一锅法制备甲基丙烯酸缩水甘油酯

PREPARATION OF GLYCIDYL METHACRYLATE BY ONE-POT METHOD

在过量环氧氯丙烷中,以季铵盐为催化剂,在阻聚剂存在的条件下,采用二氯甲烷共沸脱水,相转移催化一锅法制备了甲基丙烯酸缩水甘油酯。考察了反应时间,反应温度,催化剂种类等不同条件对产物收率的影响。结果表明,较佳的反应条件是:催化剂采用四丁基氯化铵,阻聚剂用量为甲基丙烯酸的1%,环氧氯丙烷用量为甲基丙烯酸的600%,反应温度80~85℃,反应时间3h。在此条件下,产物GC纯度大于98.5%,收率大于89%。

Glycidyl methacrylate was prepared by the one-pot method of phase transfer catalysis in ex- cess of epichlorohydrin,with quaternary ammonium salt as catalyst, in the presence of inhibitor, using dichloromethane azeotropic dehydration. The effects of reaction time, reaction temperature and cata- lyst type, etc. on the yield of the product were investigated. The optimal experimental condition is that tetrabutyl ammonium chloride was used as catalyst, the mass ration of polymerization in hibitor was 1 % of methacrylic acid, the mass ration of epichlorohydrin was 600% of methacrylic acid, the reaction temperature was 80 - 85 ℃, the reaction time was 3 h. Results showed that the GC purity of the product was over 98.5%, and the actual yield was over 89%