L. D.

COLLEGE OF ENGINEERING
AHMEDABAD – 380 015

Name:

Semester: M.E.-I Enrollment No.:

Subject: Powder and particulate Technology (3714010) Year: 2023-24

 Certificate

This is to certify that Er. Maulik Maheshbhai Chauhan

Enrollment No. _______________________________ of M.E. Semester-I

of Rubber Technology Department has satisfactorily completed

the course in the subject of Powder and particulate

Technology (3714010) within four walls of L. D. College of

Engineering, Ahmedabad -380015.

Date of Submission : ______________________________________

Staff in-Charge : ______________________________________

Head of Department : ______________________________________

II
 Certificate

This is to certify that the above term work of Er. Maulik Maheshbhai

Chauhan University Exam No. __________________________________ of M.E.

Semester-I of Rubber Technology Department is assessed for

University examination on ___________________.

Int. Examiner ______________________________________

Ext. Examiner ______________________________________

III
3714010 Index

Index
Sr. Page Date of Date of Initial
Title From To
No Start Completion of Staff

1 To study about different methods for

01 08 10-08-2023 17-08-2023
manufacturing of powdered rubber.

To study about importance of

2 09 10 17-08-2023 24-08-2023
partitioning agent in powder rubber.

To determine particle size of given

3 powdered rubber and particle size 11 12 24-08-2023 31-08-2023
distribution.

To study about dispersion of

4 13 15 31-08-2023 14-09-2023
ingredients in powder Pre-Blend.

5 To study about advantages of

16 19 14-09-2023 21-09-2023
powder and particulate rubber.

To Study About different types of

6 20 21 21-09-2023 05-10-2023
extruders for continuous processing.

To study adhesive from powder

7 rubber and bale rubber and compare 22 23 05-10-2023 12-10-2023
about it.

To Study about Compression

8 24 24 12-10-2023 19-10-2023
moulding in Powder Rubber.

9 To study about dust assessment in

25 26 19-10-2023 26-10-2023
solid rubber chemical.

To study about economic advantage

10 of powder rubber technology. 27 28 26-10-2023 02-10-2023

IV
3714010 Practical - 1

Practical: 1
Aim: To study about different methods for manufacturing of powdered rubber.

1.1 Preparation of Powdered Rubbers:

The method used depends very much as would be expected, on the polymer in question, but in general
powdered rubbers can be made either by spray or flash drying freeze or cryogenic grinding
precipitation and coagulation in line straight grinding and/or encapsulation.
Most of these processes, because of the system and the fineness and type of the polymer concerned,
produce materials which are very tacky. They would all quickly stick together and form an inseparable
mass if partitioning agents of the correct type and in the minimum but required amounts were not
used.
Materials which have been satisfactorily used in specific applications include tales, other silicates
whiting, clays. carbon blacks, starch and various compatible thermoplastic resins, dependent of course
upon whether these materials can be tolerated in the recipe or whether ash-free low ash can be
accepted within the hydrocarbon portion of the formulation.

1.2 Freeze / Cryogenic Grinding:

This system consists of freezing the particles of rubber during the finding operation with liquid
nitrogen of carbon dioxide, thus inducing brittleness of the polymer.
The frozen particles are now served in the presence of a partitioning agent to the required particle
size.

1.3 Granulating:
For the economical size reduction of natural and synthetic rubber of any kind, in form of bales, sheets
or chips, vulcanized or un-vulcanized, with or without textile reinforcement is necessary.

1
3714010 Practical - 1

1.3.1 Principle Operation

The rubber bales are fed by hand or via a conveyor belt into the Granulators series through a patented
in feed chute with shuttle flaps that guarantees a guided material feeding and a dosed material intake.
The material is the granulated to the desired size by means of the specially designed guillotine rotor.
The particle size is determined by the screen mesh size installed in the knife mill.
A pneumatic aspiration system is installed downstream from the rubber granulator in order to
discharge the heat produced during the granulating process and also to transport the granules.
The machine is easily accessible for quick and thorough cleaning as well as for knife exchange as the
upper part of the housing can be hydraulically swung open.
Low downtime is guaranteed as the rotor and the stator knives are adjustable outside of the machine
and the screen is easily exchangeable.
Material transport can be performed mechanically or pneumatically.
Standard one, two or three step size reduction systems can be offered.
1.3.2 Type of Operation
i. One Step Preparation
ii. Two Step Preparation
[Link] One Step Preparation
In cases where relatively simple types of rubber such as NBR, SBR and EPDM are to be granulated
from a standard bale size to granule particle sizes smaller than 10 mm, the granulating process can be
often performed in one step.
If the addition of a dusting agent such as talcum or zinc stearate is required, the dusting agent is
injected directly into the cutting chamber via a dosing rotary airlock as well as a high-pressure blower.
Therefore, right directly after the cut, the surfaces of the cut granules are dusted thus preventing
caking.
Overdosed dusting agent is separated from the granules by means of a recovery system and then
reused.

Figure 1.1 One step preparation

2
3714010 Practical - 1

[Link] Two Step Preparations

If standard rubber bales from relatively non-sensitive types of rubber are to be reduced to particle
sizes smaller than 4 mm, granulating systems operating on a two-step principle are used.
A granulator rotor is used for the pre-cutting of the bales.
Downstream fine granulation is also performed on a knife mill equipped with a guillotine rotor.
The rubber bales are fed by hand or by means of a conveyor belt into the Granulator and cut into
pieces smaller than 40 mm.
An additional conveyor belt transports the rubber pieces to the downstream fine granulating system
where the product is granulated to the desired particle size which is determined by the mesh size
installed in the knife mill.
A pneumatic aspiration system is installed downstream from the rubber knife mill in order to
discharge the hat produced during the granulation process and also to transport the granules.
The addition of a dusting agent such as talcum or zinc stearate is necessary for these two granulating
steps. The dusting agent is injected directly into the cutting chamber via a dosing rotary airlock as
well as a high-pressure blower. Therefore, right directly after the cut, the surfaces of the cut granules
are dusted thus preventing caking. Overdosed dusting agent is separated from the granules by means
of a recovery system and then reused.

