A mixture of:
385 grams caustic soda
139 grams tri-cresol (mixture of isomers)
110 grams Water
500 grams castor oil
is subjected to mechanical agitation and gradually heated to 250°C. At about 135°C, water and some octanone-2 begin to distill of. These compounds
are condensed and recycled into the reaction apparatus. As the temperature rises, the rate of distillation of the water and the organic compounds
distill increases. At about 210°C. a discharge of hydrogen is observed. Heating is continued until a temperature of 250°C. is reached and this
temperature is then maintained over a period of 2 hours, all the while continuing to reflux the condensed volatile compounds into the reactor. After
the reaction has been completed, the recycling of the condensates is stopped and these condensates are recovered separately. The distillate comprises
a lower aqueous layer and an upper layer of organic products whie chiefly contain octanol-2. The organic layer is rectified, and 136 grams of a
mixture containing 95% octano1-2 and octanone-2 is recovered.
The reaction mass is dissolved in about liters water. The alkaline solution is acidified with diluted sulfuric acid until a pH of about 2 is obtained,
releasing the organic acids and the phenols. The mixture is brought to a boil, whereupon the sebacic acid becomes dissolved in water and the phenols
and other organic acids form a supernatant oily layer. The hot aqueous solution is subjected to a settling step, bleached with activated carbon and
filtered hot. On cooling, the sebacic acid crystallizes from the solution. The crystals are drained, washed with water and dried.
208 grams of 99% pure sebacic acid are obtained in this way. |
