inlet temperatures and
the highest temperature in the catalyst bed. As a rule-of-thumb a concentration of 1.0-percent
oxygen at the reactor inlet produces about a 55C (99F) rise in reactor temperature if all the
oxygen is consumed by the burning.
For a given reactor inlet temperature and a given oxygen concentration, the highest
temperature in the catalyst bed can be predicted using the above rule-of-thumb. The
maximum temperature will occur in the burning zone that moves down through the reactor as
coke is burned off the catalyst.
For maximum restoration of activity, catalyst should not be heated above the maximum peak
temperatures specified below. If any temperature in the reactor is rising so fast that the
maximum may be exceeded, reduce the air injection rate. In any emergency with high
temperatures, cut off all air supply and ensure maximum gas recycle.
Because controlling the treat gas oxygen concentration is so important, an oxygen analyzer
should be installed on the treat gas stream during regeneration.
Do not raise reactor inlet temperatures and treat gas oxygen concentration at the same time.
Raising both at the same time makes it difficult to predict what will happen to peak burning
temperatures and may result in exceeding the maximum allowable temperature. Also, do not
leave the reactors with air in them without gas circulation. There is always the possibility that
a small pocket of unburned coke may ignite and begin to burn. Without gas circulation
localized hot spots can form.
The following procedure presents the principal steps involved for in-situ regeneration:
zzz) Cut out the feed and strip oil from the catalyst by circulating hydrogen-containing gas
(treat gas). If the normal feed is heavy oil, it may be necessary to first flush the unit with
light oil to ensure complete removal of oil during the stripping. All lines, low points and
separators should be drained and flushed.
aaaa) Cool the reactor to a maximum temperature anywhere in the catalyst bed of 70-
80C (158-176F). While cooling, follow the standard refinery procedures regarding
protection of equipment subject to temper embrittlement. Depressurize the reactor section
to the flare and purge the system with nitrogen.
The two valves on the 6” start up line are locked open during [Link] by-pass the
recycle gas scrubber 1502E.
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The blind should be installed at XV-030 and the scrubber inlet during regeneration.
bbbb) Set up the piping systems for condensate and caustic make-up and spent caustic
purge. Establish a level of condensate (approximately 30%) in the high-pressure
separator.
cccc) Pressure the entire reactor system to 5 barg (73 psig) with nitrogen. Close all
quench valves Start the make-up and recycle gas compressor and circulate nitrogen at
maximum rate throughout the regeneration. Check for combustibles in the recycle
nitrogen gas. Total combustible should be below explosion limits before introducing air
into the system. Continue purging until this criterion is satisfied. Fire the reactor charge
heater and circulate hot recycle nitrogen gas until the reactor temperatures reach
approximately 135 ℃ (275F) or the temperature required for temper embrittlement
considerations (if regeneration pressures exceed cold pressurization limits). Check again
for combustibles in the recycle nitrogen gas.
dddd) Increase pressure of the high-pressure separator to the normally be about 9 barg
(132 psig). The separator pressure is controlled throughout the regeneration by 15-PV-
003. The temperature of high-pressure separator should be maintained below 57℃. If
possible, keep the temperature below 45 ℃ during regeneration.
eeee) Completely check out the oxygen analyzer and then put it in service to monitor
oxygen concentrations in the treat gas.
ffff) Raise the reactor inlet temperature to 315C (599F). Do not exceed a heating rate of
30C/hr (54F/hr) per hour.
gggg) When the reactor inlet temperature is 315C (599F) and all bed temperatures are
at least 260C (500F), introduce air. The air should be added slowly, and all
temperatures in the reactors should be watched closely. Air rate should be slowly
increased until a concentration of 0.5 volume percent oxygen in the recycle gas to the
reactor is reached.
hhhh) Once air is introduced to the system, start circulation of make-up water
(condensate) at 50% of normal throughput using the caustic recirculation system. Adjust
recirculation rate to keep temperature at mixer outlet below 100C (212F). Establish a
bleed of water from the high-pressure separator to control water level. Adjust flow of
make-up water (condensate) to the suction of the circulating caustic pump to design rate.
Sample water from the high-pressure separator for pH. When pH begins to decrease, start
caustic make-up into the suction of the circulation pump at minimum rate. Adjust caustic
make-up rate to control pH of spent caustic between 6.5 and 7.5. Adjust make-up water
rate to keep dissolved solids in spent caustic less than 10 weight percent. If the pH is too
low (less than 5), corrosion may be severe. If the pH of the solution gets too high (above
10), caustic cracking may result. If the temperature or solids content at the mixer outlet is
too high, solids may precipitate out of solution. This will result in a pressure drop build-
up in the air cooler due to plugging by the solids. If pressure drop begins to increase in
the heat exchange train, increase make-up water (condensate) rate and recirculation rate
as required to wash solids from system.
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iiii) Caustic scrubbing is continued as long as any SO2 is detected in the reactor effluent and
for an additional 8 hours after SO2 concentration drops to zero. Evolution of SO2 may not
stop until after the second or third burn. The recycle gas should be checked for SO2 at
regular intervals to confirm that complete removal of SO2 is being achieved.
jjjj) At a reactor temperature of 315C (599F) inlet and 0.5 volume percent oxygen at reactor
inlet, the maximum catalyst temperature should be about 370C (698F). Watch
temperatures closely. During this time, make an independent analysis of the oxygen
content of the inlet gas to check the performance of the oxygen analyzer. If combustion
does not start at 315C (599F), raise the reactor inlet temperature at 10C (18F) per
hour to a maximum of 340C (644F). Do not attempt to start combustion by increasing
the oxygen content of the treat gas.
llll) Slowly increase the air-rate until the oxygen-content in the treat-gas reaches 1.0 volume-
percent. At 315C (599F) reactor inlet temperature and 1.0 percent oxygen, the
maximum temperature in the reactors should be about 410-425C (770-797F). If any
temperature should go above 440C (824F), stop air injection. Do not restart air
injection until all reactor temperatures fall to a maximum of 425C (797F).
mmmm) Hold the reactor inlet temperature at 315-345C (599-644F) until the first burning
wave has passed through all catalyst beds. This is indicated by all bed temperatures
having passed through peaks and by a falling temperature at the reactor outlet. About the
time the first burning wave has passed through the reactors, oxygen will appear in the
reactor effluent gas and at this time, it will be necessary to reduce air addition rate to
prevent the oxygen concentration in the treat gas from increasing. Check the reactor
effluent gas for oxygen content at 1/2 to 1-hour intervals.
nnnn) After the first burning wave has passed through the reactor (s), reduce the treat gas
oxygen concentration and raise the reactor inlet temperature at a rate of 15C (27F) per
hour, following the guidelines shown below. If a second burning wave develops, stop
raising temperature and stay below maximum temperature limits described below.
oooo) When the reactor inlet temperature is 440C (824F) and all bed temperatures
reach a minimum of 425C (797F). Slowly increase air-rate until oxygen concentration
reaches 1.0 volume-percent at the reactor inlet. Watch temperatures closely while
increasing air rate. If any temperatures start to rise, reduce air rate immediately. Do not
allow any reactor temperature to exceed 450C (842F).
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pppp) Hold 440C (824F) reactor inlet temperature at 1.0-percent oxygen concentration
for 2 hours.
qqqq) After step (q) burning is considered complete if all of the following three
conditions are met:
No oxygen is being consumed. This is indicated by the same oxygen concentration
at reactor inlet and outlet.
There is essentially no temperature rise across any catalyst bed.
There is no SO2 in the reactor effluent gases.
rrrr) Shut off the caustic make-up and air addition. Maintain reactor pressure with nitrogen.
Continue to circulate dilute caustic to the effluent train
ssss) Reduce the reactor inlet temperature to 205C (401F) at 30C (54F) per hour by
reducing the heater-firing rate. Continue recycling the treat gas until all bed temperatures
are 250-230C (401-446F). During this period, increase the make-up water (condensate)
rate to aid in flushing the system and reduce the caustic concentration.
tttt) When all reactor temperatures are below 230C (446F), stop make-up water
(condensate) and recirculation pumps and drain all water from the separators and low
spots in the unit.
uuuu) Continue to cool the reactors with treat gas. While cooling, the treat gas should
contain 1-2 percent oxygen to minimize the formation of carbon monoxide. If the reactor
are to be opened and entered, it should be cooled to the temperature set by maintenance
procedures of the refinery (normally the reactor temperature should be below 40C
(104F). If the cooled reactor is to stand idle for some time, it should be isolated and
maintained under a slightly positive pressure of dry nitrogen.
vvvv) Cooling reactors to temperatures below 75C (167F) is difficult. Increased gas
circulation can be achieved by pressuring the system with nitrogen up to the low
temperature pressure limit set for the reactors. Cooling of the treat gas can be increased
by maximizing the draft in the heater and by bypassing all reactor effluent/treat gas heat
exchangers.
Note :
22) In Regeneration, make-up/recycle gas compressor is operating, during caustic is injected,
if make-up/recycle gas compressor is trip, the caustic injection pump should be stopped
by manually to prevent caustic flowing to the reactors.
