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1. OBJECTIVE:
To study the preparation of masterbatch using lab scale Internal Mixer.
To study the effect mixing time, mixing speed and mixing temperature on
masterbatch formation in a laboratory scale Internal Mixer.
To observe the difference in the weight of the material after mixing.
2. ABSTRACT:
The main objective of this experiment is to observe the effect of temperature, RPM
and mixing time on the formation of masterbatch and also observe the mixing
phenomenon. To achieve this, 40 g of HDPE and 2.5 g of yellow pigment is added
into the internal mixer for the formation of the masterbatch. Three products were
prepared through internal mixer by changing the time and RPM of the internal mixer.
High mixing time causes degradation of the material because of the temperature of the
mixer. RPM is important for uniform mixing; high RPM can also affect the material.
So, in internal mixer RPM, mixing time and temperature should be set according to
the type of the material. In this experiment, mixing temperature carries the most
importance; it should neither be such high that our polymer starts degrading nor such
low that polymer won’t even melt.
3. INTRODUCTION:
Internal mixers are the machines which mix a wide range of rubber compounds and
plastic materials without changing the geometry of the machine needed. In lab scale
mostly Banbury mixer is used. Banbury Mixer also called rubber banbury mixer is
primarily used for mixing rubber and grinding plastics. The mixer is a machine with a
pair of rotors with a particular form and relative rotation, which plasticizes and mixes
the polymer materials in a closed state with adjustable temperature and pressure.
Banbury Mixer is suitable for: rubber products: all kinds of rubber ring, rubber hose,
adhesive tape, rubber belt, shockproof rubber, rubber roller, rubber sponge, tires,
rubber sole, oil seal, etc. Miscellaneous pieces of silicone rubber, footwear, sports
ball, etc [1].
PROCESS OF MIXING:
The method of combining polymeric materials in internal mixers with various
additives, such as nano-clay, calcium carbonate and other additives is regarded as one
of the most important steps in deciding the properties of the final product. A mixing
process typically involves two mechanisms of mixing which are given below:
Dispersive Mixing
Distributive Mixing
In general, mixing starts with a' distributive' step, followed by a' dispersive' one and
finally by the distribution of particles in the flow. The feasibility of using shear stress
and elongation stress to break up agglomerates has been studied extensively in
Dispersive Mixing. On the other hand, in Distributive Mixing, mixing machinery
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interrupts the minor phase of distributive mixing, and distributes it in the main phase.
Many related research have, however, centered on the intermeshing mixer distribution
[2].
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Fig: 3 (Two Wing Rotor of Banbury Mixer) [4]
IMPORTANCE:
Laboratory internal mixers measure and record torque and material temperature as
functions of time, which allows the study of the evolution of the mixing process.
When the polymer resin is completely molten during the last processing step, the
torque is directly proportional to the melting viscosity. The name of torque
rheometers applied to these instruments is explained by this attribute. The technology
of internal mixers has been examined repeatedly, especially in the context of rubber
processing. Flow patterns in the chamber of an internal mixer were extensively
studied both experimentally and through sophisticated numerical simulations during
the processing of a polymer melt [5].
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APPLICATIONS:
Internal (Banbury-type) mixers have found widespread use in the rubber industry,
where high-power mixing is necessary for grinding and compounding; the technology
has been successfully applied to high-viscosity and low-viscosity plastics and
chemical systems [6]. The preparation of friction material mixes is a very challenging
task for internal mixing systems under technical aspects. The limitation of this type of
application is the variety of raw materials used and the high-level filler / matrix ratio
common for formulations of friction materials. Friction materials industry can be
divided into three main application areas such as:
Automotive Applications (brake pads and linings, clutch facings for cars and
trucks)
Railway Business (Brake pads for disc brakes and brake blocks for wheel
brakes)
Industrial Applications (Mining, Construction and agricultural machines,
Anchor winches, Electromagnetic brakes and clutches etc.) [7]
4. PROCEDURE:
First turn on the power supply button of internal mixer.
