Water → Epichlorohydrin

Temperature

20 °C

Epichlorohydrin (ECH) was polymerized in bulk in the presence of ethylene glycol as an initiator and BF3 catalyst. The reaction was conducted in a 2-liter, three-necked flask fitted with a mechanical stirrer, finnel, condenser and thermometer. The reaction was conducted while maintaining the flask in a water bath at 20° C. A total of 400 grams of epichlorohydrin was slowly added to a solution of 0.25 grams of BF3 in 25 grams of ethylene glycol at rate of about 20 grams per hour. Following the 20 hour addition of epichlorohydrin, the reaction mass was held in the water bath at 20° C. for an additional 4 hours. At the end of the reaction period, 300 iL of deionized water was added into the reaction mixture with stirring to inactivate the catalyst. The organic phase in the flask was then separated from the aqueous phase and the organic phase was dried at 40° C. under vacuum for one day. The polymerization temperature was controlled by adding the epichlorohydrin slowly so that the reaction temperature did not exceed 25° C. thereby obtaining a linear polyepichlorohydrin (PECH) diol having a relatively narrow molecular weight distribution with a polydispersity of about 1.2. The number average molecular weight and weight average molecular weight of the PECH diol as determined by gel permeation chromatography (GPC) were about 1400Mn and 1700MW.

1. customfitted with a mechanical stirrer
2. additionwas added into the reaction mixture
3. customThe organic phase in the flask was then separated from the aqueous phase
4. customthe organic phase was dried at 40° C. under vacuum for one day
5. additionby adding the epichlorohydrin slowly so that the reaction temperature
6. customdid not exceed 25° C.

ORD record

ord-5c7742fc24e547e088475fb8a69e3afe

Source dataset

uspto-grants-1998_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05777013