Spent catalyst and iron sulphide deposits inside the reactor can be pyrophoric at temperatures above
70C (160F) and therefore, the reactor should be cooled to less than 50C (120F) unloading. A
nitrogen purge roust be maintained to the reactor during the unloading in order to minimize ingress
of air. In particular, opening of more than one manhole at a time should be avoided as this could
create a “chimney effect” leading to uncontrolled burning and temperature runaway in the catalyst
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bed.
It is recommended to use metal equipment for the unloading and, as a safety precaution, to have a
fire hose or steam lance ready for use if necessary. The work force engaged in unloading operations
should be adequately protected from getting into contact with the catalyst.
Warning
Nickel carbonyl, an extremely toxic substance, may be generated any time a carbon monoxide
bearing gas contacts a nickel containing catalyst at temperatures below about 200C (400F).
Strict operational and resting procedures should be followed to check for the presence of carbon
monoxide. If the atmosphere around the nickel containing catalyst measures more than 30-ppm
carbon monoxide, assume nickel carbonyl is present.
The recycle gas scrubber is provided with two beds of packing which will have to be loaded
separately. The packing is made of 2 x 4600mm 1” ceramic raschig rings. Loading will be carried out
the same way as for fuel gas H2S absorber 1601E.
25) Check that the gas injection packing support is correctly fitted as well as the hold down grid and
retaining screen detailed on the construction drawing.
27) Make sure to remove the dust and the broken rings before loading.
28) Load the rings up to the required height through the manhole.
29) Fit the top hold down screen and the hold down grid according to the drawings.
The top bed will be loaded in the same manner. The volume to be filled is the same as for the
bottom bed.
The furnace dry-out has to be carried out prior to start-up to prevent damage of refractory when the
furnace is brought into operation. The excess moisture has to be removed slowly by gradually raising
the temperature. One or more burners are lighted using fuel gas if possible for the operation but a
rotation of the burners will be done frequently for a good distribution of the released heat inside the
furnace.
The operation of the furnace dry-out will be performed according to the recommendations given in
the manufacturer manual.
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14.1.34 Description
A retractable nozzle is integral with a carriage which slides in the frame of the unit. This
nozzle has a forward advance movement combined with rotation and in this way the two
blower jets located at the end of the nozzle head follow a spiral course inside the furnace or
superheater.
Blowing only starts when the nozzle has reached a position in which the blower head has
come completely out of the wall (in order not to damage refractories and fireproof linings).
This steam opening and shut-off is effected by means of an automatic valve built into the unit.
When the nozzle has reached its “forward” position, the movement is reversed and the unit
starts going backwards in “reverse” to return to its “stop” position. When the movement is
reversed, a mechanism makes it possible to shift the pitch of the blowing spiral which
provides more efficient cleaning as the jets do not follow the same path when moving
backwards as they do when moving forwards.
Note : Never operate the unit without steam, as this is likely to damage the outer nozzle.
14.1.35 Operation
If there is a fault or breakdown of pneumatic origin, the unit can be operated manually.
Proceed as follows :
Operate the front limit switch by hand, the unit must reverse its movement. If this
is not so, switch off the air : and check the connections.
During the return movement before the unit reaches its rear limit switch, operate
the latter by hand and check that the unit stops. The unit can now be started in
normal operation.
Note : Do not carry out these operations without steam if the unit penetrates into
hot gases.
Adjustment of limit switch positions : This is a factory adjustment and must make it
possible for the carriage to stop 10 mm before the mechanical stop. It is possible to
alter this adjustment by means of the knurled adjusting screw.
For further details, consult the manufacturer's documentation.
[Link] The fuel oil pressure control valve should be set to hold approx. 3.5 bar in the
supply header. Fuel all temperature at the burner must be such as to give a
viscosity of 20/40 cSt. The burners will operate temporarily at start-up with
viscosities of 450 cSt. However it is important that after the initial start-up a
suitable oil temperature is maintained for 20/40 cSt viscosity. (Temperature 120
C.)
[Link] Drain condensate from steam header and open vide the steam valve at each burner.
Also open wide the by-pass valve provided as part of the burner piping. With only
steam flowing through the burner, check the detaching gear connections to be
certain that these are not leaking.
[Link] Close the steam by-pass valve. This valve must be kept closed all the time when
burners are firing on fuel oil. Adjust atomizing steam control valve until a slight jet
of steam is spraying from the tip. The venturi type gas pilot can be ignited with
hand-torch or the spark plug (if furnished). Pilot gas pressure recommended is 0.1-
02 bar. The gas valve and air shutter on venturi tube controls adjustment of the
flame shape and length. Air register should be open 3/4” to 1 1/2” (18 to 36 mm).
Burner is then ready to be lit-up. Be sure that the stack damper is wide open. Do
not stand directly under operating burners. In most cases for safety, it is advised
that operator stands at the side of heater when lighting burners vertically firing
under the heaters.
[Link] Very gradually open oil control valve on burner until oil ignites. This will take
place easily. Be sure that no excessive atomizing steam is used. If burner does not
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immediately light when all is spraying from the tip, shut off oi1, purge furnace7
and investigate. Perhaps the fuel oil is not sufficiently hot, atomizing steam is too
wet or water is present in the fuel oil.
[Link] After muffle blocks become red hot, gradually increase steam and oil to obtain the
capacity requested. Gradually open the air register in order to get a bright clear
flame.
[Link] The shape and Length of all flame is readily controlled by the quantity of atomizing
steam used and also with the flame angle of the oil tip. This tip should operate
without f1ame impingement on the burner block.
[Link] Before flowing fuel gas into the burner header, it is imperative that the gas burner
be disconnected and the header blown clean of all pipe scales, compounds, dirt,
etc... Use steam at 2 bars or more for this purpose.
[Link] The stack damper is to be wide open. Check the draft gauge to make sure that a
slight draft exists at burner level in the furnace. Let the unit purge for about 15
minutes under natural draft.
[Link] The venturi type gas pilot can be ignited. Keep this pilot burning while the gas
blanks are removed. This will insure ignition of any gas that might leak through
the gas valve.
[Link] With air register slightly open, the gas may be gradually turned on to each burner.
After some time the muffle block will become red hot. The air register may be then
gradually opened to shorten the flame. Too much air causes a short, sharp, unstable
flame.
[Link] An Orsat analysis should be taken at the convection zone outlet to determine the
correct adjustment of air supply. For the average radiant heat type of furnace the
following tentative adjustments are suggested :
iii) Open damper in the stack to hold a furnace draft at burner level of 0.1” to 0.15” w.c.
(2.5 to 4 mm.).
jjj) Adjust air register (when firing natural gas) to obtain a CO2 of 9% to 10% at maximum
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furnace load. If firing on hydrogen fuel gas, a minimum of oxygen must be obtained in
exhausted fumes.
[Link] If for any reason the flame should go out due to gas supply failure, do not attempt
to reignite the burner from the hot bricks or a hand-torch before you follow these
precautions :
kkk) Shut-off tight the gas valve
lll) Open wide the stack damper
mmm) Reignite burners as described
[Link] For periodic cleaning or orifices in gas burner nozzle while the unit is in operation,
a 1/2” purge connection mast be provided on the gas manifold to introduce gas or
air. When the furnace is stopped, inspect the gas burner nozzle orifices and remove
all coke or other particles. This is imperative when sulphur rich fuel gas is being
burned.
[Link] When firing fuel gas for a long period, remove entirely the fuel oil burner and hang
it in a convenient near-by position for use in an emergency. When firing fuel gas,
but the possibility of firing fuel oil is imminent, it is best to keep the fuel oil
atomizer connected. In this case a smell quantity steam should flow through the oil
burner tip to keep it cool and prevent it from being burned-off by the flame of gas.
Both fuel gas and fuel oil can be fired at the same time and in the same burner providing that
ratio is 25% of one fuel to 75% of the other. If burning some gas this will normally stabilize
the all flame and will reduce all chipping. In some cases when the fuel oil is too cold at the
start-up, the burning of fuel gas helps the atomization and vaporization of fuel oil and
stabilizes its ignition.
14.1.37 General
The reasons for accidental coke formations inside the heater tubes can simultaneously or
in succession come from different sources:
eventual problems which occur during operation and involve the change or the
deterioration of the process stream.
Thermal insulating, the coke deposits cause an increase in temperature of the tube metal
which is an irreversible process and for an equal quantity of heat absorbed: an increase
in fuel consumption, in flue gas temperature and in pressure drop which are often
noticed with difficulty.
[Link] Coke location
It is important to locate the coke formation when the heater is in operation and metal
temperature recording only is insufficient. For a given process charge, flow,
temperatures, pressures (inlet and outlet), flue gas temperature at radiant section outlet,
excess air, flow and nature of the fuel burnt, must be taken into account.
Thermal decoking has been used with success for a long time. It can be carried out
during a short time (from 1 to 3 days) according to the nature, thickness, volume of
coke to be removed and know-how of the operators. No special equipment s needed
except steam, air and water as well as associated piping and controls.
