Vacuum Distillation Column Design Report
Vacuum Distillation Column Design Report
DESIGN PROJECT
Semester 2 Session 2018/2019
Group No. 8
Supervisor Dr. Muhamad Fazly Bin Abdul Patah
Course Coordinators Professor Dr. Wan Mohd Ashri Bin Wan Daud
Dr. Fathiah Binti Mohamed Zuki
Submission Date 25 April 2019
Table of Contents
i
List of Figures
Description Page
Figure 3 Liquid flow arrangement as a function of liquid flow rate and column 7
diameter
Figure 4 Weir length correlation in the function of downcomer area, column area 8
and column diameter
Figure 5 Relationship between K2, weir height and minimum height over weir 8
Figure 8 Empirical correlation showing the relationship between ratio of net area to 10
perforation area and ratio of hole pitch to hole size in graphical plot
ii
List of Tables
Description Page
iv
List of Abbreviations
𝐴a Active area m2
𝜃c Angle of chord °
𝜃d Angle subtended by the edge of plate °
𝐴ca Area of calming zone m2
𝐴c Area of column m2
𝐴u Area of unperforated edge strip m2
𝜇 Average liquid viscosity of the feed stream cP
𝑊 Bottom product flow rate kmol/hr
ton/hr
𝐴m Clearance area under the downcomer m2
𝐸o Column efficiency %
Dc Column diameter m
𝐷 Distillate product flow rate kmol/hr
ton/hr
𝐾j Distribution coefficient of heavy key component
𝐾i Distribution coefficient of ith component
𝐴d Downcomer area m2
ℎb Downcomer backup mm
𝑡r Downcomer residence time s
ℎd Dry plate pressure drop mm
𝑞 Feed liquid fraction
𝐹 Feed rate kmol/hr
ton/hr
𝑢f Flooding velocity m/s
𝐹LV Flow factor
Ψ Fractional entrainment
𝐺 Gilliland coefficient
ℎm Head loss in downcomer mm
ℎap Height of bottom edge of apron above plate mm
𝐻t Height of column m
𝐴h Hole area m2
𝑑h Hole diameter mm
𝑙p Hole pitch mm
𝜌L Liquid density kg/m3
𝜌L,i Liquid density of ith component kg/m3
𝐿 Liquid rate kmol/hr
ton/hr
𝐿T Liquid rate for rectifying section ton/hr
v
𝐿B 𝐿W Liquid rate for stripping section ton/hr
𝜇i Liquid viscosity of ith component cP
ℎb,max Maximum downcomer backup mm
ℎ𝑜𝑤,𝑚𝑎𝑥 Maximum height over weir m
𝑢max Maximum vapour velocity m/s
𝑙s Mean length m
𝑙c Mean length of calming zone m
ℎ𝑜𝑤,𝑚𝑖𝑛 Minimum height over weir m
𝑁min Minimum number of stages
𝑅min Minimum reflux ratio
𝑢min 𝑢h Minimum vapour velocity m/s
𝑀i Molecular weight of ith component kg/mol
𝑥[Link] Mole fraction of heavy key component in bottom product
𝑥HF Mole fraction of heavy key component in feed stream
𝑥D,hk, 𝑥HD Mole fraction of heavy key component in distillate
𝑥I,D Mole fraction of ith component in distillate
𝑥I,F Mole fraction of ith component in feed
𝑥𝐵,𝑙𝑘 𝑥𝐿𝑊 Mole fraction of light key component in bottom product
𝑥LF Mole fraction of light key component in feed stream
𝑥D,lk Mole fraction of light key component in distillate
𝐴n Net area m2
𝑁e Number of stages in rectifying section
𝑁s Number of stages in stripping section
𝑁 Theoretical number of stages
𝐴p Total Area for Perforations m2
𝑃 Operating pressure of distillation column atm
𝑇 Operating pressure of distillation column K
𝑅 Optimum reflux ratio
𝐶o Orifice coefficient
ℎt Pressure drop per plate mm
Pa
𝛼lk Relative volatility of light key component
𝛼ij Relative volatility of ith component relative to heavy key
ℎr Residual head mm
𝐶 Tray spacing m
𝜃 Underwood coefficient
𝜌V Vapour density kg/m3
𝜌V,i Vapour density of ith component kg/m3
vi
𝑦i Vapour mole fraction of ith component
𝑃sat,i Vapour pressure of ith component bar
𝑉 Vapour rate kmol/hr
ton/hr
𝑄 Volumetric flow rate m3/hr
𝑢w Weeping rate m/s
𝐾2 Weir flow coefficient
ℎw Weir height m
𝑙w Weir length m
𝑤c Width of calming zone allowance m
𝑤u Width of unperforated edge strip allowance m
vii
1.0 Chemical Engineering Design
1.1 Operating Description
Distillate
Temperature 215˚C
Pressure 0.010 bar
Component mass flowrates
(kg/hr)
Palmitic acid 234.30