After that set the temperature of three heaters in the internal mixer.
Set the temperature in such a way that their average must be equal to the
melting temperature of the polymer.
In this experiment HDPE is being used and its melting temperature is 180οC.
After setting the temperature set the RPM of the internal mixer 45.
Give some time to the mixer for its pre heating.
After the pre-heating slowly add 40 g of HDPE in the mixer.
After two minutes, slowly add 2.5 g of yellow pigment in the mixer.
Mix the both material for 5 min.
Turn off the power supply and remove the master batch from the mixer.
Be careful while removing the master batch because the mixer is very hot.
After removing the master batch quickly clean the mixer by using cleaning
tools.
Observe the weight of the master batch after mixing by using weight balance.
Repeat the experiment be changing the temperature, RPM and mixing time.
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Fig: 6 (Sample 3)
6. DISCUSSION:
From the data given it is concluded that the temperature, RPM and time highly affect
the end product of the internal mixer. Temperature is a key parameter in mixing. If
the temperature is less than the melting temperature of the material then the material
will not mix uniformly and it can also the damage the machine. And if the exceeds the
melting point of the material then it will cause the degradation of the end product.
Time is also a key parameter in mixing. Mixing time is important for uniform mixing.
Mixing time has inverse relation with the temperature if the internal mixer because by
increasing the mixing time, the material can degrade and it will affect the properties
of the product. On the other hand, RPM also affect the mixing of the material. RPM
is very important for uniform mixing. High RPM can damage the rotors of the mixer
and can also cause flashing of the material.
From the calculations it can be seen that the weight of the product is decreasing after
the mixing it may be due to loss of material during the cleaning of the mixer. During
mixing some material attached to the walls of the mixer which causes the decrease in
the weight of the product. In these calculations time and RPM is changing which can
also affect the weight of the product.
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7. QUESTIONNAIRE:
Question: 1
Explain why it is necessary to incorporate compatibilizers and filler surface
treatment in the preparation of master batches.
Answer:
Compatibilization is a process that enhances the mixing properties while increasing
phase adhesion, reducing interfacial tension and stabilizing morphology. It is a
process through which the mixing properties are enhanced while increasing phase
adhesion, reducing interfacial tension and stabilizing morphology. Compatibilizers
act as additive to improve compatibility of immiscible polymers, their morphology
and the resulting properties of the blend [8].
Question: 2
What are color master batches? Explain their advantages and disadvantages in
polymer compounding.
Answer:
Master batch (MB) is a solid plastic additive used to color plastics (the color master
batch) or to impart other properties to plastics (the additive master batch). A liquid
phase of the medication is called liquid color. Master batch is a concentrated mixture
of pigments and/or additives encapsulated in a carrier resin, which is then cooled and
cut into a granular form during a heat cycle.
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Physical Property:
Master batch helps plastic improve a lot of physical property such as:
Higher toughness
Flexural stiffness
Adhesion
Printability
DISADVANTAGES IN POLYMER COMPOUNDING:
Master batches need extra storage space and longer lead times.
Another drawback is additional exposure of heat to both the carrier and the
additive; which is essential for marginally thermal stable pigments.
Master batches are premixed compositions; they use and mitigate the problems
with the additive deficient dispersion [9].
Question: 3
Prepare a list of the commercially important masterbatches available in
Pakistan. The list should include their names, formulation, functions and
concentrations required.
Answer:
Table: 2 (FAV Plastico (Pvt.) Ltd Masterbatches formulations) [10]
Masterbatch Formulation Functions Concentrations
White Polyolefin This product is Polyolefin (300
Masterbatch Styrene Polymers designed for g)
Premium TiO2 filming, injection, Styrene Polymers
Calcium blowing etc. of (300 g)
Carbonate general use. These Premium TiO2
masterbatches are (12-14 g)
used at an Calcium
additional level of Carbonate (5-10
1 per cent -5 per g)
cent depending on
the type of
application,
opacity/coloring
requirements and
end product
thickness.