[Link] Principle
nnn) A spalling or mechanical removal of the coke due to opposite dilatations between
coke and tube metal is obtained by varying steam flow and firing rate. During this
phase, the greatest part of the coke must be removed.
ooo) The burning or chemical destruction of the coke due to the chemical combination
between hot coke and steam produce CO, CO2 and H2. The chemical combination
between hot coke and oxygen produces CO and CO2.
ppp) Spalling can be sufficient in certain cases but in other cases one can elect to use the
burning phase.
[Link] General
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Steam and air decoking should not be used where tube deposits have an appreciable
content of salt or lime.
The operators chosen for this decoking operation should be well experienced. Local
conditions will dictate the detailed procedure to be used.
qqq) The heater feed will be stopped in accordance with the usual shutdown procedure.
Coils will be purged and free from hydrocarbons and the burners will be shut down.
rrr) As soon as the purging has been completed, the decoking manifolds will be connected.
sss) The equipment must be designed to isolate the process coils from normal connecting
manifolds and connected separately and simultaneously with fluids needed for
decoking for which flows, pressures and temperatures shall be controlled as also
effluent qualities and temperatures.
ttt) For this, the convection section coils will not be disconnected from those of radiant
section; steam and air will circulate in same way as normal process, no reverse
circulation will be required.
The same procedure, spalling and/or burning shall be carried out on each pass of the
heater, but in order to reduce the total consumption of steam, the pass will be decoked
one by one in a same radiant cell in which burners will be lighted, whilst in the other
cell they will be kept shut off and dampers closed. The steam will circulate in all coils
that are not in a burning phase.
uuu) The effluents coming from the coils must be checked (colours, analyses, samples).
Burnt gas must be water quenched (verify that no sampling connections are left open).
Quick analysis of effluents (fyrite - draeger) must be available.
vvv) The flue gas temperature at outlet of radiant and convection sections must be
checked and recorded. Verify pressure gages (location, length) connections and
measuring devices.
www) Skin thermocouple temperature indication should not be used only to estimate tube
metal temperature. They also serve as an indication of the combustion mode inside
tube.
xxx) The sight doors are used for visual inspection during decoking. They will be free
of obstruction (side and floor).
Check that they can be opened wide. Heater accesses around and under floor must be
made clear.
yyy) It is important that dampers of stack and burners be in good operating condition.
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zzz) Oil guns will be removed. Fuel gas will be used as fuel in order to obtain non-luminous
flames and to be able to observe tube colors changes.
aaaa) Decoking operation will take place at night in order to detect colours of tubes more
easily.
bbbb) The automatic heating control will be switched out. During a decoking operation,
the heating must be operated manually. Sometimes hand operation will be carried out
burner by burner.
cccc) The valves for control of the different fluids used for decoking operations must be
installed close to the heater to be decoked and similarly for the temperature gauge and
steam/air flow meters.
dddd) The decoking phases must be made with a minimum of heat from burners in order
to avoid overheating of tubes being decoked and thus protected.
The draft at radiant section outlet will have to be zeroed and in good state.
The connecting tubes between heater and draft gage must be cleaned.
[Link] Procedure
eeee) The shutdown and purging phases being carried out check the connections of coils
with steam, air, water, and effluents circuits.
ffff) Check location, operating conditions of control and block valves, and set circulation of
cooling and quench water.
gggg) Trim stack and burner dampers to minimum. During the decoking phase, make
sure that the heater is not with positive draft at any point and that combustion operates
with minimum air compatible with a production of luminous but non-smoking flames.
hhhh) Light up gas burners at low rate, one in every two and then, if necessary, light all
the burners in order to keep a short flame and each burner operating at a low rate. Then
progressively increase by 150 C/h, the temperature of flue gas at radiant section outlet.
iiii) Introduce steam through all the coils to be protected until the flue gas temperature
reaches about 300 C (more or less according to inlet temperature of steam).
jjjj) Watch and adjust the steam flow in order to obtain 500 C at coils outlet (under
protection) and 600 C at outlet of pass (under decoking) when the flue gas
temperature reaches 700/730 C.
Usually, the spalling starts when flue gas temperature at radiant section outlet reaches
650 C.
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kkkk) Induce spalling by reducing and increasing the steam flow. Repeat this operation
several times and observe effluents.
If large coke particles are produced, reduce steam flow to prevent erosion.
When the steam coming from the pass under spalling is clear and spalling cannot be
improved :
mmmm) Reduce the heat load to obtain 650 C at radiant section outlet.
nnnn) Reduce the steam flow in pass where burning must be carried out.
oooo) Slowly introduce air required for burning with steam/air ratio of 10 to 1 about.
pppp) Observe colours and temperatures of the tubes. The burning phase starts when
steam and air are sufficiently hot.
Hot spots move along in the same sense of direction as the air and steam.
Burning front should be observed by comparing the cherry-red colour of tube metal
where coke is burning with that of dull-red where coke has been burnt. The burning
front should move at a rate of some 30/40-cm per minute but is quite dependent on
original coke deposit and effectiveness of spalling.
The flue gas temperature must be low enough for tube to be red only where the coke is
burning. This is a temperature 700 C or about.
During coke burning, the temperature of tube metal should not exceed 730 C.
The effluent temperature at coil outlet should not exceed 700 C during burning phase.
Usually, this temperature reaches only 600/650 C.
If during the burning phase, the tube temperature increases, reduce the air-flow and
increase the steam flow.
Watch the effluents. At the beginning they will be black and at the end they should be
reddish brown. Analyze effluents - 19 % of CO2 give a steady combustion (CO and O2
will be also checked).
qqqq) When the effluents do not contain CO2 and in order to check that the coke
combustion is finished, slowly reduce the steam flow and increase the air flow.
Check the effluents with analyzer for CO2. When combustion has ceased, cut the air
flow, increase the steam flow to remove ash.
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rrrr) To complete procedure, the tube metal temperature must be slowly and progressively
reduced by 100 C/h. Reduce burner feed, air intake and hold draft at a steady value.
ssss) Cut steam flow when flue gas temperature reaches 250 C.
tttt) Shut off the main burners and, later on, the pilots.
uuuu) Cut the cooling and quench water and bring the system into normal operating
conditions.
14.1.39 Precautions
avoid quick heating and cooling; for example, in case of steam shortage, reduce
heat load by 100 C/h, then repeat the operation from the beginning.
avoid excessive velocities through tubes; coke particles are very abrasive
at the appropriate time, steam and air pressure and flows, effluents and flue gas
temperature, and all analyses must be recorded on a special sheet.
Density vs ℃
Viscosity vs ℃
Vapor pressure vs ℃
Several suppliers are able to offer corrosion inhibitor. Below are the characteristics of two
recommended commercial products.
General description
KONTOI, in operation :
detergent, acting to clean metal surfaces of corrosion products and other fouling
materials.
Solubility
C4 and heavier hydrocarbons : soluble
Water : insoluble
Typica1 use rate : 6 - 12 ppm
General description
Viscosities (cSt) :
at 15℃ : 23
at -23℃ : 120
at -34℃ : 230
at -57 ℃ : 1100
14.1.34 Introduction
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Since corrosion cracking of austenitic stainless steel can lead to failure of the equipment
involved, it is of the utmost importance that this equipment be properly protected to prevent
corrosive environments from occurring. Therefore, all operating personnel, and especially the
supervisory personnel, must be familiar with the locations of piping and equipment fabricated
from austenitic stainless steel. They should also recognize the need for special handling of
these sections of the unit during startup, shutdown, flushing, cleaning, maintenance, and
inspection, and should be thoroughly familiar with the procedures to be used for the proper
protection of the equipment.
It is recognized that corrosion cracking of austenitic stainless steel is much less likely to occur
in hydrodealkylation units than in hydrocracking and hydrodesulfurization units, because of
the relatively low sulfur concentrations involved combined with the wide use of the stabilized
grades of austenitic stainless steel. Nevertheless sufficient danger of corrosion cracking exists
in hydrodealkylation units to warrant due consideration for adequate protection procedures.
A number of both general and detailed instructions are contained in this discussion; however,
all possibilities cannot be covered.
14.1.35 General
Austenitic stainless steels are those of the “300 series,” the compositions of which are
nominally 18% chromium and 8X nickel. The most common types used in the
petroleum industry are Types 304, 316, 321 and 347. Because of their inherent high
temperature strength properties and high corrosion resistance, they are particularly
suitable for use in hydrocracking, hydrodesulfurization, and hydrodealkylation units in
areas of moderate and high temperature, and where substantial resistance to hydrogen
sulfide corrosion is required, such as in heater tubes, reactors, reactor effluent
exchangers and piping. Types 321 and 347 are stabilized to minimize intergranular
carbide precipitation and are preferred because they are more resistant to the
intergranular corrosion cracking caused by polythionic acid attack, which can occur
particularly during downtime periods when exposed to air and moisture. Since these
stabilized grades are not completely immune to intergranular corrosion cracking, special
handling procedures are recommended for the protection of these materials as well as
the unstabilized grades.
The presence of halides (chlorides are usually the most serious offenders) along with an
aqueous phase and tensile stresses can result in stress corrosion cracking of austenitic
stainless steels.
accumulate and concentrate in hot equipment, and as long as precautions are taken to
limit the chloride content to low levels in any flushing, purging or neutralizing agents
used in the system.
