Lab Report Emulsion Polymerization

Introduction
One of the most widely used polymer is polystyrene. Polystyrene is made up

from a monomer called styrene. The structure of polystyrene composed of a long
hydrocarbon chain with aromatic compound attach to the carbon. The monomer of
polystyrene which is styrene usually made up from petroleum.Polystyrene is a vinyl
polymer, it is made up from the styrene monomer by free radical vinyl
polymerization.
Figure 1.0 structure of polystyrene
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In this experiment, a polystyerene had been synthesized successfully. Usually, the

polymerization method that is used to synthesize polystyrene is the emulsion
polymerization. There are four important components that must be there in order to
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perform this emulsion polymerization method which are water, monomer, surfactant
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and water soluble initiator. The surfactant that is used in this experiment is the sodium
decodyl sulfate. In emulsion polymerization, each of the component have their own
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roles in facilitating the reaction. By performing this method, high molecular weight of
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polymer predicted to be obtained. Emulsion polymerization are performed via free

radical process where the initiator used will turn the monomer become a radical that
involve initiation, propagation and termination.
For this experiment, the monomer which is styrene supposedly prepared by

students but it was kindly prepared by the lab assistant. For the emulsion
polymerization process, about 0.0300g k2s2o8, 0.0300g na2hpo4 and 60ml of
distilled water were placed in a bottle. In the same bottle, surfactant was added
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according to the chosen set which are 1,4 and 7. The bottle were slowly shake until all
of the chemicals dissolved before adding 15ml of styrene. After that, the mixture
immediately bubbled with nitrogen gas for 1 minute and then the bottle was quickly
capped. The mixture were mixed together by shaking vigorously. Then, the bottles
containing the mixture being placed into water bath for 90 minutes. During 15
minutes interval, the bottle were taken out from water bath for shaking in 20 seconds.
10ml of coagulant solution was added after reaction time over. The product were
transferred onto a buchner funnel for filtration. By using 30ml of methanol and
distilled water, the solid polymer was washed. Lastly, the product was left overnight
in the vacuum oven for drying at 70C. The yield of dried products were obtained by
weighing the polystyrene obtained.
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Objectives
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1. To synthesize polystyrene by using emulsion polymerization.
2. To identify the mechanism involve in free radical polymerization.

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3. To determine the order of reaction according to the amount of surfactant used.

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Materials and Apparatus

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Procedure
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Figure 1.0 Graph of log Polystyrene yield against log[surfactant]
log PS yield vs log[surfactant]

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f(x) = 0.65 x + 1.98
R² = 0.98 0.9
0.8
0.7
0.6
log P S yield
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0
-2.6 -2.4 -2.2 -2 -1.8 -1.6 -1.4
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log [surfactant]
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Discussion
One of the method in synthesizing polystyrene is by emulsion polymerization.

Emulsion polymerization is one type of radical polymerization. In radical
polymerization, there are three important steps that involve initiation, propagatation
and also termination. The polymerization process will start once the initiator, water,
monomer and surfactant are mixed together and the mixture will start to emulsify. In
this experiment, it starts with mixing K2S2O8, Na2HO4 and surfactant in water. The
K2S2O8 is the free radical initiator and the reason why Na2HO4 added is to serve as
buffering agent in the reaction.
In emulsion polymerization, the monomer which is styrene will be stabilized by
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the surfactant added which is sodium dedocyl sulfate, SDS. The function of adding
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surfactant is to reduce the interfacial tension of reaction mixture. When the interfacial
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tension between the solutions are reduced, it allow the emulsification. The mixture is
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shake vigorously so it will well mixed together and forming a stable colloidal
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dispersion of a very tiny size particle called the micelles. At this state, the micelles
will provide the site for polymerization. Initiation steps will start when the initiator,
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K2S2O8 migrates into the micelles and react with the added monomer. The
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observation for this state is the solution become milky white solution. After that, the
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styrene is added into the solution as the reaction mixture is ready for polymerization
to form polystyrene. After addition of styrene, nitrogen gas is added slowly into the
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bottle for around 1 minute. The reason why this step is done to remove the oxygen gas
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by creating a nitrogen surrounding in bottle. The presence of oxygen will retard the
polymerization process and causing the reaction to become slower.
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As already mention that emulsion polymerization involve radical polymerization,

the initiation, propagation and termination process will be discussed. In initiation step,
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the initiator which is K2S2O8 will initiate the formation of radical species via
homolytic cleavage. When K2S2O8 split, the pair of electron will be broken and each
of electron will depart separately from each other. This splitting of electrons left two
fragments called the initiator fragments where each of them will have one unpaired
electron. The fragments are called the radicals. Upon addition of styrene, the double
bond in the monomer, will easily attacked by the free radical. After that, bond
between the initiator fragment and the carbon atom from monomer will formed. Then,
another electron from the double bond has nowhere to go causing the neighbour
carbon that not bonded to the initiator fragment to become radical. The mechanism in
initiation step is as follows:
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The next step is the propagation step. As initiation step causing the carbon atom
in monomer to become radical, thus it will react with other monomer by transferring
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an electron. This process will continue to happen as after the electron being
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transferred, another radical is created. Addition of more monomer creating long chain
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of polymer is called the chain reaction. This propagation steps will continue until all
of the monomer are used up.
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The final step in this chain-growth polymerization is the termination. There are
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two ways of how the polymerization terminate its process. The first one is by
disproportionation and the second one is by combination. In disproportionation, the
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polymerization will be terminated by formation of double bond at the end of polymer

