EXPERIMENT 4: SYNTHESIS OF POLYSULFIDE RUBBER

OBJECTIVE
Upon completion of this experiment, students should be able to:
1. synthesize polysulfide rubber (THIOKOL A)

INTRODUCTION

Polysulfide rubbers were among the first commercial synthetic rubbers produced. Two
chemists, Joseph C. Patrick and Nathan Mnookin, were trying to invent an inexpensive
antifreeze in 1926. In an experiment involving ethylene dichloride and sodium polysulfide,
they created a gum whose outstanding characteristic was a terrible odor. Trying to dispose of
it, the substance clogged a sink in the laboratory, and none of the solvents used to remove it
were successful. The chemists realized that the resistance of the material to any kind of solvent
was a useful property. They had invented synthetic rubber, which they christened "Thiokol,"
from the Greek words for sulfur (theion) and glue (kolla). The Thiokol Chemical Corporation
was subsequently founded on December 5, 1929.[1]

Thiokol rubber is a type of artificial elastomeric, which is invariably a polymer. An

elastomeric is a material with the mechanical property that it can undergo more elastic
deformation under stress as compared to most materials and then return to its previous size
without permanent deformation. Thiokol rubber acts as a substitute for natural rubber in many
cases. Now-a-days Thiokol rubber is used as a great deal in printing textile.[2]

Thiokol rubber are one of the important classes of polymers with excellent thermal
stability, weather-ability, solvent and oil resistance. Due to these characteristic properties, they
are used in coatings, adhesives, sealants, insulators, and other applications.[3]

Thiokol rubber is a polymer of ethylene polysulphide. Synthesis of Thiokol rubber can

be prepared by the condensation of 1, 2-dichloroethane with sodium polysulphide.

(Na2Sx, where x = 2–4)[2]

Two steps are involved for the synthesis of Thiokol rubber which are preparation of
polysulfide and the reaction of sodium polysulfide with ethylene dichloride.[1]
CHEMICALS
Sodium hydroxide
Sulphur
1,2-dichloroethane
Boiling chips

APPARATUS
Beaker
Conical flask, 500 ml
Condenser
Heating mantle
Two-neck round-bottom flask, 250 ml
PROCEDURE

Firstly, the apparatus was set up according to Figure 1. All glass to glass connections was
greased with a thin layer of grease. Next, 80.0 ml of distilled water was added to 10.0 g of
NaOH in a beaker. The mixture was stirred at room temperature until completely dissolved.
Then, this solution was poured into a two-neck round-bottom flask and slowly heated it.
after that, 13.0 g of sulphur was added into the hot solution (about 70 ºC). The reaction mixture
was reflux for 30 minutes. After this period, the mixture was allowed to cool slowly until 70
ºC. Boiling chips was added 3 pieces and 20 ml of 1,2-dichloroethane. The reaction mixture
was reflux again for 45 minutes. Filtered off the reaction mixture. The filtrate was discarded
into ‘chlorinated waste container’ and the polysulfide polymer was washed with distilled water
for several times to remove impurities. The polymer was dried with tissue paper and the weight
was recorded. Dried polymer was disposed in a water container/bottle.

Figure 1 shows Reflux set up.

RESULT.
Mass of polysulfide rubber obtained in the experiment = 9.4534 g

DISCUSSION
REFERENCE.
1. David A. Katz. (2010). Preparation of Synthetic Rubber. Journal of Chemical Education.
2. Swapna V & K.Mounika. (2018). A Study And Analysis Of Manifacturing Process Of
Thiokol Rubber . International Journal of Management, Technology And Engineering.
3. M. R. Kalaee, M. H. N. Famili, & H. Mahdavi. (2009). Synthesis and Characterization of
Polysulfide Rubber. WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.