REACTION

FORMULATION
CHEMICAL
methyl methacrylate
butyl acrylate
Sodium lauryl sulfate
Potassium persulfate
NX-100

QUANTITY
3% of charge =
1% of charge =
3% of charge =

CALCULATION
Material Balance Calculations,

EMULSION COPOLYMERIZATION OF
METHYL METHACRYLATE AND BUTYL
ACRYLATE
AIM
Emulsion copolymerization of methyl methacrylate (MMA) and butyl acrylate (BA).

APPARATUS
Three-necked flask, silicon stirrer, reflux column, thermometer cap, thermometer, heating
mantle, Dean-Stark apparatus, clamps, electric motor, rubber wire, beaker, conical flask. glass
rod, burette, etc.

CHEMICALS
Methyl methacrylate (MMA), butyl acrylate (BA), NX-100, sodium lauryl sulfate, potassium
persulfate etc.

THEORY
Emulsion polymerization is a versatile technique, widely used in industry to produce latexes for a large
variety of applications including paints, coatings, adhesives, and binders in the textiles and paper
industries1 Acrylics are a family of emulsion polymers extensively used in industry, with n-butyl
acrylate/methyl methacrylate (n-BA/MMA) being one of the most commonly used monomer systems.
This comonomer system is extremely versatile, and depending on the weight ratio between the
comonomers, latexes used for very different applications can be produced. Typically, copolymers with a
50/50 wt/wt n-BA/MMA composition are used for coatings, and those with at least of 90 wt% of n-BA are
used as adhesives. The end-use properties of these latexes depend on the microstructural properties of the
polymer; therefore, to meet the increasing demands on product quality, the structural properties of the
polymer should be con-trolled. To achieve this control, it is important to understand the fundamental
physicochemical phenomena involved in the emulsion copolymerization of n-BA and MMA. An
important aspect of this monomer system is that a gel can be formed, and the gel fraction strongly affects
the final properties of the product. To develop proper control strategies, a mathematical model able to
describe the copolymerization kinetics and the evolution of the aforementioned polymer properties should
be used. N-BA/MMA semi batch emulsion polymerizations at a fixed 50/50 molar composition. No
substantial effect of the CTA on the kinetics was observed, but the MWD decreased with the CTA
concentration, and a concentration of 1 wt % CTA was enough to avoid gel formation during the process.

PROCEDURE
1. Set the reaction assembly and charge one-third gram moles of and 1.2 moles of PPG in
the reactor along with PTSA and hydroquinone.
2. Start heating and stirring and continue for one hour under conditions of total reflux.

For Polymer content,

%Polymer content = Wt. of sample before heating Wt. of sample after heating x 100
Wt. of sample before heating
For NVM,
%NVM = Wt. of sample before heating Wt. of sample after heating x 100
Wt. of sample before heating
3. After 45 minutes add two-third gram moles of Maleic anhydride and continue heating
under total reflux for one hour more.
4. Attach azeotropic leg, i.e., the Dean-Stark apparatus and fill it to overflow point with
Xylene and add 15 mL of Xylene in the reaction mixture.
5. Heat the reaction mixture slowly upto 1500C to 2000C, and after every 15 min take out
about 1 g of sample to find out acid value.
6. When the acid value drop to between 25 to 50, stop the reaction. Drain out the azeotropic
mixture from the Dean-Stark apparatus.
7. Switch off the heating mantle as well as electric motor. Collect the final UPR resin
(product).
8. Weigh the resin to find the yield.

DETERMINATION OF POLYMER CONTENT

1.
2.
3.
4.
5.
6.
7.

Take 5 g of emulsion formed in a beaker and add 50 mL (excess) of methanol.

Weigh the beaker in which the sample is taken.
The copolymer will gel and the emulsion will break. Repeat this washing several times.
Add 2-3 drops of 0.2N HCl so to completely break the emulsion.
Now decant the solvent layer keeping the copolymer safe.
Keep this for heating for 20 to 30 minutes in an oven at 50C.
Calculate the polymer content.

DETERMINATION OF NON-VOLATILE MATTER (NVM)

1. Take a clean and dry petri dish and weigh it.
2. Take about 1 g of resin on the petri dish.
3

3. Keep it in the oven at about 100-110oC for one hour to remove the volatile components.
4. Weigh the petri dish with the sample.
5. Calculate the NVM of the resin.

PRECAUTIONS

Keep a note on the temperature every time. Do not let it cross 60C.
.Keep a control on the froth formed by washing the beaker with cold water.
While pouring hot resin in the beaker, make sure that the beaker is dry.
Use only silicon oil in the thermometer cap. Make sure that the bulb of the thermometer
is fully immersed in the oil.
Avoid direct inhalation of the fumes.
Clean the pipette with hot water immediately after use to avoid blockage by solidified
resin.

OBSERVATIONS
The polymer content of the copolymer formed is

The volatile matter present is

RESULTS
Weight of resin obtained =
Polymer content =
Volatile content =

HANDLING HAZARDS

Inhalation - Can cause central nervous system (CNS) depression. Irritating to

respiratory system.
Ingestion - Can cause central nervous system (CNS) depression.
Skin - Irritating to skin. May cause sensitization by skin contact.
Eyes - Irritating to eyes.
Chronic effects - Contains material that can cause target organ damage.
Carcinogenicity - Contains material which may cause cancer, based on animal
data. Risk of cancer depends on duration and level of exposure.
Target organs - Contains material which causes damage to the following
organs: kidneys, liver, upper respiratory tract, eyes, central nervous system
(CNS), ears.

PROPERTIES

APPLICATIONS