Acetic Acid → Triacetin

Participants

Reaction Conditions

Reaction Steps

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.

Provenance & Evidence