Figure 1.2 Two step preparation

1.3.3 Advantages & Features:

Reliable, efficient Robust design
Guillotine rotor for low friction temperature gentle size reduction
Patented infeed chute with shuttle flaps allows guided material feed as well as dosed material intake.
Good accessibility of the cutting chamber allows easy and intensive cleaning and quick screen change
Knives adjustable outside of the mill allowing for minimum downtime
Compact design

3
3714010 Practical - 1

1.3.4 Applications
Natural or Synthetic Rubber
Bales
Sheets
Chips
Vulcanized or un-vulcanized
1.4 Attrition Grinding:
1.4.1 Introduction
A dry attrition mill is a versatile fine-grinding unit
that can handle several materials under many
conditions. Common applications include grinding
ceramic powders, pigments, chemicals, food
products, plastics and rubber, minerals, metal
powders, glass frits, fibers, and cellulose.
The mill can also blend dissimilar materials, coat
particles with additives or disperse the additives
during grinding, and provide mechanical alloying.
Conditions that can be varied during mill operation
include the grinding media type, size, and ratio to
material; material federate; and grinding speed. Figure 1.3 Cross-sectional view of
Attrition Grinding Mill
The attrition mill’s dry operation saves the process
step and energy required to remove waste liquid from a wet-milling chamber and eliminates having
to dispose of the liquid, which can be costly.
The compact mill also allows you to adjust operating variables to meet your product specification.
The dry attrition mill typically provides size reduction finer than that of a vibratory mill and
comparable with that of a jet mill.
A regular-speed dry attrition mill typically can handle feed materials 40 mesh and finer; a high-speed
unit can handle feed materials 75 microns and finer.
In continuous mode, the regular-speed mill can typically reduce particles to 44 microns; the high-
speed unit can reduce them to about 5 microns and, with air classification, to about 3 microns.
In batch mode, the regular-speed mill can typically reduce particles to between 1 and 2 microns; the
high-speed mill can reduce them to about 80 percent less than 1 micron.
However, the mill is typically not suited to reducing materials to superfine submicron particles, which
requires wet grinding.
The dry attrition mill also generates more internal heat than a wet mill and can require running a
refrigerated coolant through the mill’s cooling jacket. Adjusting the mill’s material-to-media ratio and
retention time also can limit heat generated during grinding.

1.4.2 Working of Attrition Mill

The dry, fine-grinding attrition mill consists of a stationary, cylindrical, vertical grinding chamber, as
shown in Figure. A rotating vertical shaft with horizontal agitators is mounted at the chamber center.

4
3714010 Practical - 1

Grinding media, available in balls made of various materials, fill about two-thirds of the regular-speed
mill’s chamber and about one-third of the high-speed unit’s chamber.
A feed inlet is located at the chamber’s top, and a metering valve assembly with either a grid or laser-
drilled screen is located at the bottom. (A high-speed unit can be fitted with a side discharge near the
chamber bottom for discharging by centrifugal force).
A secondary feeder for adding a dry grinding aid or additive or a metering pump for dispensing a liquid
additive can also be located at the chamber top. A cooling jacket encloses the chamber and typically is
filled with water.
In operation, feed material is metered through the inlet and falls into the media bed. (If required, a
grinding aid or additive is dispensed by the secondary feeder or metering pump into the chamber).
The rotating shaft’s agitators expand and move the media bed, creating a random motion in which the
media and particles (and any grinding aid or additive) can freely move, collide, and impinge on each
other.
The action generates high shear and powerful impact for efficient grinding, creating small particles
that are more spherical than those produced by other impact milling methods.
The on-spec milled particles flow by gravity through the media bed and out the metering valve, where
the grid or screen prevents the media from exiting (or the particles are propelled by centrifugal force
through the high-speed unit’s side discharge).

1.4.3 Selection of Grinding Media

Grinding media types for attrition mills include plastic pellets, through hardened carbon steel, chrome
steel, Type 440C stainless steel, zirconium silicate, zirconium oxide (MgO or Y2O3 stabilized), 3
aluminium oxide, steatite, tungsten carbide, silicon nitride, and silicon carbide. The media are
available in a range of diameters to match your application.
Base your media selection on the following factors, which are often interrelated:
Specific gravity: High-density media generally provide better grinding results. The media should
be denser than the material being ground.
Initial feed material size: Use large media if your material has large particles; small media can’t
break up the large particles.
Final particle size: Use small media to achieve finer grinding.
Hardness: Hard media will grind more efficiently and wear more slowly.
PH: A strong acid or alkaline material can react with some metallic media.
Discoloration: When your final product color is important, closely match the media color to the
material color. For instance, use white media with a white material.
Contamination: Because wear particles from the media can enter your material, choose media
whose wear particles won’t affect product quality or that can be removed by a magnetic separator,
a chemical reaction, or sintering.
Cost: Long-wearing media tend to be more expensive. But a media type that initially costs two to
three times more than another can be a long-term bargain because it can last five to six times
longer.

5
3714010 Practical - 1

1.4.4 Control of Operating Variables

Minimize your material’s moisture content: A material with high moisture content (over about 5
percent) can cake inside the grinding chamber and stop the process. Keep your material’s moisture
content as low as possible. In some cases, you can operate the mill at a higher temperature to drive off
moisture.
Minimize particle size variation in the feed material: A feed material with a broad particle size
range often produces a wide final particle size range. Such a feed material also can make your decisions
about process mode, mill type, media, and other factors more difficult.
Control the federate: Although both gravimetric and volumetric feeders are suitable for feeding the
mill, make sure the feeder is accurate. The more accurate the federate, the better your grinding results.
Maintain the right material-to-media ratio. If your material-to-media ratio is too high, it will reduce
the media’s velocity and impact and reduce the grinding efficiency. But if the ratio is too low, the media
will impact itself and wear quickly. The optimal material-to-media ratio delivers efficient grinding.
Use grinding aids and additives: You can continuously feed a chemical grinding aid or additive to
the mill during grinding. The chemical can do one or more of the following:
Minimize the effects of any inherent moisture in the feed material.
Change the inherent electrical charge on each particle’s surface or reduce negative effects of any
static charge that develops during grinding.
Act as a partitioning agent between particles to prevent agglomeration (an example is fumed silica,
whose abrasiveness separates particles).
Function as a lubricant between particles (an example is fatty acid, which oils particle surfaces).
Eliminate the additional process step of introducing an additive or ingredient downstream from
the mill.

