CHAPTER 3

Material and Methods:

3.1 Chemicals:
Allyl Bromide.
Mercapto Ethanol
Saccharin Sodium
Ethanol
Dimethyl sulphoxine (DMSO)
Sulphuric Acid
Dichloromethane
Titanium Chloride (TiCl3)
Aluminium
Sodium Chloride (NaCl)
Acetone
Sand

3.2 Apparatus:
Heating Mental
Iron stands
Cononical Flasks (Quick fit )
Fractionating Column
Condenser
Round Buttom Flasks
Plastic pipes
Water pump
 Electric oven
Cotton
Capilliary tubes
Test tubes
Test tube holders
Test tube stands
Spirit lamp

3.3 Purification of Solvents:

Purification of DMSO
For purification of DMSO we need,
1. Quick fit (any flask)
2. Heating mental
3. Fractionating column
4. Condenser
5. Flask (for collection)

Procedure
1. First of all take some DMSO according to need for experiment and put into
Quick fit.
2. Switch on the heating mental the DMSO present in the quick fit start
warming and then start boiling when temperature reaches 189 degrees
Celsius.
3. At boiling temperature, the evaporation process just begins and the liquid
form of DMSO is converted in gaseous form and these gaseous form is
passing through Fractionating column where it seperate the mixture of
vapours.
 4. The vapours passing through condenser condense again into liquid form of
DMSO through process of condensation because of the rapid decrease in
temperature.
5. The liquid form of DMSO after the process of distillation is collected in flask
which is 99 percent pure and now we can used it in our experiment.

3.4. Alkyl Halide (Ethyl Chloride)

Purification of ethanol
We purify the ethanol to removes the impurities present in it which can
hurdle in our experiment.
For that reason the ethanol is purified through the same procedure as we
did to DMSO.
The purified ethanol is now available for our experiment.

3.4 Distillation of Chemicals:

3.5 Chemical Properties of Chemicals:

Allyl bromide is a clear liquid with an intense, acrid, persistent smell and is
flammable. It is insoluble in water, but soluble in alcohol, ether, acetone, carbon
tetrachloride, and chloroform.
2-Mercaptoethanol is widely used because the hydroxyl group confers solubility
in water and lowers the volatility. Due to its diminished vapor pressure, its odor,
while unpleasant, is less objectionable than related thiols.
Sodium and calcium saccharine are white crystalline powders that are very
soluble in water. It has no caloric value and does not promote tooth decay. It is
not metabolized by the body and is excreted unchanged.
Saccharin, sodium salt appears as odorless white crystals or crystalline powder.
Aqueous solution is neutral or alkaline to litmus, but not alkaline
to phenolphthalein. Effloresces in dry air. Intensely sweet taste.
Ziegler–Natta catalyst is a type of catalyst made from a mixture of chemical
compounds that are mainly used in the synthesis of polymers belonging to 1-
alkenes such as alpha-olefins which are hydrocarbons containing a double carbon-
carbon bond.
Ziegler-Natta catalyst, any of an important class of mixtures of chemical
compounds remarkable for their ability to effect the polymerization of olefins
(hydrocarbons containing a double carbon–carbon bond) to polymers of high
molecular weights and highly ordered (stereoregular) structures.

3.6 Physical Properties of Chemicals:

3.6.1 Allyl bromide;
Density 1.398 g/cm;
Melting point −119 °C (−182 °F; 154 K);
Boiling point 71 °C (160 °F; 344 K).

3.6.2 Mercaptoethanol;

Odor Disagreeable, distinctive;

Density 1.114 g/cm3;

Melting point −100 °C (−148 °F; 173 K);

Boiling point 157 °C; 314 °F; 430 K;

3.6.3 Saccharin;
Appearance White crystalline solid;

PH Range 2–7

Temperatures 150° C (302° F).

Density 0.828 g/cm;

Melting point 228.8 to 229.7 °C

(443.8 to 445.5 °F; 501.9 to 502.8 K);

Solubility In water.