Once a unit has been placed on stream, even if the sulfur content of the feed stock is
low, all items made of austenitic stainless steel should be considered to contain a layer
of iron sulfide scale. Even though these layers of scale in many cases may be very thin,
they represent a potential hazard to the underlying steel. The action of water and
oxygen on this sulfide scale forms weak sulfurous type acids, commonly referred to as
polythionic acids, which can attack austenitic stainless steels and cause intergranular
corrosion and cracking. These stainless steels are vulnerable to this type of corrosion,
particularly in areas of residual tensile stresses and in areas where intergranular carbides
may exist, such as the heat-affected zones adjacent to welds. Therefore, special
precautions should be taken to protect austenitic stainless steel from this corrosive
environment.
[Link] Protection against Polythionic Acid Attack
Since these acids are formed by the action of water and oxygen with hydrogen sulfide or
sulfide scale, elimination of either liquid phase water or oxygen will prevent these acids
from being formed. Since there will usually be an equilibrium amount of water vapor
present during the normal operation of a unit, during shutdown periods this water vapor
can be prevented from condensing by maintaining the temperature of the austenitic
stainless steel equipment above the dew point of water.
Neutralization
and maintaining an ammoniated nitrogen blanket or by washing with a dilute soda ash
solution.
Nitrogen used for the purging and protection of austenitic stainless steels should be dry
and the oxygen content should be limited to a maximum of 100 mol-ppm. If the only
nitrogen available has an oxygen content in excess of 100 mol ppm, or if the oxygen
content is unknown, then as a safeguard ammoniated nitrogen should be used where
possible. However, for this case, catalyst safety considerations might be necessary.
10) All personnel working in the unit should be familiar with the toxic nature of
ammonia, and must follow proper safety precautions in working with the system
when it contains ammonia. For example, workers opening flanges or manways in a
system containing ammonia should be equipped with fresh air masks or other
oxygen breathing equipment.
11) In order to preserve the activity of the catalyst in the reactors, ammonia is not to be
passed over the catalyst when it is in its oxidized form, that is, whenever the
catalyst is either fresh or freshly regenerated. When dealing with platinum type
catalysts, ammonia should be excluded regardless of the state of the catalyst.
12) Brass and most other copper alloys are subject to corrosion attack from ammonia.
Therefore, arrangements should be made to isolate this equipment from the system
before admitting any ammonia.
Composition
Aqueous neutralizing solutions of soda ash (Na2CO3) should be prepared in the range of 2%
to 5% by weight. Preheating the water to about 38C (100F) will facilitate dissolving all
the soda ash. In this range a sufficiently high level of alkalinity will be provided to affect
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Neutralization Techniques
Whenever a soda ash solution is used for neutralizing and protecting austenitic stainless
steel, the piping or piece of equipment involved should be filled completely full with the
solution.
The equipment should then be allowed to soak for a minimum of two hours before the soda
ash solution is drained and the equipment is exposed to the air. If there are any pockets of
unvented high areas in the equipment which cannot be reached by filling with the soda ash
solution, then the solution should be vigorously circulated through the equipment to assure
thorough contact of all austenitic stainless steel surfaces. This circulation should be
continued for a minimum period of two hours before draining and exposing the equipment to
air. For extremely large surfaces, such as reactor or large vessel walls and internals, where
filling with soda ash solution is not only impractical but in some cases impossible because of
foundation load limitations, it is recommended to wash the areas very thoroughly by means
of a high pressure hose equipped with a spray nozzle. This type of washing will have to be
done after the vessel has been opened to allow entry. Until the soda ash washing has been
completed, the vessel should be maintained under a nitrogen blanket to prevent the entry of
air.
Protective Film
In all cases of flushing or washing with soda ash solution, after the solution is drained from
the equipment, the surfaces should be allowed to dry so that a film or fine deposit of soda
ash remains on all surfaces for added protection against polythionic acid formation.
Therefore, after draining the soda ash solution, do not rinse the system with steam or water.
For large accessible surfaces, such as vessels or reactor walls and internals, the excess dried
soda ash can be removed just prior to startup with a brush or dry cloths; do not use wet
cloths and do not flush with steam or water. The small amount of soda ash remaining on the
reactor surfaces, even if it were all deposited on the catalyst, would not have any significant
effect on the activity of catalyst.
14.1.37 Hydrotesting
When conducting hydrostatic tests on new austenitic stainless steel equipment, the water used
should have a chloride content not exceeding 50 ppm by weight, in order to reduce the
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possibility of concentrating chlorides in pockets or dead areas of the system. If chlorides were
allowed to accumulate and concentrate (such as during subsequent heating operations) in such
areas, stress corrosion cracking could result. If the only water available has a chloride content in
excess of 50 ppm, then 0.5 wt-% of sodium nitrate should be used.
Whenever a piece of equipment has been used for the processing of hydrocarbons in
hydrocracking, hydrodesulfurization of hydrodealkylation service, it must be assumed that some
degree of sulfide scale can be present. Therefore, even if this sulfide scale is so slight that it is
difficult to detect, the possibility of polythionic acid formation with resulting intergranular
corrosion cracking exists. Even if the equipment has been cleaned by mechanical means,
burning or acidizing, it is difficult to assure that no traces of sulfide scale remain. Therefore,
any hydrostatic testing (and any cleaning by hydroblasting) operations on used equipment
should be conducted using the dilute soda ash solution specified for neutralizing this equipment.
Here again, a protective film of dried soda ash should be allowed to remain on the surfaces of
the equipment while it is exposed to the air.
The austenitic stainless steel tubes in a reactor charge heater can best be protected by
maintaining a balanced set of small fires (or pilots, as applicable) in the heater box at all
times, even when there is no circulation of process material through the tubes. These small
fires should be adjusted to keep the tubes warm and dry to maintain the environment inside
the tubes above the dew point of water. As a general rule about 205C (400F), as
measured by thermocouples placed in the hip sections of the heater and directly below
convection coils that may exist, will usually be sufficient for this purpose. The dew point,
however, should be determined for each specific condition involved and the temperature
should be adjusted as necessary. Only fuel gas, firing should be used for this operation
because of the difficulty in controlling and maintaining sufficiently small flames when
burning fuel oil. It is important during these periods of heater operation that the heater
firing be under strict control and that the firing pattern be properly established to provide
good heat distribution. Sufficient thermocouples should be installed throughout the hip
sections of the heater to provide a good measurement of the firebox. These temperatures
and to monitor the distribution of heat in the firebox. These thermocouples should be
located below any convection bank in the heater, and should be connected to a continuous
recorder provided with high and low alarm points. The low alarm point should be set at
about 150C(300F) and the high alarm point at about 232C (450F).
CAUTION: Stack temperatures should never be used to control firebox temperatures.
If it should be necessary for any reason to shut down the fires in charge heater containing
austenitic stainless steel tubes, then this should be done only when it is absolutely certain
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that the environment within the tubes does not contain both oxygen and water (or water
vapor). As a result of the operation of the reactor effluent water wash facilities in units so
equipped, there will normally be an equilibrium amount of water present in the entire
reactor circuit both during normal operation and during or after a period of in situ catalyst
regeneration. If the heater fires must be shut down during a period of normal operation, it
is required only that no oxygen is present, which is usually the case during normal
processing periods. As the heater tubes cool there will be small amounts of water
condensing inside the tubes; however, this water should not be harmful in the absence of
oxygen.
If the heater must be cooled down and it is suspected that trace quantities of oxygen might
be present, then before cooling the heater the system should be depressured completely, but
do not evacuate. Evacuation at this point is perhaps possible, but not recommended
because it introduces the possibility of allowing air to enter the system. Continue to
maintain the 205C (400F) FIREBOX temperatures while depressuring and purging. After
the system has been depressured, pressure with nitrogen to any convenient pressure level.
Repeat this, depressuring/pressuring procedure as many times as required to reduce the
oxygen concentration, by dilution, to as much below 100 mol ppm as is possible and
reasonable. Then the fires can be shut down and the heater allowed to cool.
Neutralization
If neutralization is necessary, such as when a tube or tubes are cut out of the coil, or any
time when exposure to air at temperatures below the dew point of water cannot be avoided,
the tubes should be filled with soda ash solution and allowed to soak for a minimum of two
hours. With vertical coils, where it is not possible to completely fill the unvented upper
return bends, it is necessary instead to vigorously circulate the soda ash solution through the
tubes for a minimum of two hours to assure contact of all surfaces. After draining the soda
ash solution, do not flush with steam or water but instead allow a film of protective soda
ash to remain in the tubes.
Exterior Surfaces
Whenever heater fires must be shut down and the tubes are allowed to cool, it is
recommended that the exterior tube surfaces be protected, especially in heaters where fuel
oil or high sulfur content fuel gas is employed. As a result of the sulfur in the fuel, a sulfide
or sulfate scale can build up on the exterior tube surfaces. If moisture is allowed to
condense on the tubes as the heater box is cooled, the action of oxygen and moisture on the
scale can form polythionic acids which can attack the austenitic stainless steel tube surfaces
and lead to intergranular stress corrosion cracking. There are two recommended procedures
that can be followed to prevent this from occurring: First, it is possible to prevent any
moisture from condensing on the tubes, and thus prevent the formation of polythionic acids,
by purging the firebox with copious amounts of dry air. Normal instrument air is prepared
by processing through a set of dryers where the dew point is reduced to a sufficiently low
level to prevent condensation from occurring at ambient conditions. This air can be
effectively used to maintain a dry air blanket in the heater box both during cooling and
throughout the entire period the fires are out. In order to minimize the consumption of
instrument air, and to prevent moist air from entering the heater box, the stack damper, all
burner air registers, and all doors and ports in the heater box should be kept closed.