1.5 Spray drying

1.5.1 Introduction
A process for the preparation of polymer powders
from polymer dispersions by feeding a polymer
dispersion continuously into an atomization
apparatus and separately therefrom but at the same
time also introducing a liquid agent, the dispersion
and the liquid agent being completely mixed within
at the most one second and the mixture being
immediately thereafter dried with evaporation of the
volatile constituents to form a powder composed of
particles having an average diameter of from 0.05 to
1 mm, and the polymer powders prepared by this
process. Figure 1.4 Spray drying method

1.5.2 Process for the Preparation of Polymer Powders by Spray Drying

A polymer in the form of an aqueous emulsion is supplied to a mixing nozzle with internal mixing
device.

6
3714010 Practical - 1

The liquid agent consists of a solution of an inorganic salt and/or an organic acid which is added to
the emulsion in the mixture nozzle and mixed with the emulsion.
Both liquids are introduced into the nozzle by means of pumps in which pressures of from 10 to 30
bar occur upstream of the nozzle.
After intensive mixing, the mixture leaves the nozzle, e.g. in the form of a hollow spray one which
enters the stream of hot gas or steam of a spray drying tower.
At inlet temperatures of the hot gas of from 50 to 400 C., in particular from 100 to 200 C., and outlet
temperature of from 50 to 200 C., in particular from 70 to 150° C., the polymer dries to a powder which
has particularly advantageous properties for technical application without requiring further
purification.
The polymers prepared according to the invention are improved in their thermoplastic processing
characteristics and thermostability compared with conventional powders prepared by atomization
drying.
The advantageous properties are particularly effective when the improved powders are used for the
modification of vinyl chloride polymers.
[Link] Example
A styrene/butadiene rubber latex (SBR latex) containing a copolymer of 35% by weight of styrene and
65% by weight of butadiene is used as graft stock.
The latex has a polymer content of 32.4% by weight and an average latex particle diameter (d50 value)
of 120 nm. 40 The copolymer has a gel content of 88% by weight.
The latex was prepared by radical emulsion polymerization at 60° C., using potassium
peroxydisulphate as initiator and the sodium salt of disproportionated abietic acid at pH values of
from 11 to 12. 45 and the graft polymer is prepared.

1.5.3 General description of process

The polymer emulsion is fed from a dosing pump into a mixing nozzle designed for internal mixing.
The liquid agent consists of an aqueous solution of an inorganic salt and/or an organic acid.
It is also introduced into the nozzle by a dosing pump at a fixed quantitative ratio to the polymer
emulsion.
The resulting mixture leaves the nozzle at the top of a spray drying tower in the form of a hollow spray
cone composed of droplets measuring from 10 to 500 pm in diameter.
The drying medium used is air with reduced oxygen content (less than 5%). This air is recirculated
with the addition of nitrogen and enters the spray drier at temperatures Tin of from 150 to 200 C. and
leaves the drier at temperatures of Tout of 50 to 100° C.
In the spray drying tower, the polymer is dried from its initial water content of from 50 to 80% to
residual water content of from 0.05 to 2%, and during this process agglomeration and/or a chemical
reaction may take place in the flying droplets to improve the physical properties of the polymer
powder.
Working up of polymer emulsion A by the process described above Air temperatures: Tin=170°
C.-5 C., Tour=80' C.E30' C. The quantity of air is then approximately 25 to 30 times the quantity of
water to be evaporated. Emulsion A is supplied as main mass stream to an internally mixing nozzle
(manufactured by Schlick, Model 770/1) by means of an eccentric screw pump while the bias pressure

7
3714010 Practical - 1

in the nozzle is about 15 bar. A solution of 30g of magnesium sulphate per 5g of acetic acid in 250 g of
water is supplied as smaller liquid stream per kg of solids content of emulsion A by means of a
correspondingly smaller dosing pump. On leaving the spray drier and separation from the air stream,
the dried polymer powder has residual moisture contents of from 0.2 to 0.8%.
Working up of emulsion B by the process described above Air temperatures, Tin=160 to 170° C.;
Tout-80' C.E3' C. The quantity of air is approximately equal to 25 to 30 times the quantity of water to
be evaporated. Emulsion B is supplied as main stream to an internally mixing nozzle of Schlick, Model
770/1 by means of an eccentric screw pump, the bias pressure in the nozzle being approximately 10
to 12 bar. 100 g of a 4% by weight solution of magnesium Sulphate (MgSo4) in water per 1 kg of solids
content of emulsion B are sup plied to the mixing nozzle from a dosing pump. On leaving the spray
drier and separation from the steam of moisture, the dried polymer powder has a residual moisture
content of about 0.5%.
Working up of emulsion B: By a method analogous to that of process (II2) using 100g of a 3% by
weight solution of calcium format per 1 kg of solids content in emulsion B. On leaving the spray drier
and separation from the air stream, the dried powder has a residual moisture content of 0.5% by
weight.
Process for working up emulsion B: The process is analogous to that of II.3, using an aqueous
solution of aluminum sulphate. The residual moisture contents of the powder were in the range of
from 0.3 to 0.5% by weight.

1.6 Conclusion
Powdered rubber production methods like freeze grinding and granulating offer efficient size
reduction, while attrition milling provides versatility for various materials and applications.
Choosing the right method depends on factors like polymer type, desired particle size, and budget.

8
3714010 Practical - 2
Practical: 2
Aim: To study about importance of partitioning agent in powder rubber.

2.1 Introduction
Many materials are used to separate or partition the small particles of powdered rubber in order to
prevent agglomeration.
This is necessary irrespective of the method of manufacturing of the powder, or indeed of the type of
rubber.
The amount of partitioner can of course vary and is dependent upon the ultimate properties required.
Typical materials commonly used include magnesium and calcium silicates, silica, calcium carbonate
and starch.
The efficiencies of partitioning agents vary considerably, but all have been found to be usable under
specific conditions. Silica types are however the best.

