Butyl Polymers Asia - Pacific

1




S. MAJUMDAR
ExxonMobil Company India Pvt. Ltd.
Bangalore Research and Development
Technology Centre, Plot - 5, Road No - 8
Export Promotion Industrial Park
White Field, Bangalore - 560066
INDIA

AP-ATD 02 004
MIXING AND EXTRUSION
BRDTC, India
Sept. 23-26, 2002
BANGALORE BUTYL - EEB SEMINAR
Butyl Polymers Asia - Pacific
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CONTENTS:

INTRODUCTION
OPEN MILL MIXING
INTERNAL MIXING
EXTRUDER
SUMMARY
Butyl Polymers Asia - Pacific
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TWO TYPES OF MIXING
OPEN MILL MIXING
INTERNAL MIXING
Some common Termonologies:

Mastication / Premastication
Master batch
Final Batch
Batch size / Batch weight
Mixing cycles
Upside down mixing
Dump temperature
Dispersion
Butyl Polymers Asia - Pacific
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OPEN MILL MIXING / TWO ROLL MILL
Butyl Polymers Asia - Pacific
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SCHEMATIC DIAGRAM OF TWO ROLL MILL
Some common
Termonologies:

NIP GAP
FRICTION RATIO
COOLING CORED
ROLLS
SAFETY DEVICES
MILL BAGGING
Butyl Polymers Asia - Pacific
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OPEN MILL MIXING
Very briefly, the open mill mixing is to masticate the polymers until
an even and smooth band is formed around the front roller.
The fillers and oils are added alterately followed by addition of
valcanizing materials.
During whole operation cutting and blending is carried out for proper
mixing.

Two roll axes are horizontal and parallel and the distance between
the two rolls are made adjustable by screws.

Open Mill Mixing of inner tube compound is very rare now , yet it is
existing praticularly for a small and new plant.In some cases final
batches will be mixed only in two roll mill. Following are the
important parameters for Open Mill Mixing:

Adjust narrow nip gap for band formation

Butyl Polymers Asia - Pacific
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Maintain friction ratio of mill 1:1.25. Adjust temperature of mill
around 40
0
C, which can be done either by passing steam or by
rubber mastication without opening water circulation vlave. Add all
rubber.

Add ZnO and Stearic Acid and allow band formation.

Add 50% of black (higher reinforcing black should be added at the
beginning).

Remaining 50% black is added with oil and increase nip gap
gradually to avoide over- mastication and open water circulation
full. After mixing is over, sheet out from mill to cool.

Add curatives at the last stage of cycle but make sure that the batch
temperature is with in 90
0
C.

Two roll mills are usually fitted with various safety devices,some
to protect the operator, some to protect the machine.
Butyl Polymers Asia - Pacific
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Different roll size will have different capacity of batch weight of two
roll mill. Following are some standard batch weight with respect to
roll size:


Roll Size (DxL inch) Batch Wt. (kg)

12 x 26 10 - 15
14 x 36 20 - 30
16 x 42 35 - 45
18 x 48 55 - 65
22 x 60 90 - 100
24 x 84 120 - 130


Butyl Polymers Asia - Pacific
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INTERNAL MIXING
The two types widely used are
Banbury and Intermix.
Productivity is cosiderably higher
than two roll mill.
Some features that increases
productivity :
Volume
Rotor speed
Rotor Design
Ram Pressure
TCU
Butyl Polymers Asia - Pacific
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SCHEMATIC DIAGRAM OF INTERNAL MIXER
Some important features
are:
ROTOR
CHAMBER
RAM
DISCHARGE DOOR
FEED HOPPER
OIL INJECTOR
DUST SEALS

Butyl Polymers Asia - Pacific
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DIFFERENT TYPE OF ROTOR OF BANBURY
MIXER
Rotor design plays a very
important role in the
mixing and dispersion of
filler in the rubber.

Rotor design is different in:

Two wing vs Four wing

Tangent system vs
Interlocking system
Butyl Polymers Asia - Pacific
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Tangential Interlocking

Butyl Polymers Asia - Pacific
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INTERNAL MIXER

In an internal mixture, the key requirement is the proper
dispersion of filler in the rubber.

Butyl compound mixing is done in two stages. First stage
or Master Batch contains all ingredients except the
curatives and in the second stage or Final Batch, only
curatives are added.

In order to get better dispersion, the use of Banbury
volume is very important. In case of Master Batch, the
normal loadings is 10-20% higher than that used for GPR
compound. For Butyl rubber mixing, it is better to use fill
factor close to 0.90 for better dispersion of carbon black.

Banbury batch weight is calculated in the following
manner: Batch weight (kg) = Banbury volume (liter) x Fill
Factor x Compound Specific Gravity


Butyl Polymers Asia - Pacific
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As the Banbury becomes older the fill factor changes from 0.9 to 1.0
due to wear and tear of Banbury rotor and chamber,Banbury volume
also increases.

Quality of mixing will depend on the following :

Type of Rotor

Banbury volume loading

Banbury starting temperature

Black : Oil ratio in the Master Batch

Sequence of loading

Dump temperature
There could be a variety of sequences of loading. Examples are given
below (considering 5' of mixing cycle for 230 liter banbury):


Butyl Polymers Asia - Pacific
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Time (minutes) Operation

(a) 0' Polymer
0.5' - 1.0' 1/2 black, ZnO
2.5' 1/2 black, stearic Acid, Oil
3.5' Clean run
4.5 - 5' Dump at = 160
0 -
170
0
C


b) 0' Polymer
0.5' All black, ZnO, St Acid
2.5' Oil (at 130
0
C)
3.5' Clean run
4.5' - 5' Dump at = 160
0
- 170
0
C




Butyl Polymers Asia - Pacific
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Some important parameters in mixing

Due to difference in co-cure characters, butyl rubber can not be blended
with GPR, whose containmination results in improper cure, reduction in
ozone resistance, drop in tension set etc.