Stearic acid 324.58
Oleic acid 2000.46
Feed Linoleic acid 270.66
Temperature 242˚C
Pressure 3 bars
Component mass flowrates
(kg/hr)
Palmitic acid 234.73
Stearic acid 334.38
Oleic acid 2023.46
Linoleic acid 272.21
Crude Palm 289.15
Kernel Oil
Bottom
Temperature 258˚C
Pressure 0.013 bar
Component mass flowrates
(kg/hr)
Palmitic acid 0.44
Stearic acid 9.80
Oleic acid 23.00
Linoleic acid 1.55
Crude Palm 289.15
Kernel Oil
The column is operated on a continuous basis. As high temperature can cause severe damage to
the column, the operating pressure of the column will be reduced to 0.013 bar to lower the
boiling point of the components. The operating temperature of the column will be at an average
temperature of 258˚C. This is because the feed has been set to operate at a temperature in
between the boiling points of the components.
The temperature of distillate and bottom product streams will be slightly lower and higher than
bubble point temperature, respectively as total condenser and partial reboiler are being used.
The factors discussed below influence the choice between trays & packings. As these are
guidelines for selection of trays or packings for a particular service, it is recommended to
analyse each design case on its own merit for selection. Below is the comparison between these
two types of contacting device:
2
Table 1: Comparison of type of distillation column.
Packed Bed Column Plate Column
small-diameter columns (less than 0.6m) variable liquid and/or vapour loads
more choices in materials of construction low liquid rates · large number of stages
for packings especially in corrosive and/or diameter
service (e.g. plastic, ceramic, metal alloys)
high liquid residence time
lower pressure drop (important in vacuum
distillation) dirty service (plate columns are easier to
clean)
less liquid entrainment · low liquid hold-
up, especially suitable for thermally presence of thermal or mechanical stress
sensitive material due to large temperature changes which
might lead to cracked packings
foaming liquids can be handled more
readily (less agitation of liquid by the exotherms requiring cooling coils inside
vapour) column
Tray column is selected for the design of DC-203 as it is the most common used in large-scale
distillation process as well as its easiness to be cleaned. Also, it can be observed from the mass
flowrates in Figure 1 that the tray column will be more suitable. This is because the flow rates in
this process are large and these will require a large diameter. In cases when the diameter is large
it is more convenient to have plates or trays.
3
• Light Key: Oleic acid (A)
• Heavy Key: Trilaurin (B)
Where, 𝛼𝑖𝑗 = relative volatility of ith component with respect to heavy component
𝐾𝑖 = distribution coefficient of ith component
𝐾𝑗 = distribution coefficient of heavy component
Distribution coefficient for each component, however, was determined from the ratio between
the saturated vapor pressure of the component and the total operating pressure of the column.
𝑃𝑠𝑎𝑡,𝑖
𝐾𝑖 = Eq. (2)
𝑃
The saturated vapor pressure for the fatty acids was determined from Antoine equations based on
Antoine coefficients obtained from NIST Chemistry WebBook.
𝐵
𝑃𝑠𝑎𝑡,𝑖 = 𝑒 [𝐴−𝑇+𝐶] Eq. (3)
The relative volatility of all the components are tabulated in Table 2 in Appendix A.
𝑥 𝑥
𝑙𝑜𝑔[( 𝐴 ) ( 𝐵 ) ]
𝑥𝐵 𝐷 𝑥𝐴 𝑊
(𝑛 + 1)𝑚 = Eq. (4)
log 𝛼𝐴𝐵
4
Where:
αAB : The relative volatility of light key to heavy key
𝑥𝐴𝐷 : The mole fraction of light key in the distillate
𝑥𝐵𝐷 : The mole fraction of heavy key in the distillate
𝑥𝐵𝑊 : The mole fraction of heavy key in bottom
𝑥𝐴𝑊 : The mole fraction of light key in bottom
The minimum number of stages determined from Fenske equation is 6 stages with the necessary
parameters obtained from mass balance sheet.