Table 2.1 Effect of Type and Quality of Partitioner Versus Time

Magnesium Calcium Calcium

Silica Starch
Silicate Silicate Carbonate

Percent Time (mo) Time (mo) Time (mo) Time (mo) Time (mo)
Polymer
Partitioner 1 3 6 1 3 6 1 3 6 1 3 6 1 3 6

2½ 2 2 3 1 2 3 1 2 3 3 — — 3 — —
5 1 1 2 1 1 2 1 2 2 3 — — 3 — —
NBR
7½ 1 1 2 1 1 2 1 1 2 3 — — 2 3 —
10 1 1 1 1 1 1 1 1 1 2 3 — 2 3 —

2½ 1 2 2 1 2 2 1 1 2 3 — — 3 — —

5 1 1 1 1 1 1 1 1 1 3 — — 3 — —
CR
7½ 1 1 1 1 1 1 1 1 1 3 — — 3 — —

10 1 1 1 1 1 1 1 1 1 3 — — 2 3 —

2½ 2 3 3 2 3 3 2 3 3 3 — — 3 — —
5 1 2 2 1 2 2 1 2 2 3 — — 3 — —
NR
7½ 1 2 2 1 2 2 2 2 2 3 — — 3 — —
10 1 1 2 1 1 2 1 1 2 3 — — 3 — —

2½ 1 2 3 1 2 3 1 2 3 3 — — 3 — —
5 1 1 2 1 2 3 1 1 3 3 — — 3 — —
SBR
7½ 1 2 3 1 1 2 1 1 2 3 — — 3 — —
10 1 1 1 1 1 1 1 1 1 3 — — 3 — —

1: Free Flowing, 2: Slight compacted, but easily broken down with light figure pressure, 3: compacted, but
not easily broken down.

9
3714010 Practical - 2

It is obviously essential to prevent sticking especially when transportation and storage conditions are
so variable and when climatic changes are superimposed on top of these.
The ideal amount of partitioning agent is also critical in that the effectiveness is so different according
to the agent and the physical properties required of the ultimate vulcanizate.
Correct choice of agent is therefore necessary and the advice of the polymer producer or processor
should also be sought in order to obtain optimum properties in the particular recipe.
Assuming that everything is correct, it should be possible to obtain cured properties at least equal to
or better than the same compound recipe made from baled polymer, on an exact weight for weight
replacement basis of baled polymer by powdered rubber including partitioner.
The effects of transportation and storage by post pallets on the free-flowing properties of powdered
rubber, using partitioning agents as listed in table has been examined in 25kg bags.
The bags were stacked four deep and the material was examined in the bag at the base of each stack
of post pallets. Transportation included examination of lorry container loads. The effects of this
treatment are shown in table.

Table 2.2 Effect of Magnesium Silicate at 2½, 5, 7½, and 10% Levels with NBR Powder

Tensile strength (kg/cm2) Elongation at break (%)

NBR
Control 2½% 5% 7½% 10% Control 2½% 5% 7½% 10%

1 92 130 135 133 101 150 200 215 185 155

2 124 131 132 125 103 160 200 205 190 155
3 106 126 123 125 107 170 215 195 170 165
4 112 122 128 119 114 159 195 190 185 150

Average 109 127 130 126 106 160 203 201 183 156

Std.
13 4 5 6 6 8 9 11 9 6
dev.

The results obtained at various levels of partitioning agent show that silicate materials are
immediately suitable, and the effect of quantities between 2.5 percent and 10 percent shows that the
best results are obtained at around 5 percent concentration, before a drop in physical properties is
noticeable.
A fascinating point that has been confirmed by numerous researchers in the field of powdered rubber
is that the use of powdered materials produces a definite pattern of greater consistency when
compared to the bale rubber control materials, and that powdered rubber recipes have higher tensile
and elongation properties in general.

2.2 Conclusion
Partitioning agents are crucial for powdered rubber, preventing caking and maintaining flow. Silica
types perform best, with 5% ideal for NBR, delivering improved tensile and elongation properties
compared to baled rubber. Choosing the right agent and amount ensures optimal storage and even
enhances cured properties.

10
3714010 Practical - 3
Practical: 3
Aim: To determine particle size of given powdered rubber and particle size distribution.

3.1 Types of screen analysis:

1. Differential analysis
2. Cumulative analysis

3.1.1 Differential analysis:

The screen analysis in which the weight fraction material retained on each screen is reported in a
tubular or graphical form as a function of the mesh size/screen opening is called differential analysis.
After shaking amount of material retained on each screen is expressed as the weight fraction of total
sample.
Screen analysis of a sample is reported either in a tubular form or as graphs. ∙
Result of a screen analysis can be reported in a tubular form to show the weight fraction of mesh size.
Two numbers are needed to specify the size.
1. One for the screen through which the function passes
2. Other for the screen on which that fractions are retained
10/15 where 10 is mesh number through which material passes and 15 is mesh number on which
material retained.
The average particle size of the particular screen is calculated as the arithmetic mean of two screen
opening used to obtain the fraction.

3.1.2 Cumulative analysis:

The screen analysis in which the cumulative weight fraction of the material retained (cumulative
oversize) or passing through (cumulative undersize) each screen is reported in a tubular or graphical
form as a function the screen opening is called cumulative analysis.
It is simply obtained from the differential analysis by adding cumulatively the individual weight
fractions of material retained on each screen under consideration.
𝑁𝑇

∅ = ∆∅1 + ∆∅2 + ⋯ + ∆∅𝑁𝑇 = ∑ ∆∅𝑁

𝑁=1

where, Δ ɸ1, Δ ɸ2,… are the weight fractions of material retained on screens 1, 2,……
For the entire sample, the value of ɸ is unity.

3.2 Procedure
A screen analysis of a material is carried out by using testing sieves.
A set of standard screens is arranged serially in a stack in such a way that the coarsest and finest of
the screens is at the top and bottom respectively.

11
3714010 Practical - 3
Place the sample on the top screen and shaking in a definite manner, either manually or mechanically,
for a definite period of time.
The material retained on each screen is to be removed and weighed. ∙ The amount of material retained
on each screen is expressed as the weight fraction of the total sample.

3.3 Conclusion
Particle size of powdered rubber is determined by sieve analysis, measured as differential (fractions
retained per screen) or cumulative (total retained/passed) weight, using standardized shaking and
calculation methods.

12
3714010 Practical - 4
Practical: 4
Aim: To study about dispersion of ingredients in powder Pre-Blend.

