酯化闭环法合成甲基丙烯酸缩水甘油酯的研究

Study on the synthesis of glycidyl methacrylate by esterification and ring-closing reaction

以苄基三乙基氯化铵为催化剂,采用酯化闭环法合成了甲基丙烯酸缩水甘油酯。通过对产物环氧值和产率的测定以及红外光谱和核磁共振波谱分析研究了酯化反应中阻聚剂种类及用量、催化剂用量、原料配比,反应温度以及闭环反应中原料配比对合成的影响。结果表明,酯化反应过程对产物的质量和产率影响较大。优化的反应条件为:阻聚剂4-甲氧基酚添加质量分数0.3%,催化剂质量分数0.8%,n(甲基丙烯酸)∶n(环氧氯丙烷)=1∶1.25,反应温度80~90℃,n(中间产物)∶n(50%Na OH水溶液)=1∶1.1,可使产物产率达到80%左右。

The glycidyl methacrylate was synthesized by esterification and ring-closing reaction using benzyl triethylammonium chloride as catalyst. The effects of inhibitor type and amount,catalyst amount,raw material ratio,reaction temperature of esterification and raw material ratio of ring-closing reaction were investigated by measuring the epoxy value and yield of the product and analysis of IR and NMR.The results showed that the effects of esterification reaction on the product quality and yield were great. The optimum conditions were as followed:mass fraction of polymerization inhibitor 4-methoxy-phenol 0.3%,mass fraction of the catalyst 0.8%,n(methacrylic acid)∶n(epichlorohydrin)= 1 ∶ 1.25,reaction temperature 80-90 ℃,n(intermediate)∶ n(50% Na OH solution)= 1 ∶ 1.1 and the yield of the product could reach 80%.