𝛼𝑖 · 𝑥𝑖,𝐹
∑𝑖 =1−𝑞 Eq. (6)
𝛼𝑖 − θ
5
1.7 Theoretical Number of Stages, N
By using the information obtained from Fenske and Underwood equation, Gilliland correlation is
used to determine theoretical number of stages to achieve desired degree of separation. Gilliland
correlation is given by,
𝑁−𝑁𝑚𝑖𝑛 1+54.4𝐺 𝐺−1
= 1 − exp[(11+117.2𝐺) · ( 𝐺0.5 )] Eq. (7)
𝑁+1
𝑅−𝑅𝑚𝑖𝑛
𝐺= Eq. (8)
𝑅+1
Eo is applied throughout the whole column, i.e. every tray is assumed to have the same
efficiency. There are several correlations that are used to predict column efficiency, one of the
most widely used correlation is O’Connell expression that can be expressed in the form;
Eo (%) = 51 – 32.5 log (μavg ·αLK ) Eq. (9)
μavg = ∑ 𝑥𝑖 · 𝜇𝑖 Eq. (10)
Modified versions of Andrade equation, which introduce one or more constants to improve the
fit to the experimental data have been used to determine viscosities of components. One of the
correlations with higher order terms used is;
𝐵
𝑙𝑛µ𝑖 = 𝐴 + + 𝐶𝑇
𝑇
6
From the information obtained from column efficiency, actual number of stages can be obtained.
The results are summarized in Table 5 in Appendix A.
𝑁𝑎 = 𝑁𝑒 + 𝑁𝑠 Eq. (12)
Both equations can be solved simultaneously for Ne and Ns thus determining the feed location.
The results of the correlation are summarized in Table 6 in Appendix A.
7
2.2 Column Diameter
The column diameter must be selected so that flooding does not occur, however at the same time
vapor velocities that are high for greater plate are needed. The column diameter is determined
from the flooding correlation for a chosen plate spacing. The superficial vapour/gas velocity
(𝑈nf) at flooding through the net area relates to liquid and vapor densities according to Fair’s
correlation.
𝐶sb is an empirical constant, depending on tray spacing and can be estimated against the flow
parameter (𝐹LG) based on mass flow rate of liquid (𝐿) and vapor (𝑉).
The liquid density is a function of temperature and determined through coefficients. The gas
density on the other hand is determined from aspen.
𝜌𝐿 = ∑𝑖 𝑥𝑖 · 𝜌𝐿,𝑖 Eq. (14)
𝜌𝑣 = ∑𝑖 𝑦𝑖 · 𝜌𝑣,𝑖 Eq. (15)
Where, 𝜌𝐿.𝑖 = liquid density of ith component (kg/m3)
𝜌𝑣.𝑖 = gas density of ith component (kg/m3)
𝑥𝑖 = liquid mole fraction of ith component
8
𝑦𝑖 = vapor mole fraction of ith component
Typically, the design velocity (𝑈n) through the net area is about 85% of flooding velocity (𝑈nf)
It is a common practice to have uniform tower diameter in all sections of the column even
though the vapor/gas and liquid loadings are expected to be different to minimize the cost of
construction.
The diameter of column is calculated by the following steps;
ii. Net Cross-Sectional Area for Vapor Flow Above the Tray, An
Following the recommendation of estimating column size based on 85% flooding, the
required net tray area is:
1 𝑄
𝐴𝑛 = (0.75) (𝑈 ) Eq. (17)
𝑛
Where, 𝑈𝑛 = design velocity (m/s)
4𝐴𝑡
𝐷𝑐 = √ Eq. (19)
𝜋
The summary of the outcome from these calculations is given in Table 7 in Appendix A.
9
3.0 Tray Design
The tray design of DC-203 is mostly derived from empirical formulas used in fluid mechanics in
graphical means. Tray design comprises of selection of tray type, dimensions of single tray,
liquid flow pattern over the plate, weir design and hole design alongside with verification that
weeping conditions will not take place during normal operation of DC-203.
i. Sieve Plate: This type of plate is the simplest type of cross-flow plate. The vapour passes
the holes in the plate and the liquid is retained on the plate due to the vapour flow. In
occasions when flow rates are low liquid weeps through the holes, and this reduces plate
efficiency. Usually the perforations are small holes however, in some cases larger holes
and slots are also made use of.
ii. Bubble-cap Plate: This type of plate is the most traditional and oldest type of cross flow
plate. Various designs have been developed. For most applications the standard cap
design would be specified. In this type of plate, the vapour passes up pipes which are
known as risers. The risers are enclosed by a cap with a jagged edge or slots. Risers
ensure that a level of liquid is maintained on the tray at all vapour flow-rates.
