9-OAHSA synthesis

Yield:154086-90-5 274 g

Reaction Conditions:

with perchloric acid at 60; under 10 Torr; for 24 h;

Steps:

D D. Estolide Bonding of Oleic Acid

(0107) 341 g out of 682 g of the oleic acid obtained in operation C and 8.5 g of 70% purity perchloric acid were introduced into a 500 cc flask, which in turn was ‘connected to a fractional distillation apparatus (Spaltrohr HMS 300C, Fischer technology Co., Ltd.). Next, the fractional distillation apparatus was heated to 60° C., followed by reducing the pressure of the fractional distillation apparatus to 10 torr, and then maintained for 24 hours while slowly stirring the components. The resulting material was introduced into a 2 L beaker, followed by quenching with a mixed solution of KOH/ethanol/DI-water (3.4 g/100 cc/900 cc) while stirring the resulting material. After confirming by pH measurement that remaining acid was not present in the mixed solution, the mixed solution was left until the temperature of the mixed solution decreased. Next, the mixed solution was introduced into a separatory funnel and settled, followed by selectively removing a water layer after the water layer and an organic layer were separated. The separated organic layer was introduced again into the fractional distillation apparatus (Spaltrohr HMS 300C, Fischer technology Co., Ltd.), and cut at 385° C., thereby removing the unreacted material. 49 g of the unreacted material was separated, and 274 g of an estolide polymer was secured.

References:

US2016/9630,2016,A1 Location in patent:Paragraph 0106-0107