Calcium Filler PE It has good PE (100 g)
Masterbatch PP physical PP (100 g)
Styrene resin as a properties that Styrene resin as a
carrier include; the carrier (20-30 g)
disperity, stability
and does not
affect the position
of the system
screw operation.
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HDPE based Base polymer This polymer is Base polymer
Wax used in (300 g)
Heat stabilizer manufacturing or Wax (3-7 g)
Compatiblizer preparation of Heat stabilizer (9-
Pigment polyethylene 11 g)
films. Compatiblizer (4-
98g)
Pigment(19-30 g)
PET based Base polymer Use in Base polymer
Wax engineering (800 g)
Heat stabilizer polymers for high Wax (8-10 g)
Compatiblizer strength Heat stabilizer
Pigment application. For (12-15 g)
example in blow Compatiblizer (9-
molding and 12 g)
extrusion Pigment(30-35 g)
Question: 4
Explain the importance of using laboratory scale internal mixers for carrying
out product development of polymer blends.
Answers:
In processing polymer blends, equipment selection, conditions, and formulation are
highly important to control the final morphology. Lab scale internal mixer is
important for the development of the polymer blends because through it we can
identify the effect of temperature, mixing time and RPM on the final product which is
useful information for industrial scale processes.
8. REFRENCES:
[1] “What is Banbury Mixer ? How to maintenance rubber banbury mixer? - FYI Tester.”
[Online]. Available: https://fyitester.com/what-is-banbury-mixer-how-to-maintenance-
rubber-banbury-mixer/. [Accessed: 18-Feb-2020].
[2] S. Ahmed Salahudeen, R. H. Elleithy, O. AlOthman, and S. M. AlZahrani,
“Comparative study of internal batch mixer such as cam, banbury and roller:
Numerical simulation and experimental verification,” Chem. Eng. Sci., vol. 66, no. 12,
pp. 2502–2511, 2011.
[3] “Schematic representation of distributive and dispersive mixing. Adapted... |
Download Scientific Diagram.” [Online]. Available:
https://www.researchgate.net/figure/Schematic-representation-of-distributive-and-
dispersive-mixing-Adapted-from-108_fig8_312306154. [Accessed: 18-Feb-2020].
[4] J. L. White, K. Min, and P. Science, “Specialty Polymers & Polymer Process- ing
Processing Methods Applicable to Thermoplastic Elastomers,” no. Figure 1, pp. 12–
16, 2017.
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[5] T. S. Alves, J. E. S. Neto, L. H. Carvalho, and E. L. Canedo, “Engineering modeling of
laboratory internal mixer,” Annu. Tech. Conf. - ANTEC, Conf. Proc., vol. 2, no.
January, pp. 1076–1083, 2014.
[6] “Process Plant Machinery--Internal Mixers: Single- and Twin-Screw Extruders (part
1).” [Online]. Available: http://www.industrial-electronics.com/engineering-
industrial/process-plant-mach_18.html. [Accessed: 18-Feb-2020].
[7] A. Schmitz, “Application and advantages of internal mixers in friction material
industry,” KGK Kautschuk Gummi Kunststoffe, vol. 63, no. 4, pp. 139–142, 2010.
[8] “Compatibilizers - an overview | ScienceDirect Topics.” [Online]. Available:
https://www.sciencedirect.com/topics/materials-science/compatibilizers. [Accessed:
19-Feb-2020].
[9] “(No Title).” [Online]. Available: https://www.plastics-technology.com/articles/an-
overview-masterbatch-plastics-technology. [Accessed: 19-Feb-2020].
[10] “Vawda & Co.” [Online]. Available: https://www.vawda.com/products/fav-
masterbatch.html. [Accessed: 19-Feb-2020].