4.1 Introduction
In any rubber compound it is essential that good dispersion of all of the Compounding ingredients is
achieved, in order to optimize the properties of the particular recipe.
The method is normally used for deciding the correct degree of dispersion in a compounded recipe
includes measuring tensile strength and elongation at break at various stages of cure, and then
plotting the tensile product and examining the Plateau in the curves so produced.
Additionally, modules and perhaps tears trend, hardness and compression set maybe used as added
criteria.
The test gives a Reasonably accurate measure, but unfortunately take rather long period of time to
carry out, and search are therefore not ideally suited as routine factory quality and process control
checks in the high-speed context or off powder blending and mixing techniques.
Other methods are those developed by Cabot Carbon Limited and Dunlop using visual and transmitted
line standards to compare the torn surfaces.
Indeed, these are very good and quite accurate, although once again requiring time and a fair degree
of skill of assessment during the fixing of the rating.
Electrical and other microscopic techniques have also been developed but for obvious reason very few
routine controlled laboratories have all these facilities.
It is therefore evident that a rapid and accurate system is required to ensure adequate mixing and its
measurement on a production busy is not such a method developed from the old T 50 test, which was
a means of measuring the state of cure, by low-temperature techniques, is worth of consideration.
The T 50 value is the temperature at which 50% recovery of the specimen has taken place after a cure
dumb Belle sample has been stretched by 100 %, frozen in a bath of acetone alcohol and carbon
dioxide mixture and a load to regain temperature.
This is very rapid and accurate means of deter mining the state of pure, and while generally used for
natural rubber composition it is also applicable to many other polymers, including SBR, NBR&CR,
because of the relation between T/50 value and the glass transition point of the polymer. This value
is quite clear, distinct and reproducible for each compound.
It is assumed that in using this technique, and contrary to some theories days has been shown to be
so in practice, if the smallest ingredients in the compound weight wise, namely the curative, activators
and accelerators, are correctly and eventually disposed, then the state of cure at the appropriate time
and temperature must be and indeed is, correct.
If there for the small items are well dispersed, it is more than a reasonable and fair Assumption that
the large quantity feelers including the blacks and inorganic materials are likewise disposed for any
particular compound, there is a finite T/50 value, and this correlates well with the Cabot rating.
Thus T/50 test can be used as a very rapid and Handy practical factory control for dispersion.
Table shows the three control compounds. Figure shows reproducibility possible, under controlled
conditions. The rating chart devised by Cabot carbon Limited is shown in figure 3.1.

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3714010 Practical - 4
Table 4.1 T/50 – CABOT Comparisons

Nitrile Polychloroprene Natural rubber/SBR

Results
Sample No. T/50 value Cabot T/50 value Cabot T/50 value Cabot
(°C) rating (°C) rating (°C) rating

1 —15.0 4.5 —22.5 4.3 —33.0 4.8

2 —15.0 4.5 —22.5 4.5 —33.0 4.5

3 —15.0 4.5 —22.5 4.5 —33.0 4.5

4 —15.0 4.5 —22.4 4.5 —33.0 4.3

5 —15.0 4.5 —22.5 4.5 —32.9 4.5

6 —14.9 4.5 —22.5 4.8 —33.9 4.5

7 —15.0 4.5 —22.5 4.5 —33.0 4.5

8 —14.9 4.5 —22.5 4.3 —33.0 4.5

9 —14.9 4.5 —22.5 4.5 —33.0 4.5

10 —15.0 4.3 —22.4 4.3 —32.9 4.3

11 —15.1 4.3 —22.4 4.8 —33.1 4.5

12 —15.1 4.8 —22.6 4.8 —33.1 4.5

13 —15.1 4.5 —22.5 4.5 —33.1 4.5

14 —15.1 4.5 —22.6 4.3 —33.1 4.5

15 —14.9 4.5 —22.6 4.3 —33.0 4.5

16 —15.0 4.5 —22.5 4.8 —33.1 4.8

17 —14.9 4.5 —22.5 4.5 —32.9 4.5

18 —14.9 4.5 —22.4 4.5 —32.9 4.5

19 —15.1 4.5 —22.5 4.5 —33.0 4.5

20 —15.0 4.5 —22.6 4.5 —33.0 4.5

Average —14.995 4.5 —22.5 4.5 —33.0 4.5

Standard
0.0745 — 0.063 — 0.07 —
deviation

14
3714010 Practical - 4
5 10
Cabot

4 0

T/50 Value (°C)

Cabot Rating

3 -10
T/50

2 -20

1 -30

0 5 10 15 20

Figure 4.1 NBR - Number of samples

4.2 Conclusion
T/50 test offers a rapid and
accurate method for assessing
ingredient dispersion in
powder blends, correlating
well with established visual
rating systems. This makes it a
practical and efficient tool for
production control.

15
3714010 Practical - 5
Practical: 5
Aim: To study about advantages of powder and particulate rubber.

5.1 Advantages are as follows:

The elimination of the bale cutting operation.
Much shorter mixing cycles than when using either conventional internal mixer or open milling
techniques. In the case of some of the high Mooney value nitrile compounds; it is now possible to use
the internal mixers, whereas previously only open mills could be used.
Less power consumption.
Less plant maintenance.
Less capital-intensive -plant possible.
Better ultimate dispersion.
Possibility of more rapidly accelerated compounds being mixed.
Considerably less heat memory retained when using some of the more-difficult polymers such as
polychloroprene, and hence less scorch tendency.
Possibility of direct feed to the extruders and molding presses, thus eliminating the internal mixer
and/or open milling operations.
No need for pre-mastication and master batching.
Easier control in the factory.
Considerably lower dump temperatures after mixing.
Better environmental conditions
Dealing with each of these advantages in more detail, the following important points are highlighted:
5.1.1 Bale Cutting Eliminated
Bale cutting of the various polymers is part of the everyday processing in all rubber factories, and is
both fairly highly capital intensive and labour and time consuming.
For obvious reasons, if the powder route is being used, as the polymer is already in a directly and
easily usable form, the bale cutting operation can be eliminated.
5.1.2 Shorter Mixing Cycles
A normal GRG type of internally mixed compound, by direct process, takes approximately 10 min to
mix, depending upon formulation and polymer.
Some mixers can take up to 12 min and even longer if two-stage or master batch processes have to be
used.
As a general statement, by the use of powdered polymers, not only can master batching be eliminated
but the mixing cycle can be drastically reduced.
Satisfactory mixes using pre-blends can be dropped from the mixer in a mixing time of 2 min and in a
time as low as 3 min by the use of non-preblended material with satisfactory physical and processing
properties.
It can thus be seen that internal mixer outputs can be increased at least threefold by the direct mixing
of powdered polymer weight for weight with baled polymer, or outputs of at least fourfold with the

16
3714010 Practical - 5
pre-blends of the whole mix via the intensive mixer initially physical properties are also at least equal
to, or an improvement on, the controls. The improvement of physicals is in both T/S and E/B both at
the same time. This is a common occurrence with powdered rubber compounds.