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Second, an alternate method of protecting the tubes from polythionic acid attack is to cover
the exterior tube surfaces with a protective film of soda ash, which will act to neutralize any
polythionic acids as they are formed. The neutralizing soda ash should be the same dilute
solution recommended for general neutralization, and should be applied to the tube surfaces
as soon as the heater box has cooled sufficiently to prevent vaporizing the soda ash
solution, and preferably before any moisture has begun to condense out on the tube
surfaces. A fairly efficient and effective method of applying the soda ash solution is to
utilize a vat or tank with a small portable pump which can pump the solution through a hose
fitted with a spray nozzle which will produce a fairly fine mist. NOTE: A low pressure
spray is advisable as high pressure may erode the refractory. Small diameter pipe
extensions can be fitted to the hose to allow reaching up to the tube areas at the top of the
heater box. This type of spray equipment will minimize the soda ash consumption and
provide a reasonable means to reach all tube surfaces which are exposed to the heater
flames. Once the soda ash solution has been applied, it should be allowed to dry to form a
protective film on the surfaces of the tubes; do not wash off this protective film.
If the exterior tube surfaces are heavily coated with an oxide or carbonaceous material, it
should be removed by wire brushing or sandblasting. This cleaning, however, will also
remove any protective soda ash film which may have been applied. In this case, the tube
surfaces should be further protected by applying maintain a dry air blanket in the heater box
both during cooling and throughout the entire period the fires are out. In order to minimize
the consumption of instrument air, and to prevent moist air from entering the heater box,
the stack damper, all burner air registers, and all doors and ports in the heater box should be
kept closed.
If lines leading to or from heat exchangers containing austenitic stainless steal are to be
opened, blinds can be rapidly inserted to isolate the exchanger, while maintaining a
nitrogen purge through the exchanger involved to prevent air from entering. A nitrogen
blanket or continuous nitrogen purge should then be maintained in the exchanger during
this maintenance period.
If shell and tube exchangers containing austenitic stainless steel are to be opened and
inspected, or if the tube bundles are to be pulled, then before exposing this equipment to air,
both shell and tube sides should be flooded with soda ash solution and allowed to soak for a
minimum of two hours. If there are any pockets or high areas which cannot be reached
with the soda ash solution, then the soda ash solution should be vigorously circulated
through the exchanger for a minimum of two hours. Do not rinse with water, but instead
allow a film of soda to remain on the surfaces.
If tube bundles of austenitic stainless steel are to be cleaned by hydroblasting, then soda ash
solution should be used for this purpose instead of just water.
Any time a reactor is to be opened, maintain sufficient nitrogen purges to prevent the entry
of air into any part of the system and isolate the charge heater coils and the reactor effluent
system with blinds. A blanket of nitrogen should also be maintained in the reactor,
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When the reactor internals are to be exposed to air for a prolonged period of time, such as
during a catalyst change, the reactor walls and internals should be washed very thoroughly
as soon as possible with a high pressure hose, using copious amounts of soda ash solution.
A portable pump and a vat of soda ash solution on skids is advisable for this operation. In
order to do this washing properly, a workman equipped with a fresh air mask and following
all other proper safety precautions, might have to enter the vessel to make sure all surfaces,
including the underside of the top head, are thoroughly wetted. Be especially careful to
thoroughly soak welded areas with particular emphasis on welds normally required to
support heavy loads, such as those on support beams, grids and trays. When the reactor
contains trays, which would make wetting all surfaces with soda ash solution difficult, a
sufficient amount of soda ash solution should be sprayed around the top of the reactor, and
allowed to rain down through the reactor to wet as much of the surfaces as possible in the
areas below the top tray. Be sure to thoroughly soak and keep wetted any used catalyst
remaining in the reactor. Then air can be drawn through the reactor so that personnel can
enter. During this time, a small flow of soda ash solution to the reactor should be
maintained, and as each tray manway is removed, the vessel area beneath that tray and the
underside of the tray should be thoroughly washed with soda ash solution.
After washing with soda ash solution, allow the surfaces to dry with a fine deposit of soda
ash. Do not rinse this residue off with water. Later, just prior to reloading catalyst, wipe as
much excess soda ash residue from the surfaces as possible with brushes or dry cloths; do
not use water or wet cloths.
When it is necessary to reduce the temperature in an austenitic stainless steel charge heater coil
below the dew point of water when oxygen is present, such as during the procedure of cooling
the catalyst bed to a temperature which would allow entering the reactor following a catalyst
regeneration, the oxygen must first be reduced to an acceptable level. Maintain the final
reactor temperature used in the regeneration and continue gas circulation; and depressure to the
minimum allowable for recycle compressor operation. Then pressure with nitrogen. Conduct
compressor operation. Then pressure with nitrogen. Conduct this procedure at least three
times, or as necessary to reduce oxygen concentration in the circulating gas by dilution to as
much below 100 mol ppm as is possible and reasonable. Maintain reactor temperatures and gas
circulation, after shutting down and draining the caustic and water systems, until the reactor
system is dry and no more water collects in the separator. Then the system can be cooled to
about 65C (150F) at the reactor outlet. At this point, shut down the recycle gas compressor
but maintain heater fires sufficient to maintain about 205C (400F) FIREBOX temperatures
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14.1.39 References
Additional information on the subject of protection of austenitic stainless steel can be found in
the NACE Standard RP-01-70, entitled "Recommended Practice, Protection of Austenitic
Stainless Steel in Refineries against Stress Corrosion Cracking by use of Neutralizing
Solutions during Shut Down" and approved October 1970. Copies may be obtained from
NACE Headquarters, 2400 West Loop South, Houston, Texas 77027.
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ASTM
Specific Gravity 1/W 1/D
D1298/D4052
LOW PRESSURE 15-S-201 Composition UOP539/ D1946 2/W 1/D 1/M
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Note : Refer to Routine Sample Testing and Scheduling available on RIS under the Lab Analysis tab for the
prevailing schedule which is updated on a regular basis
15.2.1 General
The samples of the various petroleum product and by-product will be taken using the sampling
facilities provided in each unit.
Table 2
Applicable Types of Sampling Facilities
Sampling Special Features of the Sample
Sample Category
Type Sampling Facility Connection No.
(above 55 oC)
2 High temperature at Quench Gas flow decreased Check the TI-012, Tl-013, TI-014
reactor outlet 1501 D and Tl-015. Check if any bad
thermocouples. Eliminate the bad
thermocouple.
Controller malfunction-rectify
cause
5 High Reactors pressure drop Coke formation inside Test Feed LGO.
reactors due to heavier feed Eliminate Source
stock
6 High pressure drop across Coke formation inside heater Decoking procedure to be carried
heater 1501 B tubes out after plant shutdown
7 High tube skin temperature Coke formation inside heater Decoking procedure to be carried
for heater 1501 B tubes out after plant shutdown
8 High tube skin temperature Misdirected or long flames Generally caused by improper
for heater 1502 B draft, dirty burners, etc. Rectify the
cause
11 Flooding of the Scrubber High Vapor flow Higher amount of flashed gas from
1502 E. High delta P 1502 F. Check PIC-003 output, if
abnormal, take to manual and
adjust control valve opening to
normal. Rectify controller
12 Off-spec product from Improper Stripping Check the operation of the 1502B
Stripper 1501 E and rectify any problems. Check
reflux flow.
13 Flooding of product Stripper High Steam flow into column Check FIC-016 output, if abnormal,
1501 E take to manual and adjust opening
of Control valve to normal
position.
Rectify cause.
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14 High corrosion at Reactor Low Wash water rate Adjust wash water rate to the
Effluent Air cooler, design value. Wash water should
1502 C. be at least 20% liquid water at
injection point
The following APC Control strategies are implemented in Unit 15 APC Controller R152 & R153.
Throughput maximization.
Physical constraints
Charge Heater and Stripper Reboiler:
- Minimum Excess O2% in Flue Gas control.
- Maximum TST Control.
- Maximum Convection Section temperature Control
- Maximum Radiation Section Temperature Control
- Fuel Gas Pressure controller windup state control
Reactor
- Reactor inlet temperature control
- Reactor outlet control
Tank Feed level controller windup control.
Stripper Column Flooding (PDI) control.
Stripper overhead drum level controller windup state control.
Feed Surge Drum level control.
Please refer U15 APC Controller Operating Guidelines for further details.
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Corrosion in low alloy steel such as 5%, 7% and 9% caused by mercaptan usually happens
when the service temperature is high enough to decompose mercaptan. According to above
paragraph, above 650℉, the corrosion can be a problem in low alloy steel. Above that
temperature, stainless steel such as 321 and 347 can be used in high temperature mercaptan
service.
