Experiment No.3

Experiment No.
Objective: To understand the emulsion polymerization techniques by converting butyl acrylate and
acrylic acid into poly (butyl acrylate-co-acrylic acid)
Apparatus and materials required: Measuring cylinder, RB flask with lid, glass rod, magnetic stirrer,
water bath, burette stand, pH strips, thermometer, butyl acrylate (monomer 1), acrylic acid
(monomer 2), Sodium dodecyl sulphate(as surfactant), Ammonium persulphate(as initiator), Liquor
Ammonia, NaOH pallets, Distilled water
Theory:
Emulsion Polymerization
In emulsion polymerization, monomer (oil or water insoluble or partial soluble) is dispersed in the
aqueous phase (water) as a uniform emulsion. When monomer is added into water and agitated
emulsification takes place. The size of the monomer droplet form is around 10 -7 to 10-5 cm. Emulsion
is stabilized by surface active agent (surfactants) or protective colloids. The surfactant serves the
purpose of lowering the surface tension at monomer-water interface and facilitates emulsification of
the monomer in water. Above the critical micelle concentration, surfactant form micelle. In micelle
formation, the surfactant molecule aggregates in such a way that the polar end of the molecule
aligns themselves outward and the hydrocarbon ends come close to each other at the interior. Due
to proximity of the hydrocarbon ends of the all-surface active molecules, the interior of micelle acts
as hydrocarbon phase where the monomer can be solubilized. Water soluble initiators such as
persulphate or hydrogen peroxide or redox initiator are used in emulsion polymerization. The
surface layer of the micelle formed by polar end of the surfactant molecule is highly hydrophilic and
hence appreciable concentration is present at this place.
Polymerization starts at the surface layer of the micelle and proceeds towards inwards. When the
monomer present inside the micelle consumed, more monomers diffuse into micelle from the
monomer droplet present in aqueous phase. The chain growth continues till another radical species
enter and arrest the chain growth. With more and more polymer formation, the polymer chains
agglomerate into fine particles and get surrounded and then stabilized by the surfactant layer of the
micelle. As the polymer concentration increases, it absorbs the monomer and swells in size and
enlarge the size of micelle. At particular stage, the micelle bursts and surfactant molecules form an
absorption layer around the polymer particle. At the end of polymerization, fine particles of
polymer, stabilized by the surfactant layer and disperse uniformly in the aqueous phase and produce
milky white dispersion known as latex. The latex can be directly used for making adhesives or water-
soluble emulsion paints or the polymer can be isolated from the latex by destabilizing the emulsion,
by spray drying or freeze drying.
Monomers such as vinyl chloride, butadiene, chloroprene, vinyl acetate, acrylates, methacrylate are
polymerized by emulsion polymerization technique.
Advantages of emulsion Polymerization
 High molecular weight of polymers achieved.

 Fast polymerization rates
 Low viscosity even at high solid contents
 Independent control of rate and molecular-weight
 Allow removal of heat from system
 The final product can be used as such, does not need to be altered or processed.
Disadvantages of emulsion polymerization
 Contamination of products with additives

 More complicated in case of water soluble monomers
 For dry (isolated) polymers, water removal is an energy intensive process.
Acrylic emulsions of Poly (butyl acrylate-co- acrylic acid)
Acrylic emulsion is a milky white polymer emulsion that is mainly produced when acrylic monomer
undergoes polymerization by using an initiator in the presence of emulsifier with water as a solvent.
Acrylic polymer emulsions are a water-based polymer that can be produced from methyl
methacrylate, butyl acrylate, 2-Ethylhexyl acrylate, acrylic acid, methyl acrylate etc. polymers with
specific attributes for a variety of applications or uses can be produced by choosing appropriate hard
and soft monomers. Acrylic polymer emulsions and other water-based acrylic polymer products are
used as important tools by industrial coating and graphic arts industries. It also possesses excellent
water resistance properties that make it useful in the textile industry, such as – for flannelette
blankets, non-woven fabrics and lamination. Selected acrylic polymer products are also used in civil
engineering for – cement mortar, caulking and elastic cement. Acrylic polymer emulsions are used
for its various benefits like UV resistance, elongation balance, water resistance, good adhesion.
Procedure
1. In a rinsed and dried round bottom flask, 0.16g of emulsifier sodium dodecyl sulphate(SDS)
was combined with 40 ml of distilled water
2. Then, using a measuring cylinder, 24ml of butyl acrylate (BA) (monomer 1) and 16ml of
acrylic acid (AA monomer 2) were weighed and mixed with the solution.
3. To make the mixture basic, 50 mL of liquid ammonia (NH 3) was added, and the mixture was
agitated for 20 minutes with a magnetic stirrer.
4. Sodium hydroxide pellets were added as required during mixing to raise the pH from 4 to
between 7 and 8.
5. The temperature was steadily raised up to 80°C while the contents were stirred.
6. To start the polymerization, 0.16g of initiator ammonium persulphate (APS) was added to the
flask since it produces free radicals when heated.
7. The flask was sealed with a lid and heated for 30-40 minutes until it reached 80°C.
8. After 45 minutes, the flask was withdrawn from the stirrer and cooled in still air by removing
the lid.
9. Then, pour the content into the Petridish and put it in Hot air oven maintained at 105±1°C.
10. After complete drying, remove from oven, weigh it, and report the yield.
Results
Precautions

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Advantages of emulsion Polymerization

 High molecular weight of polymers achieved.

Disadvantages of emulsion polymerization

 Contamination of products with additives

Acrylic emulsions of Poly (butyl acrylate-co- acrylic acid)

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