10
Figure 4: Diagram of a Bubble-cap Plate
iii. Valve Plate: This type of plate is very much like sieve plates however, the only
difference being that they have large diameter holes which are covered by movable flaps.
When the vapour flow increases the movable flaps lift. Valves plates can operate more
efficiently at lower flow rates in comparison to sieve plates. At low flow rates the valves
in the valve plate’s close.
When selecting the plate type many factors are considered including cost, capacity, operating
range, efficiency and pressure drop. Of the three types sieve plates are the cheapest and are
satisfactory for most applications. The operating costs of sieve plates and the pressure drop is
lower compared to the other types of plates. For these reasons the selected type of plate for the
distillation column is sieve plates.
11
governing equations merely comes from rule of thumb. The tray dimensions along with
governing equations are summarised in Table of Appendix B
12
Figure 7: Selection of liquid flow arrangement
ii. Weir length: With segmental downcomers the length of the weir fixes the area of the
downcomer. The chord length will normally be between 0.6 to 0.85 of the column
diameter. A good initial value to use is 0.77, equivalent to a downcomer area of 12 per
cent. The relationship between weir length and downcomer area is given in Figure 8 .
13
Figure 8: Relation between downcomer area and weir length
iii. Weeping condition: Weeping occurs at low vapor/gas flow rates. At low vapor flow
rates, liquid start to leak/rain through the perforation (called weeping). The weeping
tendency increases with increasing fractional hole area and liquid flow rates. The
weeping rate can be determined from empirical graphs as suggested by Coulson &
Richardson
Figure 9 shows the relationship between K2, weir height and minimum height over weir.
From Table 9 in Appendix B, both umax and umin are well above the weeping rate, therefore
weeping will not occur during normal operation of DC-203.
14
Figure 9. Relationship between K2, weir height and minimum height over weir
𝐶𝑜 can be obtained from Figure 10; which has been adapted by Liebson et al. (1957)
15
Figure 10: Discharge coefficient, sieve plates (Liebson et al., 1957)
16
i. Criteria 1: Downcomer back-up must be less than half of the tray spacing
The downcomer area and plate spacing must be such that the level of the liquid and froth in
the downcomer is well below the top of the outlet weir on the plate above.
In terms of clear liquid, the downcomer back-up is given by:
ℎ𝑏 = (ℎ𝑤 + ℎ𝑜𝑤 ) + ℎ𝑡 + ℎ𝑑𝑐 Eq. (24)
Head loss in the downcomer, ℎ𝑑𝑐 is estimated using the equation given by Cicalese et al.
(1947)
𝐿 2
ℎ𝑑𝑐 = 166 [𝜌 𝑤𝑑 ] Eq. (25)
𝐴 𝐿 𝑚
Where, 𝐿𝑤𝑑 = liquid flow rate in downcomer (kg/s)
𝐴𝑚 = downcomer area (m2)
ii. Criteria 2: Downcomer residence time must be greater than 3 s for satisfactory contact
between vapor and liquid.
Enough residence time must be allowed in the downcomer for the entrained vapor to
disengage from the liquid stream. The downcomer residence time is given by:
𝐴𝑑 ℎ𝑏𝑐 𝜌𝑙
𝑡𝑟 = Eq. (26)
𝐿𝑤𝑑
Where, ℎ𝑏𝑐 = clear liquid back-up (m)
iii. Criteria 3: Fractional entrainment should be less than 0.10 to prevent liquid
entrainment within the vapor phase rising upwards.
Fractional entrainment, ψ, can be estimated from the correlation given by Fair (1961), Figure
11.29, as a function of the liquid-vapor factor FLV, with the percentage approach to flooding
as a parameter. The percentage flooding is given by:
𝑢𝑛 (𝑏𝑎𝑠𝑒𝑑 𝑜𝑛 𝑛𝑒𝑡 𝑎𝑟𝑒𝑎)
%𝐹𝑙𝑜𝑜𝑑𝑖𝑛𝑔 = Eq. (27)
𝑢𝑓
Where, 𝑢𝑛 = actual velocity based on net area (m/s)
𝑄
𝑢𝑛 = 𝐴 Eq. (28)
𝑛
By referring to hb, tr and ψ in Table 11, all the three criteria were satisfied and therefore
flooding will not occur in DC-203 operation.