3.7 Preparation of Catalyst

Ziegler natta catalyst is prepared by mixing ethene, sodium, aluminium powder and titanium
chloride.
First we prepare a ethyl chloride which require for the catalyst preparation. For this we set all
require aquipments and chemicals. We set a round bottom flask in a heating mental and fit a
fractionating column on it. Now we set a condenser with a column and a reagent bottle is fixed
with a condenser to collect the ethyl chloride.
After setting all the required setup we start a reaction. For this we put a sodium chloride in a
flask which is fitted in a heating mental and also added a some amount of ethanol mixed both
and added a sulphuric acid in it and start a heating process.
After sometime the reaction starts and the desire product formed. We collect it in a reagent
bottle and check by the help of flame test. If it gaves a blue flame it is our desired. After this we
took a some amount from it and start a next reaction.
Now the time is reached to mix the sodium with ethyl chloride and also added a aluminium in a
powdered form in the solution and start a stirring for a 24hours.
After stirring the titanium chloride in added in it.
So our desired catalyst is prepared which we are going to use in the synthesis of polymer.

3.7.1 Preparation of ethene

Procedure:
1. Add some appropriate amount of H2SO4 to ethanol with some amount of NaCl
already present in flask.
2. The flask is attached with fractionating column and condenser and at the end of
which attached another flask to collect ethene.
3. The flask containing a mixture of NaCl, H2SO4 and Ethanol is placed on heating
mental so that the reaction is takes place and ethene is produced.
4. The ethene produced is in gaseous form the gaseous form of ethene is passed
through fractionating column and finally through condenser, the condenser is used
to cooled down the vapours into liquid form.
5. The flask used for collection is placed in ice cubes so that it can not converted again
into vapours form as it has very low boiling point.

3.7.2 Mixing of ethene with sodium (M1)

The ethene produced is now mixed with sodium and then stirrer in magnetic stirrer hot plate
for 24 hours.

3.7.3 Mixing of Aluminium powder with M1

The M1 produced is now mixed with Aluminium powder and stirrer for 24 hours
in magnetic stirrer hot plate.
Let we have a product named as M2.

3.7.4 Addition of TiCl3 to M2

The titanium chloride is added to M2 to formed the final product ziegler natta catalyst.
This catalyst is used for further our reaction.

3.8 Product SAH1

We took a few ml of marcapto ethanol in a conical flask by the help of pepite and
mixed with a allyl bromide and set it on the magnetic hot plate for a stirring and
leave it for a 24hour at stirring.
After 24hours we put a catalyst as ziegler natta and pass a ethene gas from the
solution until the liquid starts changing into solid .when the light yellow solid
product form that is our product.
We repeat this for three times at the end the SAH1 is formed now we take a
spectra for this product.

3.9 Product SAH2

We took sodium salt of saccharine and allyl bromide are mixed in the presence of
DMSO as a solvent to produce SAH2.The pale yellow liquid is formed at the end
this is our desire product which we are going to use in the formation of long chain
polymer.
3.10 Product SAH3
We took a few ml of marcapto ethanol in a conical flask by the help of
pepite and mixed with a allyl bromide and set it on the magnetic hot plate for a
stirring and leave it for a 24hour at stirring.
After 24hours we put a catalyst as ziegler natta and passed a ethene gas from the
solution until the liquid starts changing into solid. When the light yellow solid
product form that is our product.
Now we washed our product by using different solvents like water, chloroform,
dichloromethane.
3.10.1 Washed with Water;
We took our product which is prepared in a labortary in a solid from the
round bottom flask to the small beakers and put some amount of water to
remove the impurities present in a product. After this we dicorded the water from
the sample and leaved it for a day to dry. When this dried we use an other solvent
like chloroform.
3.10.2 Washed with Chloroform;
Now we use chloroform for washing the sample after using water. When
sample is dried we added a chloroform in a sample and after a few hours discord
a chloroform from the sample and leave a sample for a day to evaporate a
chloroform from the sample. The sample dried after a day or two.
3.10.3 Washed with Dichloromethane;
The sample is dried after some days the chloroform evaporated in a open
atmosphere. After chloroform we washed a sample with dichloromethane. We
added a few ml of dichloromethane and shaked a sample to remove the
impurities which are dissolve in a dichloromethane. Few hours we discorded a
dichloromethane and leave it for drying. The sample dried we took a spectra by
the help of infrared spectrometer.
3.11 Product SAH4
We took some amount of marcapto ethanol in a conical flask and mixed
with a allyl bromide. And set on a magnetic hot plate for a stirring and stire it for
24hour. After that we prepare another solution in which we took a sodium salt of
saccharine and allyl bromide in a flask and dissolve them in the presence of DMSO
solvent. Now we mixed both the solution in a round bottom flask and add a few
drop of ziegler natta catalyst in it. After this we pass a ethene gas from the
solution and the product SAH3 prepared in a solid form. Now we take this yellow
solid and take its spectra by the help of infrared spectrometer.