5.1.3 Power Consumption

Without doubt there is less power used in the internal mixer, when powders rather than bales are
used.
For example, the fact that more batches in unit time can be mixed, as is shown in the 'shorter mixing
cycles section above, is one proof.
Table 5.1 T/50 – CABOT Comparisons
Polymer Internal mixer
2-stage mix Preblend non-preblend Straight mix
(control) 2 min 3 min 10 min
T/Sα E/B T/S E/B T/S E/B T/S E/B
NBR 109 160 118 180 116 175 — —
CR — — 113 240 114 240 112 235
NR/SBR — — 95 590 98 585 87 560
αT/S = kg/cm2

Furthermore, the fact of lower dump temperatures proves that less energy has been used, and this is
also confirmed by the internal mixer electrical load charts.

5.1.4 Less Plant Maintenance

As has been mentioned, it is a fact that more batches may be mixed in unit time: as a simple example,
it 1s possible to eliminate at least one shift from the three normally operated, and still achieve the
same volume of output.
Thus, there is an immediate maintenance saving of 33%, plus many other fringe benefits.

Table 5.2 Power Consumption Comparisons

Polymer Control Powder mix (same recipe)
Average dump average dump
max. amps max. amps
temp. (°C) temp. (°C)
NBR 140 220 115 145
CR 145 170 115 135
NR/SBR 150 165 110 125
The whole mill room operations should be closely examined to see where savings of time, etc. can be
achieved with the obvious ultimate savings of plant maintenance.

17
3714010 Practical - 5
5.1.5 Less Capital-Intensive Plant Possible
This is a very obvious fact that as more output is achieved in unit time, less heavy mixing plant is
required than hitherto, on a weight for weight basis, with obvious processing cost improvements.
Furthermore, if the direct pre-blend powder route is in operation, then here will be an obvious
reduction in the normally used, very heavy processing equipment in the mill room.
Table 5.3 Temperature Comparisons
Polymer Dump Temperature (°C)
Control (bale) powder
NBR 140 115
CR 145 115
NR/SBR 150 110

5.1.6 Better Ultimate Dispersion

The rheograph traces confirm this. Because of this, physical tests taken from factory mixed material
correlate much more closely with those obtained from laboratory mixed batches: it is customary, with
bale mixed material, to apply a factor of approximately 10% to allow for fall-off in properties due to
the dispersion being lower from the factory compound.

5.1.7 Greater Acceleration of The Curing System Possible

This is an established practical fact, in that normally heavy loaded compound plus high acceleration
which normally must be mixed on open mills because of the high temperatures reached can now be
mixed in the internal mixer. This particularly applies to NBR loaded compounds, and also to some CR
qualities.

5.1.8 Less Heat Memory-CR Rubbers

Polychloroprene is a polymer which has a heat memory; that is, at all stages of processing, the heat so
developed is additive and accumulative within the polymer.
Thus, unfortunately, particular in high loaded type compounds, the basic and already difficult scorch
properties are aggravated.
Because of the fact that powdered rubber compounds, both mix and process cooler (as has been
discussed), the accumulative build-up of heat in the compound is considerably reduced and hence
scorch tendencies are almost eliminated and subsequent processing properties improved. Direct Feed
to Extruders/Moulding Presses Work has shown that this is now an established processing fact.

5.1.9 Possibility Of Elimination O/ Pre-mastication And Master-batching

Indications are that certainly several master-batching operations can eliminate, depending upon
polymer and end product.
Additionally, the results of the work shown under 'shorter mixing cycles' are very applicable.
Obviously, each set of local conditions will require examination, but the result of the exercise will be
very worthwhile.
18
3714010 Practical - 5
5.1.10 Easier Control in The Factory
Because of the comparative simplicity of the powder route process, easier factory control is an
immediate and obvious fringe benefit, and the development of the dispersion measurement test from
the ASTM T/50 method as a process control test has already proved itself in bulk factory manufacture.
5.1.11 Lower Dump Temperature from Internal Mixer Route
This very advantageous property of the powder route via internal mixers is linked very closely with
the fact that less power consumption is needed because of the physical form of the polymer as
presented to the mixing machines. Table 9, using exactly the same compound but either in bale or
powder form, confirms this point. Because of lower dump temperature, there are also less fumes on
discharge.
5.1.12 Better Environmental Conditions
The mixing and mill room areas of many rubber factories are dusty, and this is obviously not desirable.
Indeed, as a result of the Health and Safety at Work Act 1976, maximum atmospheric threshold limit
values are laid down for the various materials used in rubber formulations.
The use of powdered rubber pre-blends enables all the materials to be bulk handled in a closed system
thus making it possible for extremely clean and dust-free working conditions. Furthermore, because
powdered rubber processes much cooler than the bale counterpart of the same recipe, there are less
fumes during the various processing Operations.
The possibility of explosive conditions being encountered has also been examined. A preliminary
investigation has been carried out by the Insurance Technical Bureau. "It is stated that the rubber
powder may not, in itself, be a dust explosion hazard, but some of the ingredients, such as finely
divided sulphur, are potential hazards if mishandled. The guiding principle must be that at no time
may a hazardous immaterial be dispersed as an explosive dust or cloud in the mixer. This can be
avoided by ensuring that inert components are disposed first, thus inserting the atmosphere inside
the mixer.

5.2 Conclusion
Powdered rubber offers significant advantages over baled rubber, including faster processing, lower
energy consumption, better dispersion, reduced heat buildup, and improved environmental
conditions. This makes it a more efficient and sustainable choice for rubber manufacturing.

19
3714010 Practical - 6
Practical: 6
Aim: To Study About different types of extruders for continuous processing.

6.1 Farrel-Bridge (MVX) Extruder:

This composite machine is designed to compact, mix, vent and extrude hence its designation MVX.
Synchronisation of each of the four stages is
automatically controlled by the machine
design the rate of output being controlled
by the extruder speed within the available
power of the motor driving the rotors and
the temperature of the mixed material.
The machine is also designed to allow the
efficient transfer of heat between the mixed
material and the heat transfer surfaces,
thus achieving very accurate heat and Figure 6.1 Farrel-Bridge (MVX) Extruder
hence energy control.

6.2 Stewart-Bolling Mixtrumat:

This machine is designed to operate continuously by feeding two or more ingredients or a pre-blend
into it.
Then feed screw conveys the material to the mixing chamber, where the material is massed and fluxed,
transferred to the transverse screw and extruded. Vacuum vent and forward end die variations are
available options.

