采用两步法合成甲基丙烯酸缩水甘油酯(GMA).通过中和反应,由甲基丙烯酸和氢氧化钠反应制得甲基丙烯酸钠盐;经研磨干燥,加入不同的阻聚剂和相转移剂,与环氧氯丙烷(ECH)按一定比例在干燥的反应体系中反应,减压蒸馏后得到产物.结果表明:该反应的最佳阻聚剂为对苯二酚,相转移催化剂为四丁基溴化铵(TBAB).通过正交实验设计优化了反应条件:反应温度90~95℃,反应时间4 h,物料配比w(甲基丙烯酸钠)∶w(ECH)=1∶6.产率达到86.5%,用盐酸丙酮法测得环氧值高达98.6%.
Glycidyl methacrylate(GMA) was synthesized through two steps. Firstly, Sodium methacrylate was prepared from methyl acrylic acid and NaOH, which was ground and dried. With different inhibitors and phase transfer catalysts, GMA was gained by the reaction of Sodium methacrylate and Epichlorohydrin(ECH) with a certain percentage in a dry reaction system and distilled through vacuum distillation. The results show that hydroquinone is the best inhibitor, and phase transfer catalyst is tetra-butylammonium bromide (TBAB). The optimum reaction conditions are obtained by the orthogonal experimental design : the reaction temperature is 90 - 95 ℃, the reaction time is 4 h,w(sodium methacrylate) :w(ECH) = 1:6. Under the given conditions the yield of products can reach 86. 5% with purity of 98.6%.