17
3.8 Hole Design
i. Hole Diameter:
The plate hole diameters (𝑑h) from 3 to 12 mm are commonly used. The bigger sizes are
susceptible to weeping. The holes may be drilled or punched, and the plate is fabricated from
stainless steel and other alloys than carbon steel. For this design, 5 mm hole diameter is used.
Figure 11 and Figure 12 portray the graphical determination of angle of chord and ratio of
hole pitch to hole size. Table 12 in Appendix B summarizes the information obtained from
the calculation performed for this section. The hole pitch determined from the empirical
correlations shows that it is more than twice the hole diameter. Therefore, a stable operation
of DC-203 can be maintained.
Figure 11: Relation between angle subtended by chord, chord height and chord length
18
Figure 12: Relation between hole area and pitch
19
References
20
APPENDIX A SUMMARY OF CHEMICAL ENGINEERING DESIGN OF DC-203
Table 2: Summary of relative volatilities of all the chemical components present in DC-203
system
Chemical Component Relative Volatility, α
Palmitic Acid 5.732883324
Stearic Acid 3.044142597
Oleic Acid 3.569782491
Linoleic Acid 4.685529004
Tricaprylin 46.50067814
Tricaprin 6.028940344
Trilaurin 1
Trimyristin 0.159281418
Tripalmitin 1.79061E-06
Triolein 0.00053738
A
Table 6: Summary of outcomes from Kirkbride approximation
Variable Equation Value
Number of stages in 11
rectifying section, Ne Eq. (11) & (12)
Number of stages in 5
stripping section, Ns
Feed Tray location - 11th stage
B
APPENDIX B SUMMARY OF TRAY DESIGN OF DC-203
C
Table 10: Summary of outcomes for pressure drop estimation
Variable Equation Value
% Perforated area 𝐴𝐻
× 100
𝐴𝑝 9.1%
Plate thickness to hole 𝑃𝑙𝑎𝑡𝑒 𝑇ℎ𝑖𝑐𝑘𝑛𝑒𝑠𝑠
diameter ratio 𝐻𝑜𝑙𝑒 𝐷𝑖𝑎𝑚𝑒𝑡𝑒𝑟 0.91
Orifice coefficient, Co Figure 10 0.816
Dry plate pressure drop, hd 𝑢ℎ 2 𝜌𝑣
ℎ𝑑 = 51 ( ) ( )
𝐶𝑜 𝜌𝑙 48.887 mm of liquid
Residual head, hr 12500
ℎ𝑟 =
𝜌𝐿 19.294 mm of liquid
Total pressure drop ℎ𝑑 + ℎ𝑟 + ℎ𝑤 + ℎ𝑜𝑤,𝑚𝑎𝑥 143.576 mm of liquid
−3
Pressure drop per plate 9.81 × 10 ℎ𝑡 𝜌𝑙 912.49 Pa
D
Table 12: Summary of outcomes for hole pitch design calculation
Variable Equation Value
Ratio of weir length to 𝑙𝑤 0.676
column diameter 𝐷𝑐
Angle of chord, ϴc Figure 11 86˚
Angle subtended by edge of 𝛳𝑑 = 180˚ − 𝛳𝑐 94˚
plate, ϴd
Mean length, ls 𝛳𝑑 3m
𝑙𝑠 = 𝜋(𝐷𝑐 − 0.05) ( )
180
Area of unperforated edge 𝐴𝑢 = 0.05𝑙𝑠 0.15 m2
strip, Au
Width of unperforated edge From figure 9 0.05 m
strip allowance, wu
Width of calming zone From Figure 9 0.05 m
allowance, wc
Mean length of calming 𝑙𝑐 = 𝑤𝑢 + 𝑙𝑤 1.32 m
zone, lc
Area of calming zone, Aca 𝐴𝑐𝑎 = 2𝑙𝑤 𝑤𝑐 0.127 m2
E
APPENDIX C SKETCH OF TRAY LAYOUT OF DC-203
Cartridge type construction is used. Allows 50 mm unperforated strip round plate edge and
50 mm wide calming zones.
1320 mm
Figure 13: Sketches of the tray layout for distillation column BT-301