chain. On the other hand, if the polymerization is terminated by combination, the end
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product will resulting a branched polymer. At the end of this reaction, coagulating
agent is added into the polymerization product. The coagulating agent used was the
aluminium sulphate. The role of coagulating agent is to neutralize the charges of
molecules and eliminate repulsive forces among the molecules. Once the coagulant is
added, the polystyrene will start to thicken and easier to be collected.
At the end of this experiment, the amount of yield for polystyrene in each set
were determined. The chosen set for our experiment are 1,4 and 7. For each set, the
yield are 2.3797g for set 1, 6.9201g for set 4 and 8.8509g for set 7. Based on the
graph of log PS yield against log[surfactant] in figure 1, it shows that the relationship
between the yield and amount of surfactant used are directly proportional. It is
because of the amount of surfactant used that helps in emulsifying the mixture. As the
surfactant aids to create more micelles and stabilize the monomer, it will provide
more site of polymerization thus it will resulting more product which is polystyrene
will form. Apart from that, the rate order of this emulsion polymerization of styrene
also obtained by plotting the graph of log PS yield against log [surfactant]. From the
slope, it is _____. By rounding up this value, the rate order obtained is 1.
Conclusion
In a nutshell, the proper technique of synthesizing polystyrene has been learnt
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from this experiment by performing emulsion polymerization. Apart from that, the
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mechanism of radical polymerization also has been discussed in the discussion part.
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The main steps that is very important in radical polymerization are initiation,
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propagation and termination. Finally, the rate order of emulsion polymerization of
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styrene is obtained from the graph of logPS yield against log[surfactant] which is first
order. The graph portrays a nearly linear relationship between the amount of
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surfactant used and the amount of polystyrene yield so it can be said that the
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relationship is directly proportional.

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As the result obtained are not very satisfying, it can be concluded that there are a
few errors happened while conducting this experiment. The mixture of solutions
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might not be vigorously shake thus the solutions are not perfectly mixed that resulting
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the polymerization process to be interrupted. Other than that, there might be some
oxygen that has not been displaced by the nitrogen gas which will affect the rate of
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polymerization. In addition, the actual yield of polystyrene for each sets are not very
accurate as some amount of the polystyrene were not transferred onto the filter paper
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for filtration as it stuck in the bottle and some might drop during the process of
transferring the polystyrene onto a petri dish for dying. Consequently, the yield of
polystyrene will decrease a bit from the supposed yield.
In order to increase the efficiency and accuracy of this experiment, there are some
precaution steps that need to be done. Firstly, the mixture should be thoroughly mixed
so that it will emulsify which will increase the rate of polymerization. On top of that,
during the bubbling of nitrogen gas into the solution, it should be done gently and
slowly to avoid the solution from spilling. After that, make sure to rinse the bottle
with enough solvent so that the filtration process will produce more amount of
product.
References
1. William Reusch. (Jul 7, 2015). Free Radical Polymerization. Retrieved from:
https://chem.libretexts.org/Courses/Purdue/Purdue_Chem_26100%3A_Organi
c_Chemistry_I_(Wenthold)/Chapter_08%3A_Reactions_of_Alkenes/8.7.%09
Polymerization/Free_Radical_Polymerization
2. Polymerdatabase.com. (2015). Retrieved from:
http://polymerdatabase.com/polymer%20chemistry/Polystyrene.html
3. Ana Maria Fernandez and Loubna Jebbanema. (Aug 1, 2007). The Effect of
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Surfactant Selection on Emulsion Polymer Properties. Retrieved from:
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https://www.pcimag.com/articles/87271-the-effect-of-surfactant-selection-on-
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emulsion-polymer-properties
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4.
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Kholtoff I. M. & Hansen J.L (1955). Mechanism of emulsion polymerization
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of styrene with persulfate as activator in the absence and presence of mercaptan and a
retarder. Retrieved from:
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https://onlinelibrary.wiley.com/doi/abs/10.1002/pol.1955.120158012
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Introduction

One of the most widely used polymer is polystyrene. Polystyrene is made up

Figure 1.0 structure of polystyrene

In this experiment, a polystyerene had been synthesized successfully. Usually, the

polymer predicted to be obtained. Emulsion polymerization are performed via free

For this experiment, the monomer which is styrene supposedly prepared by

2. To identify the mechanism involve in free radical polymerization.

3. To determine the order of reaction according to the amount of surfactant used.

Materials and Apparatus

log PS yield vs log[surfactant]

One of the method in synthesizing polystyrene is by emulsion polymerization.

As already mention that emulsion polymerization involve radical polymerization,

polymerization will be terminated by formation of double bond at the end of polymer

relationship is directly proportional.

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