18.2 SULPHUR
Sulfur and sulfur compounds may attack carbon and low alloy steels at temperature above
500℉ (260℃) and nickel base alloys such as Alloy 600 at temperature above about 600℉
(315℃).
Sulfidic corrosion is most often associated with sulfur in crude oil (as organic sulfides and/or
as H2S). It can cause severe pitting and general wastage in carbon and low alloy steels at
temperatures exceeding 500℉ (260℃).
Heated sour oil, at temperatures exceeding about 850℉(455℃), becomes less corrosive due to
the liberation of corrosive species. Note that the McConomy curves show a maximum
corrosion rate at about 850℉ (455℃). At higher temperatures, the residual sour oil is less
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corrosive.
Coke builds up on the process surface, protecting those surfaces from sulfur corrosion.
Refractory linings are often used in both vessels and piping. A low iron-containing
refractory is required, since spalling of the refractory has been associated with iron
oxide contaminants in the refractory.
Pure liquid sulfur is stored in pits made of Type V concrete. Piping for liquid sulfur
is usually carbon steel. Heating, normally by steam tracing, is employed to keep the
sulfur molten. Liquid sulfur in the presence of air can be very corrosive to carbon
steel. Nitrogen blanketing or alloys such as Alloy 20 Cb-3 or Type 310SS are
employed.
14.1.36 Sulfidation
Sulfur and sulfur compounds may attack nickel-base alloys at temperatures above about 600℉
(315℃). The threshold temperature for this attack depends on both the process and the alloy
composition. Sulfur attack can assume several forms and can be quite severe, particularly
under reducing conditions. While pitting can occur, severe sulfidation usually involves either
inter-granular attack or fluxing due to molten sulfides.
When carbon steel is used, care should be taken the metal temperature not to exceed
300℃ (575℉) by using internal refractory lining. Alternatively alloy materials (5Cr,
7Cr, Type 321, and so on) may be substituted for the carbon steel.
14.1.37 Facilities under High Temperature Sulfide Service containing Mercaptan and Corrosion
Aspect
The light gas oil feed contains approximately between 1.05 and 1.5wt% sulphur. The feed
stream is charged with hydrogen upstream of Reactor Charge Furnace (1501B) and heating in
the shellside of 1501C1~C4 renders it corrosive to carbon steel. This necessitates the use of TP
321 stainless steel and TP 347 S.S clad for the exchanger shell and downstream pipework to the
Reactor Charge Furnace (1501B) to resist sulfidation attack.
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Heating the feed in 1501B to 362℃necessitates a further upgrade of material to Type 347 S.S.
for the heater tubing and connecting pipework to the Desulphurization Reactor (1501D/1551D)
18.3 HYDROGEN
Generally, steel can be damaged by hydrogen in high temperature and high pressure service. And
temperature is more significant factor than pressure, evaluating service environment. The failure
which it is called “hydrogen attack” is not happened in low temperature service. The temperature
limit is considered about 220℃. Above 220℃, hydrogen molecule (H2) can be decomposed to
hydrogen atom (H). It diffuses through metal and combine C. On the result, CH4 can be formed
in metal structure and fissuring occurs. Another deterioration mechanism, surface decarburization
also can be happened in similar ways. But fissuring is more harmful than surface decarburization.
Hydrogen damage like hydrogen attack is successfully controlled through the use of chromium-
molybdenum steel and austenitic stainless steels, appropriately selected for resistance at a
specific temperature and hydrogen partial pressure. Selection of materials for hydrogen service is
based on API Publication 941 “Steel for hydrogen service at elevated temperature and pressures
in petroleum refineries and petrochemical plants”.
Mercaptan service equipments are also on hydrogen service. And all of them are made of
stainless steel. So, failure by hydrogen damage can’t be a problem.
Hydrogen sulfide can cause sulfide stress corrosion cracking (SSCC), and hydrogen induced
cracking (HIC).
All of the above forms of hydrogen cracking begin with wet hydrogen sulfide corrosion, which
supplies hydrogen as a corrosion product when the sulfide ion combines with iron to form iron
sulfide.
The low-to medium-strength carbon steels are most resistant to SSCC. Piping and vessel
carbon steels are usually kept at specified minimum tensile strengths of 70 ksi (480 MPa) or
less. Higher strength steels are very susceptible to SSCC.
It is essential to control weld hardness. NACE RP0472 places a limit of 200BHN on carbon
steel weld metal hardness. Weld procedure qualification testing requires the heat affected
zone hardness not to exceed 248 VHN. NACE MR0175 contains detailed recommendations
on hardness and fabrication limitations for many of the metals and alloys encountered in
plant design.
Preheat and proper welding procedures are the appropriate measures for controlling
hardness associated with welding ordinary carbon steels, since the hardness of their
weldments is usually not a problem. Postweld heat treatment is usually not necessary unless
other crack-inducing agents (such as amines) or other cathodic poisons (such as cyanide)
are also present. In such cases, reduction of residual stress is usually to reduce the
susceptibility to stress cracking. For such severe SSCC services, postweld heat treatment is
recommended.
HIC occurs primarily in plate and plate products made of “dirty” steels. Such steel plates
contain excessive amounts of nonmetallic inclusions (primarily manganese sulfide),
flattened by the rolling. HIC rarely occurs in product forms other than plate or plate
products. The tendency of a steel to undergo HIC is aggravated by a banded ferrite-pearlite
microstructure.
Steel made from continuously cast steels (steels that are poured through a chilled mold and
solidify as an elongated slab) are typically less segregated.
Either hardness or heat treatments such as normalizing or postweld heat treatment do not
significantly influence HIC initiation.
HIC is minimized in plate and plate products by specifying a clean steel and a requirement
for inclusion shape control.
Forgings, castings and seamless pipe are considered to be essentially immune to HIC, since
they normally do not contain the flatttened non-metallic inclusions necessary to generate
HIC cracks.
Generally, killed carbon steel is used in wet H2S service. According to the amount of H2S and
H2S partial pressure, specialized requirements such as PWHT and limitation of impurity
elements (e.g. S & P) is required for carbon steel to prevent from occurring of SSC & HIC.
More details about material requirements in wet H2S service, please refer to ‘Specification for
materials in wet H2S service (sour service)’ (Doc. No. : 7J48N-00-00-55-003).
14.1.36 Equipment and Pipeline in Wet Sour Service and Corrosion Aspect
As the result of operation, S and N can be removed in the form of H2S and NH3 from the feed
stream containing sulfide and organic compounds. Stream containing these kind of
components is corrosive when condensed. When water vapors in the Desulphurization
Reactor (1501D/1551D) effluent cools and begins to condensate, a very corrosive mixture of
ammonia, hydrogen sulfide, water, and chloride (if present) is formed. Control of corrosion in
the piping downstream of the point of injection of wash water is accomplished by using the
proper design for the piping and heat exchangers, and by using the proper rate of injection of
water and controlling the content of constituents in the water that can accelerate corrosion.
Reactor Effluent Cooler (1502C), High Pressure Flash Drum (1502F), Stripper Overhead
Condenser (1505C), and Stripper Off Gas K.O. Drum (1505F) downstream line or equipment
itself can be on wet sour service. Equipment and piping which is marked as under wet sour
service condition on MSD (7J48N-64-64-56-001~4) is made to resist wet sour service
corrosion according to wet sour specification (Doc. No. : 7J48N-00-00-55-003)
A measure of the potential corrosivity of the reactor effluent stream with respect to wet
ammonium bisulfide corrosion is the Kp factor. This factor is defined as the product of the
ammonia and hydrogen sulfide mole percent in the dry stream entering the air cooler.
18.5 AMINE
The primary use of amines is in acid gas (CO2 and/or H2S) removal system. Amine solutions
can cause pitting and stress corrosion cracking in carbon steels. Post-weld heat treatment is
usually recommended for amine services, in which the amine concentration exceeds two wt.
percent, to avoid stress corrosion cracking. Exceptions are equipment and piping in
uncontaminated (i.e., fresh) amine service, in which stress corrosion cracking does not occur.
Rich amines (amines saturated with acid gas) can cause erosion corrosion in carbon steel
tubing and piping.
For systems used to remove CO2, stainless steels are usually required unless the amine system
is inhibited. Inhibited systems built of carbon steel have been shown to work well but are
subject to severe corrosion in CO2-rich vapor spaces if the system is not carefully designed
and operated.
For systems in which the acid gas is composed of at least five percent H2S, carbon steel is
commonly used. The iron sulfide surface scale that forms on carbon steel usually protects it
from CO2 corrosion.
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Generally, amine systems use carbon steel equipment. All new welded carbon steel equipment
and piping in amine service shall be PWHT to prevent stress corrosion/cracking of welds and
heat affected zone. Recent industry-wide corrosion/cracking experience has shown this to be
especially important.
Equipment exposed to amine streams is Recycle Gas Scrubber (1502E) which is used to
remove H2S remaining in the vapor. Corrosion is likely to be more severe in amine systems
removing only carbon dioxide (CO2). Amine solutions containing mixtures of H2S and CO2,
or H2S alone, are progressively less likely to require higher alloy construction materials.
