Acetic Acid → Triacetin

Temperature

105 °C

An autoclave was charged with defined amounts of materials in a molar ratio of 6 mol of ethylene oxide per 1 mol of concentrated glycerol for cosmetics manufactured by Kao Corporation, and a reaction was carried out at 150° C. using a 1% by mol KOH as a catalyst with applying a given pressure of a reaction pressure of 0.3 MPa until the pressure was at a constant level, and the reaction mixture was then cooled to 80° C. to provide a reaction mixture containing a non-neutralized catalyst. KYOWAAD 600S (manufactured by Kyowa Kagaku Kogyo) was added as an adsorbent of the catalyst to the reaction mixture in an amount 8 times the weight of the catalyst, and subjected to an adsorption treatment at 80° C. for 1 hour in the presence of nitrogen. Further, a liquid mixture after the treatment was filtered with a Büchner funnel (Nutsche) in which a filter paper No. 2 was precoated with Radiolite #900 to remove the adsorbent to provide an ethylene oxide (6 mol) adduct of glycerol (hereinafter referred to as POE(6) glycerol). A four-necked flask was charged with this ethylene oxide adduct of glycerol, the contents were heated to 105° C. while stirring at 300 r/min, and acetic anhydride was added dropwise in a defined amount for about 1 hour, in a ratio of 7.2 mol per mol of the POE(6) glycerol to react. After the dropwise addition, the reaction mixture was aged at 110° C. for 2 hours, and further aged at 120° C. for 1 hour. After aging, unreacted acetic anhydride and a by-product acetic acid were subjected to topping under a reduced pressure, and a treated mixture was further steamed, to provide POE(6) glycerol triacetate. The resulting POE(6) glycerol triacetate had an average molecular weight of 490.

1. customto react
2. additionAfter the dropwise addition
3. waitfurther aged at 120° C. for 1 hour

ORD record

ord-74f28d6371204c86939edb24daca8f8c

Source dataset

uspto-grants-2013_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08455579B2