During mixing carbon black with butyl rubber, enough time or shearing
force is to be provided for better dispersion because butyl has
comparatively lower affinity towards carbon black then GPR.

Combination of different types of carbon black are good provided
dispersion are equally good. Different type of carbon black will have
different affinity for butyl rubber due to the difference in surface area.

Carbon black with higher surface area will provide better green strength
but difficult to get dispersed in butyl rubber. If dispersion of above black
is inadequate, this can create problems as porous extrusions and blister
in vulcanizate.

Butyl Polymers Asia - Pacific
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Some important parameters in mixing

Mineral fillers are not generally recommended in inner tube formulation as
this may cause die plating problem. Down time, scrap and rejections often
increase due to the use of mineral filler.

The key requirement for processing aids is to improve upon the
processability with minimum effect on the vulcanizates. Paraffinic oil or
slightly naphthenic oil with VGC less than 0.90 and viscosities of 40-80 sus
at 100
0
C are best.

Master Batch batch weight is very important.Normally 10 - 20 % higher
batch wt. Is used than GPR. Very high batch weight has always adverse
effect on banbury dust seals. For final batches, it is desired to fill 80% of
the total Master Batch weight.

Dump temperature of Master batch should be between 160 - 170
0
C and
that for final should not exceed 105
0
C.

Butyl Rubber is better premasticated either in banbury or in open mill
mixing.This increases the acceptance of ingredients . In case of difficulty
in premastication, butyl is recommended to keep at hot house (60-80
0
C).
Butyl Polymers Asia - Pacific
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EXTRUDER

Extruders are machines
which force rubber through
a nozzle or die to give a
profiled strip of material.

BC,PC,TB and OTR Tubes
are given shape through
different sizes of extruders.
Butyl Polymers Asia - Pacific
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SCHEMATIC DIAGRAM OF EXTRUDER
Some important
features of Extruder
are:

FEED HOPPER
BARREL
SCREW
HEAD
DIE


Butyl Polymers Asia - Pacific
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EXTRUDER

HOT FEED EXTRUDER AND COLD FEED EXTRUDER

Hot feed extruders most commonly used

-L/D usually 4-6
-Force feed roller is advantageous
-200 mm (8 inch) is adequate for most PC & TB sizes
-250 mm (10 inch) is desirable for larger sizes

Cold feed extruders normally selected for newer plants

-L/D usually 12-20
-Offer more dimensional control and minimal porosity
-Eliminate need for warm-up and feed mills
-Higher output for given screw dimention than hot feed



Butyl Polymers Asia - Pacific
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SOME OPERATING GUIDELINES FOR HOT FEED EXTRUDER

Implies that the feed rubber is in hot condition,which means that the
rubber being fed here is premilled from a two roll mill.

Compound auto-feeder is desirable

Always use blend of multiple batches at the auto-feeder for uniform
dimension of the extrudate.

Maintain rolling pencil bank on the feed mill for better dispersion and less
air trapment.

Monitor addition of rework at a constant ratio of around 10 - 15%.

Fix nip gap of feed mill for all time and maintain change in volume by
change in the width of the feed strip of extruder.

Maintain constant feed strip for fixed size of the tube.

Feed strip temperature should be between 80 - 90
0
C.

Butyl Polymers Asia - Pacific
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The speed of feed conveyor, extruder RPM, take-off conveyor and
cooling line are to be synchronized.


All the above parameters will ensure extrudate with (I) minimum porosity,
(ii) minimum variation in viscosity and scorch, (iii) better dimensional
control at a constant rate.


Butyl Polymers Asia - Pacific
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SOME OPERATING GUIDELINES FOR COLD FEED EXTRUDER

Implies that the feed rubber is in hot condition .

Keep extruder barrel filled and use force feed roller to feed extruder.

Standardize extruder RPM for each tube size.

Keep barrel and screw temperature within 50-60
0
C and die
temperature 110-120
0
C.

The design of die should be such that :

There is smooth entry of extrudate through die and the increase in
pressure gradient is maintained optimum.

There is no excess injection of talc or dusting ingredients.

The speed of feed conveyor, extruder RPM, take-off conveyor and
cooling line are to be synchronized.

Butyl Polymers Asia - Pacific
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Pulling down extrusion on take-off conveyor should be avoided. It
is desired to make different die for different sizes of tubes.

Efficient and thorough cooling is essential.

Cold feed extruder possess the following advantages over Hot Feed Ext.

(a) Less capital cost (no mills etc.)

(b) Less labour involved

(c) Better temperature control of the compound.

(d) Capability of handling both high and low Mooney compound

(e) Better dimensional control


Butyl Polymers Asia - Pacific
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SUMMARY


Butyl Mixing can be carried out both in Two roll mixer as well as in
internal mixer.
Two roll mill mixing is not popular now-a-days.It is used in small and
new plants.In some cases final batches are mixed in two roll mill.
Internal mixer is very popular for its higher productivity and uniformity
in mixing.
Different internal mixer may have different rotor design and chamber
volume.
Extruder gives the desired profile of compounded rubber before
vulcanization.All types of tubes are given shape through different
sizes of extruders.
Hot feed extruder is more in use than Cold feed extruder .
Cold feed extruder provided better dimensional control and other
advantages over hot feed extruder.
Butyl Polymers Asia - Pacific
26
BRDTC
by
Samir Majumdar
Sept. 23-26, 2002

AP-ATD 02 004
BANGALORE BUTYL - EEB SEMINAR
MIXING AND EXTRUSION
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