Moisture and air react readily with iron sulfide to form polythionic acids in refinery equipment
during downtime. The acids attack sensitized stainless steel and cause intergranular cracking.
Furthermore, austenitic stainless steels exposed to chlorides and moisture are susceptible to stress
corrosion cracking. To prevent these types of corrosion, austenitic stainless steel piping, heater
tubes, and exchangers should be internally washed with a dilute alkaline solution immediately after
shutdown if the equipment is to be opened or cannot be kept tight and internally dry during the
downtime. The alkaline rinse also prevents the ignition of pyrophoric sulfide or iron deposits
exposed to air.
The deposis of ammonium bisulfide salt (NH4HS) can lead to exchanger and piping fouling and
under deposit corrosion. Onstream intermittent water slugging may be employed in carbon steel
equipment to remove the ammonium bisulfide salt deposits.
Erosion/Corrosion of the piping and heat exchanger is minimized by the limiting the velocity in the
equipment downstream of the water injection point. The velocity should be limited to 6m/s max. for
carbon steel, and 9m/s for high alloy steel.
Reactor Effluent Cooler (1502C) and Stripper Overhead Condenser (1505C) outlet line is the first
condensing point of corrosive gas. So corrosion monitoring device should be installed on these line
to monitor corrosion and corrosion rate.
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This section provides the effluents from the No.2 GO Hydrotreater (Unit 15). Vapor releases, liquid
discharges and solid discharges are provided separately.
Total amount of 13,956 kg/hr of flue gas from the Reactor Charge Furnace (1501B) and the
Stripper Reboiler (1502B) is released to atmosphere with the following composition.
Emission
Heater No. NOx (mg/Nm3) SOx (mg/Nm3) Particle (mg/Nm3) Remarks
1501B/1502B 322.9 12.4 <5
Regulation 360 500 5
Sour Water
No effluents; Sour waters from the HP Flash Drum (1502F) and the LP Flash Drum (1503F)
are sent to the Sour Water Stripper Section in Unit 11.
No effluents; Spent caustic from the HP Flash Drum (1502F) is sent to the Amine Regeneration
Unit (Unit 49).
Slops
No effluents; Slops from the Gas Oil Trim Cooler (1504C) is sent to the Light Slop Tanks
(2121F, 2145F).
The catalyst will be replaced by fresh catalyst at end of its life time. Total of 88.4 m3 will be
disposed during each catalyst replacement.
During start-up the metal-oxides will be converted to metal-sulfides, which is active state of
the catalyst. During operation the catalyst will be deactivated due to coking and accumulation
of contaminants present in the feed.
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In addition practically any contaminant present in the feed (arsenic, lead etc) will be removed
and accumulated on the catalyst. These contaminants have not been specified and it is therefore
impossible to predict these accurately.
Typically the amount of fines from the catalyst screening is less than 2-3 wt%. Depending on
the content of solid contaminants in the feed, the fines will mainly be catalyst fines and hence
have the same composition as the catalyst mentioned above.
Almost all hydrocarbons and chemicals can be dangerous if improperly handled. Therefore
the operators should be thoroughly acquainted with the hazardous properties of all materials
in use and should be properly drilled in the correct procedure for these materials.
Because of the hazardous nature of the hydrocarbons and chemicals used in the unit, it is
mandatory to make regular inspections of all equipments, exchangers, vessels, piping and
valves. Any leaks must be reported immediately and action, which may include unit shut-
down, started as fast as possible.
The operators should be familiar with the location and use of fire fighting equipments :
hydrants, steam lances, water spray, monitors, extinguishers; and of safety equipments, safety
showers, eye bath and all other emergency equipments which may be installed in the unit.
In addition, each operator should be thoroughly familiar with first aid measures and should be
able to take appropriate action in use of an incident.
Periodic practice drills and more especially fire fighting drills should be used to reinstruct the
operators in the hazards involved and the proper emergency action required so as to ensure
the maximum protection both for personnel and equipments.
Refer Emergency Response plan procedure QQP-R-HS-QP001 for more details on the
Emergency scenarios, Assembly points layout, Emergency call out chart, Emergency contact
list, Firefighting equipment list, safety equipment list and Incident command guide.
All hydrocarbons involve a fire and explosion hazard. The most hazardous liquid petroleum
products are those having flash point below 55 C : crude oil, gasolines, etc. Light
hydrocarbons at ambient temperatures can produce vapours which are heavier than air and
form an explosive mixture with air. Therefore, a special care should be given to any
operation where that risk occurs, such as draining or venting of pumps or vessels and
sampling.
Any leak must be repaired as soon as possible and preventive measures taken immediately
(water spray, steam or nitrogen hoses, sand on liquid pools, etc).
In addition to the fire and explosion hazards, the operators must be also thoroughly
acquainted with the hazards of hydrogen sulfide which can cause death even in a very low
concentration. Nitrogen is more especially dangerous as it is generally unsuspected since it is
the main component of atmospheric air. For this reason the danger of nitrogen must be
emphasized and the operators instructed in the procedures and precautions to be taken before
entering a vessel previously inerted.
Gas detectors are provided for the unit to monitor the presence of explosive or flammable gas.
This is an instrument for indicating to the operator the presence of a mixture of explosive or
flammable gas. In general, the unit area, even during normal operation, should be monitored
with gas detector tests at schedule intervals and if a dangerous amount of gas is detected,
steps should be taken at once to determine the source and eliminate it.
When specific materials are handled where the maximum allowable concentration is low,
such as hydrogen sulfide (H2S), specific detectors for these materials must be provided.
In case a leak develops in a line (or equipment) carrying a volatile hydrocarbon liquid or
vapor, the leak should be covered with a blanket of steam until repairs are made or the
pressure is reduced. Repair of leak, no matter how small, should not be delayed.
Hydrogen Sulphide is one of the more dangerous materials in industry. In its handling,
two types of hazards must be taken into account, it extreme toxicity and its explosive
nature when mixed with air or sulphur dioxide.
burning eyes, and clouded vision. A concentration of 100 ppm of hydrogen sulphide in
air can cause coughing, irritation and loss of smell after 2-15 minutes and drowsiness
after 15-20 minutes. A concentration of 1000 ppm of hydrogen sulphide in air can
make one unconscious at once with early cessation of respiration and death in a few
minutes.
Some precautions against poisoning to be taken in working with hydrogen sulphide are:
13) Closed-in areas should be well ventilated, preferably with a forced draft.
14) Equipment containing hydrogen sulphide should be tightly sealed. Any leaks
should be repaired immediately.
15) At seals or stuffing boxes where leaks might occur during normal operation, means
should be provided for venting the escaped gas to a safe location.
17) Masks furnishing pure air should be worn by personals who are likely to be
exposed to the gas.
18) Personnel who may be exposed to low concentration of the gas should frequently
retire to areas of fresh air.
19) As a good safety measure personnel should learn to recognize the early symptoms
of hydrogen sulphide poisoning.
A simple test with lead acetate solution on white paper will indicate the presence of
hydrogen sulphide. Depending on the concentration, the paper will turn yellow or
brown.
Monoethanolamine
Certain metals are attacked by monoethanolamine, notably copper and its alloys, iron,
aluminum and its light alloys.
Glass is equally suitable for smell quantities but the demi-johns should he protected by
a stronger metallic envelope which is suitable padded.
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[Link] Hazards
wwww) Toxicology
Monoethanolamine and its concentrated solutions are caustic with respect to the
skin and mucous membranes both eye and respiratory. The concentration of the
vapour limit in air is 3 ppm, 8 mg/m3.
[Link] Recommendations
At ambient temperature, the product is only slightly volatile and slightly inflammable.
The risk of contamination of work areas is unlikely. Nonetheless, because it is caustic
on the skin, certain precautions must be taken in storage and in use.
In particular :
Avoid all contact with the skin and use protective clothing.
In the event of leaks or spillage, add sodium bisulphate, dilute with water,
neutralize and put to sewer with a large volume of water. In the event of large
spillage, recover and incinerate.
Corrosion Inhibitors
Nature :
Precautions :
Avoid contact with skin. Contaminated clothes must not be worn for a prolonged
period. Eyes should be protected.
First aid :
In case of accidental contact with the skin wash with soap and water.
Precautions :
Some of the light amines are dangerous to health by inhalation, ingestion and by skin
adsorption, so :
Wear protective clothing, namely, goggles, resistant rubber gloves and proofed
body garments. Change any contaminated clothing immediately and wash any
areas in contact thoroughly with plenty of soap and water.
Ensure good ventilation and avoid frequent or lengthy inhalation of the vapors. In
the event of spillage in a confined atmosphere, avoid breathing vapours and use a
respirator.
The solvent is inflammable and the product must be kept away from flames and
naked 1ights.
Fire Hydrant: 8
Foam/water Monitor: 2
Deluge Skid: 1
Hydrocarbon Detector: 9
Portable DCP: 18
Wheeled DCP: 1
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SCBA Set: 1
It is important to monitor the feed and product qualities regularly in order to protect the unit from
poor feed and to evaluate the performance of the unit. A Recommended Laboratory Test Schedule
has been provided in the previous section to illustrate the typical control analyses, test methods and
frequency of sampling.