6.3 Shaw Extruder:

These machines incorporate the two important features necessary to ensure high quality output i.e. a
constant feed to the screw and also screw of sufficient and adequate length to supply sufficient work
to the rubber, without creating excessive temperature rise.
This is a minimum of 14:1 length: diameter ratio. The feed is controlled by a feed roller, thus either
allowing feed by cold strips or by hopper feeding of cold chunks.
A special chunking or dicing machine has been specially designed for this purpose.

6.4 Plastic screw Extruder:

The basic feature of this type of extruder is its screw design. Material is fed via the throat of the
extruder and along the scroll.
The first function of the scroll is similar to any other conventional extruder. It then changes to a helical
form of lead length double that of the screw flights about it.
The portion nearest to the barrel forms with it a narrow aperture, through which the stock has to pass.
Additionally, a vacuum system may be incorporated along the barrel thus virtually ensuring non
porous extrusions.

20
3714010 Practical - 6

Figure 6.2 Plastic screw Extruder

6.5 Pirelli Extruder:

The principle of this machine is shown in figure, the volume of the screw channel reduces
progressively through the section, and an equivalent volume of stock equal to this reduction is
continuously spilled back over the screw flights towards the feed.
This ensures back blending and also vigorous circulation within the screw channel.

6.6 Transfer Mix Extruder:

This machine can be used for dual purpose, either for continuous mixing or for extrusion.
When used as a cold feed extruder the design of the screw barrel allows the stock to pass backwards
and forwards prior to final extrusion and this ensures adequate warming up with water cooling which
is quite efficient.

6.7 Conclusion
Continuous processing offers multiple extruder designs: MVX for compacting, mixing, venting, and
extruding; Mixtrumat for continuous feeding and mixing; Shaw for constant feed and sufficient work;
plastic screw for non-porous extrudes; Pirelli for back blending and circulation; transfer mix for
continuous mixing or extrusion.

21
3714010 Practical - 7
Practical: 7
Aim: To study adhesive from powder rubber and bale rubber and compare about it.

7.1 Introduction
In the branch of the rubber industry where adhesives and doughs for the proofing and spreading
industries are manufactured, once again many and varied systems are used, dependent upon
evolution and local conditions. It is therefore only possible to generalize, but it is already very
apparent that powdered and particulate technology will have a large part to play in the future of this
section of the rubber industry.
For that matter, the polymer manufacturers have been the industry with particulate sized polymers,
such as NBR and CR, in special viscosity ranges for many years. This achieves much faster dissolving
in solvent than with the conventional necessity of masticating and soaking in solvent.
In compounded from, adhesives and dough are manufactured by thoroughly masticating the prior to
final mixing and then sheeting the compounded mix to approximately 1 mm thick. This is then placed
in a rectangular metal box, complete with lid, and covered in the appropriate solvent for that polymer.
Layers of polymer and solvent are then alternated, until the bin is filled and the lid is then placed in
position. This operation is known as laying-down. The solvent is allowed to swell the compound for
up to 96 h, in some cases, after which the swollen mass is cut with a spade and transferred to a mixer
for final mixing. The machine used may be Z- blade in principle, ball-mill type or vertical paddles. At
this stage more solvent is usually added to bring the final viscosity and the total dissolved solids to the
desired levels of consistency.
Work with powdered rubber pre-blend has been shown that is possible to eliminate the laying-down
here the procedure, thus enabling the pre-blend to be placed at once in the mixer, with the solvent,
and complete a satisfactory solution within hours rather than days.
By using a system, a system where the black is in intimate contact with the polymer (produced in the
wet state during final polymer processing) exceptionally smooth, rapid and uniform doughs can be
produced, e.g. Polyblac NBR (BP chemicals Ltd, London) andIncarb. Synthetic rubbers (International
synthetic rubber [Link], Hythe, Southampton)
Typical commercial solvents used for adhesives and doughs are as follows (it is essential that, when
handling the solvents, care is taken with regards to fire hazards, particularly static electricity, and also
that the laid-down threshold limits for atmosphere control are complied with):
NBR Toluol or chlorinated solvents.
CR toluol or chlorinated solvents.
SBR petroleum napatha.
NR petroleum napatha.
EPDM petroleum napatha.
The effect of toluol on typical NBR hose industry adhesive as shown in fig bellow and this can also be
great practical importance and value within the adhesive and proofing industries.

22
3714010 Practical - 7

7.2 Conclusion
Powdered rubber simplifies adhesive and dough production, eliminating laying-down and facilitating
rapid dissolving in solvents, leading to quicker and more efficient manufacturing.

23
3714010 Practical - 8
Practical: 8
Aim: To Study about Compression moulding in Powder Rubber.

8.1 Introduction
Conventional compression moulding techniques require the preparation of blanks in the pre-
moulding operations, and these are of course made from conventionally mixed compounds, and then
clicked out from sheet or from sheet or from screw and/or rem extruded sections.
If powdered technology principles are applied to these operations, it is immediately apparent that
here is a possible area for its use.
Early attempts to compression mould compounds direct from the preblender were unsuccessful, until
compacting by palletisation had taken place.

Figure 8.1 Compression moulding in Powder Rubber

The problems were caused by entrapped air and spillage of the power due to movement when closing
the press.
However, when pellets where fed to the compression mould, satisfactory mouldings were produced
from some materials, having low Mooney plasticity characteristics. This particular operation has
parallels in the thermosetting branch of the plastics moulding industry.
By continuing the exercise along the same technical course as for direct extrusion, i.e. continuous
compaction, it should also be possible to feed the continuous strips via a screw linked to either an
injection or transfer moulding press.
Furthermore, by the design of suitable machinery it will also be possible in due course to direct
injection mould from powder pre-blend.
The technology of injection and transfer moulding from a compounding angle has parallels in
extrusion technology and the result are shown in table which illustrate this point.

8.2 Conclusion
Compression molding with powder rubber holds promise for eliminating pre-molding and directly
feeding pellets or continuous strips, potentially streamlining production for low-plasticity materials.

24
3714010 Practical - 9
Practical: 9
Aim: To study about dust assessment in solid rubber chemical.

