耦合法制备甲基丙烯酸甘油酯工艺研究

摘要

The reactive diluent glycerol methacrylate was synthesized from glycerol and methyl methacrylate by coupling technology. The reaction conditions including different catalysts,polymerization system and the ratio of reaction materials were investigated and optimized. The optimal conditions were obtained as follows: the catalyst anhydrous potassium carbonate (7% of the glycerol mass), hydroxyanisol inhibitors, and molar ratio of alcohol to esters 1:9, refluxing time 7 h. Under above conditions, the total content of glycerol trimethacrylate and glycerol dimethacrylate can reach to 95.66%. GC and LC-MS were applied to characterize the products.%以价格低廉的甲基丙烯酸甲酯和甘油为原料，利用反应分离耦合技术，通过酯交换反应合成了光固化体系的主要成分活性稀释剂甲基丙烯酸甘油酯。考察并优化了催化剂、阻聚体系、投料比等并得到了最佳工艺条件：无水碳酸钾为催化剂，用量为甘油质量的7%；空气和对羟基苯甲醚为复合阻聚剂体系；甘油与甲基丙烯酸酯投料摩尔比为1：9，回流反应7 h。在此工艺条件下，产品中三甲基丙烯酸甘油酯与相应双酯的总含量达95.66%。采用气相色谱仪及液相色谱-质谱联用仪等对过程及产品进行监控及定性定量分析。