Since feed quality is of utmost importance, a few comments are provided on this subject.
nn) Vigilant feed monitoring, especially during times of change in feedstock or in operating
condition of the up-stream unit, is necessary to protect the equipment, especially catalyst from
poisoning due to metals and/or carbon deposition. In general, a deterioration in feed quality
can be caused by up-set or abnormal condition of the up-stream unit.
oo) It is preferred that the feed tanks be used as surge and unit be fed directly from the up-stream
units. In any event, care must be taken to keep the tank air free, i.e., gas blanketed with fuel
gas or nitrogen.
The dissolved oxygen picked up in a non-blanketed feed tank will, in combination with the oil,
foul the combined feed exchangers, heater, and the catalyst bed, increasing the reactor pressure
drop. To avoid this type of fouling, it is necessary to monitor the blanketing system
periodically ensure it is working properly.
It is recommended to find that daily operating plots are the best technique for unit performance
evaluation. The unit performance interpretation technique must, therefore, be chosen such that
these factor are normalized before performance is evaluated.
The following data is generally plotted :
Reactor temperature
Reactor pressure
Feed Quality
H2/HC Ratio
LHSV
Catalyst Protection, Aging and Poisons
From such daily operating plots, any change in unit performance that is not accounted for by a
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corresponding change in unit operating variables may be readily recognized and corrective action
taken, if necessary.
Monitoring the heater has taken on more emphasis as refiners wish to maximize their run lengths by
maintaining the lowest possible tube temperature for a given operation. This not only minimizes
fuel costs, but also tends to increase heater tube life. One can see that the following can readily
contribute to a shortened tube life and will require premature retubing.
Indeed this list is not complete and several other items could be added. In order to cover the subject
more thoroughly, refer to the Heater vendor’s detail instruction.
The operator should survey the heater visually at least once per shift to ensure that :
Along with the visual check, a calculation of heater duty should be made at least once per day
during normal operation.
Monitoring the heater temperatures should be done hourly during normal operation and should
include all inlet and outlet temperatures and all tubeskin temperatures. IN NO EVENT SHOULD
THE HEATER BE OPERATED ABOVE THE MAXIMUM TUBESKIN TEMPERATURE OR
ABOVE THE DESIGN HEATER DUTY.
Following is a summary of the expected tube skin temperatures.
In general, corrosion rate of the metal will depend on the operating conditions with the nature of
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fluids. However, typical corrosion rates vs. operating temperatures are given on attached Figures as
a reference.
Continuous monitoring of the wash water injection with proper control is recommended.
A constant supply of wash water is necessary to remove ammonium hydrosulfide (NH4HS) from
the reaction products. The water injection rate is typically between 3 and 5 vol.% of the fresh feed
rate. The exact injection rate depends on the amount of the nitrogen in the feed. This also ensures
that ammonia is removed from the recycle gas, as it is a temporary catalyst poison, and that
ammonium hydrosulfide does not deposit in the reactor products condenser.
Should water not be available to dissolve the ammonium hydrosulfide, it can form a solid at the
operating temperatures of many air fin coolers. The salt formation temperature has been related to
the concentration of ammonia and hydrogen sulfide in the gas stream, increasing as the product of
the partial pressures of H2S and NH3 increase. Therefore, removal of ammonia or hydrogen sulfide
will lessen the chances of salt formation.
Should salt deposits be a problem, Hydrotreating units are normally designed to allow the operator
to add wash directly to each bundle in the fin fan cooler.
During the cycle, coke will build up on the catalyst surface within the pores reducing the reaction
surface and consequently the activity. An adjustment will be required on the reactor inlet
temperature to compensate for this activity loss. In general, the difference between start of run and
end of run inlet temperatures could be as much as 30℃. This change is very gradual over typically a
2-3 year period.
Detail information for the catalyst performance from Manufacturers, if available, will be included in
this section later.
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Figure 1
a)
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b)
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c)
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d)
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e)
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f)
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Refer to document
7J48N-11-15-20-001F5
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7J48N-15-00-30-005 Cause & Effect Diagram And Common Trouble & Shutdown Alarm
List
Description
Drawing No.
Hydrogen sulfide is one of the more dangerous materials in industry. In its handling, two
types of hazards must be taken into account, its extreme toxicity and its explosive nature
when mixed with air or sulfur dioxide. Although at first this concentration can be readily
recognized by its odor, hydrogen sulfide may partially paralyze the olfactory nerves to the
point at which the presence of the gas is no longer sensed. Hence the odor of the gas,
strongly unpleasant though it is, is not a reliable safeguard or warning against its poisonous
effect.
So the H2S monitoring system is installed in the area of possible sources of H2S leakage as
follows:
The monitoring system will be set to sound alarms when the detected H2S concentration
reaches 5 ppm.
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26.2 COMPRESSOR
When shutting down a heater with austenitic stainless steel tubes, it is crucial to ensure the absence of both oxygen and water vapor to prevent corrosion. This requires maintaining a minimum firebox temperature of 205°C (400°F) during depressurization and purging stages. The system should be purged and filled with nitrogen to reduce oxygen levels well below 100 mol ppm before cooling the heater. Maintaining a dry air environment during cool periods further prevents oxygen ingress and conforms to preventative measures against sulfide scale and corrosion .
The specifications for the catalysts used in the LGO Hydrotreating unit (Unit 15) include the TK-554 as the principal desulfurization catalyst with a 1.3 mm three-lobed structure, sock loaded in both reactors. It has a high density of 810 kg/m³. The TK-554 catalyst design is supported by a graded bed system in the reactors, featuring TK-10 and TK-550 catalysts alongside ceramic inerts. The reactors incorporate a 19 mm inert base topped with 75 mm layers of 6 mm and 3 mm inerts, ensuring stable catalyst support and minimizing pressure drop .
Sulfide scale in stainless steel equipment can lead to severe corrosion issues, notably the formation of polythionic acids when exposed to moist environments with trace oxygen. These acids cause intergranular corrosion cracking, particularly compromising equipment integrity. As a result, maintenance protocols necessitate preventive measures, including regular cleaning with soda ash solutions and ensuring environments with minimal moisture and oxygen exposure. These practices are critical to prevent long-term damage and operational failures in the Hydrotrating units .
When activating new catalyst layers after replacing a small percentage (less than 10%) of the catalyst, the procedure involves drying and purging the reactor with nitrogen until the oxygen level is below 0.5 volume percent. The starting temperature is maintained at approximately 150°C (300°F) to minimize catalyst reduction. The pressure is raised in controlled increments using natural or make-up gas, ensuring tight system checks at each pressure level .
During the start-up of the LGO Hydrotreating unit, natural gas is used initially for pressure control. The process involves gradually raising the pressure in 7 barg steps while using the HP flash drum pressure controller to check for leaks at each step. Natural gas aids in pressure control of 1701F. Following this, hydrogen via a small make-up line helps raise the system pressure to operating levels. The reactor is pressurized to its normal operating pressure while avoiding the ductile-brittle transition temperatures of structures which could limit pressure. Additionally, the design involves bypassing the recycle gas scrubber during this phase .
Handling austenitic stainless steel, particularly post-hydrocracking or hydrodesulfurization, presents challenges due to possible sulfide scale formation. This scale can lead to polythionic acid corrosion if not managed. Therefore, hydrostatic testing and cleaning should include neutralization steps using diluted soda ash solutions to prevent corrosion. A soda ash protective film should be allowed to dry on the surfaces post-cleaning to avoid air and moisture contact, minimizing the risk of intergranular corrosion .
Managing pressure variances involves using a gradual pressure increment process via the HP flash drum pressure controller, ensuring leaks are checked at every step. This approach aims to safely ascend to operational pressures while respecting design limitations, such as avoiding ductile-brittle transition issues. Controlled pressurizing steps facilitated by natural or make-up gas ensure system integrity before full operational pressures are reached, and a comprehensive leak-checking process is critical .
When opening an exchanger with austenitic stainless steel, it's essential to flood both shell and tube sides with a soda ash solution to prevent air contact. Maintain a continuous nitrogen purge throughout the maintenance process to eliminate air presence. After maintenance, allow a protective soda ash film to dry on the surfaces rather than rinsing with water, which ensures ongoing protection against corrosion and deterioration .
Inert materials in the reactor, such as 19 mm ceramic spheres and graded bed systems, play a supportive role in stabilizing the catalyst operations by providing structural support and minimizing pressure drop across catalyst beds. These inerts create a stable physical environment, protecting catalysts from fouling, facilitating even flow distribution, and enhancing overall catalytic efficiency. The use of a layered system with varying inert sizes aids in improved catalyst bed integrity and operation sustainability in the LGO Hydrotreating unit .
The ductile-to-brittle transition temperature (DBTT) significantly influences reactor operations, imposing limits on starting pressures during cool temperatures to avoid material brittleness and potential failure. Understanding DBTT is critical for determining safe operational limits, informing gradual pressurization protocols while ensuring complete material toughness. Start-up procedures must account for these thresholds, employing pressure control measures that remain within the safe temperature range to prevent catastrophic structural failures and ensure material integrity during operation transformations in the reactor system .