9.1 Introduction
The following describes an extremely simple devices, developed in the laboratories of ICI Dyestuffs
Division, which can compare realistically, reproducibly, And conventionally the relative dustiness of
different chemicals.
Concept and requirement:
Dustiness is never a desirable feature in a product for use in the rubber industry.
It may result in a minor, half-accepted nuisance which impairs efficiency and irritates the work
force.
In the worst case it may be an explosion hazard, or it may render working condition intolerable
by contamination of materials or by physiological effect.
A full realization of these implications by rubber chemicals manufacturers has led in recent years
to the appearance of many specialized physical forms of rubber chemicals designed to minimize
dustiness.
These have taken the form their of granular materials (frequently referred to as pellets, rods,
grains or seeds), or modified powders in which the dustiness has been reduced by treating the
powder with a trace of mineral oil or similar liquid.
Because the treated rubber chemical must still meet stringent specifications for purity,
dispensability in rubber and free-flowing characteristics for weighing and handling.
It is rarely possible to achieve a physical form which is satisfactory in all technological aspects
yet completely free from dust.
Objective assessments of relative dustiness are difficult to make in the laboratory in a way which
will have any meaning in the context of large-scale handling of the product in the weighting and
mixing shops.
It is therefore highly desirable to have a simple, objective, laboratory test which is cheap, quick,
reproducible, capable of providing a permanent or semi-permanent record of the results, and
above all realistic in terms of large-scale operation.
A number of devices available which work on the basic principle of shaking the test material in a
current of air or gas, passing the air the filter. This method is frequently very misleading because,
although it measures a proportion of material which may be regarded as dust, it gives no
indication of the ability of the dust to travel and remain in the air. Thus, these tests will not
differentiate between a material containing 10% of a course, quick, particle fineness; yet former
may be acceptable in a mixing shop, where as the latter might be quite intolerable.
The following describes an extremely simple devices, developed in the laboratories of ICI
Dyestuffs Division, which can compare realistically, reproducibly, And conventionally the relative
dustiness of different chemicals.
9.2 Principle
The basic principle used is that of following a small simple of product to fall into the middle of an
enclosed space and recording how the material is eventually deposited on the floor of the enclosed
space. A completely non-dusty materials will form a neat, compact heap centered on the point of
impact.
25
3714010 Practical - 9
9.3 Device
It consists of long, vertical glass tube leading into a box, the floor of which is covered with black paper.
A shallow central vessel is placed beneath the glass tube.
This vessel retains the non-dusty material, which is removed before you outside of the vessel is
assessed.

9.4 Process Description

To carry out a test, 5 g sample of the material to be tested is dropped down the tube, the rate of Edison
been without influence on the result.
When the dust has settled the box is opened and the central vessel and black pepper carefully removed
Separated black pepper now shows a ‘halo’ pattern caused by the dusty fragments in the test material.
The most valid and convincing results are seen by comparing, for two or more materials, the actual
patterns formed in this way

9.5 Conclusion
It is a simple, objective, laboratory test which is cheap, quick, reproducible, capable of providing a
permanent or semi-permanent record of the dust.

26
3714010 Practical - 10
Practical: 10
Aim: To study about economic advantage of powder rubber technology.

10.1 Introduction
Many mixings and processing advantage shown by powdered rubber recipes are now proven facts in
many plants worldwide, and the technology as such is considered to be correct, but obviously
economics cannot be overlooked.
It is essential that all aspect of the operating process in use should be closely examined, in the light of
which existing stages can be eliminated or speeded up.
To establish this, flow charts should be drawn of the current methods in use, and these compared with
the system which would be used with the powder route.
Usually, the ultimate crunch is the additional costs which have to be absorbed by the premium charged
for the powder.
On balance, however it is considered that bearing in mind the technical advantages, the scales are
tipped in favour of powder, and a completely open mind should be kept before making the final
decisions. The future for powdered rubber technology should be bright.
In an attempt to quantify the potential savings of powdered rubber technology.
It is necessary to generalize rather than be specific, because as previously mentioned there is a
diversity of existing processes, and also of powder premiums, brought about by the powder
preparation route, dependent upon the polymer.
There is also a considerable variance of powder premium charges even with the same polymer,
between suppliers, so all of this has to be carefully considered.
There are, however, several common factors peculiar to any on factory, and these are:
1. Labour cost
2. Fixed costs, related to capital, rent
3. Variable costs, including utilities
4. Material costs
Material costs are common because the same recipe, on a weight for weight basis, is used for either
the bale or the route, and the difference in cost therefore becomes a straight addition of the powdering
premium on to the hydrocarbon content of the recipe.
Thus, taking labour cost, fixed costs, variable costs as the basic costs, it is possible to derive an
equation:

Conversion cost/kg = Labour cost/kg + Fixed cost/kg + Variable cost/kg

If production mixing rates are included, the equation becomes,

Conversion cost/kg = (Labour cost/h+ Fixed cost/h) / Mixing route (kg/h) + Variable cost/kg

In typical rubber processes, two factors are known (a) the manning levels and (b) the capital cost of
the equipment being used.
At this point, the flow charts previously mentioned should be examined, relative to the plant and
equipment being used in the various operations up to the vulcanisation stage.
27
3714010 Practical - 10
From this, the manning levels for each stage may be summed, and also the replacement value at
present day costs of some of the heavy mixing and processing equipment, which could well be almost
written off but some day will need replacing or at best will require very expensive overhauls.
Therefore, taking the last equation, and introducing manning levels and capital costs, the derived
equation becomes

Conversion cost/kg = (Manpower + Fixed costs) / Mixing route (kg/h) + Variable cost/ kg

In order to quantify the manpower and fixed costs, together with the variable costs, it is necessary to
consider the various items relevant to the local factory location. These obviously will vary from factory
to factory, company to company and area to area. The main factors are
Wage rate(w)
Over heads(x)
Depreciation(y)
Maintenance(z)
Variable costs(V)
Energy(e)
These factors should now be converted to unit time i.e. per hour and the values substituted in the
equation

Conversion cost/kg = (M+F+V)/R

Where M is the= manpower (w x number of men), F the fixed costs (x +y +z), V the variable cost and R
the mixing rate (kg/h).
If this exercise is carried out for each particular process, and the savings set against the power
premium of the polymer, it is then very quickly apparent which route should be taken.

10.2 Conclusion
Powdered rubber technology can outweigh its cost through reduced labor, fixed costs, and faster
mixing rates, offering potential economic benefits despite polymer premiums.

28