酯加成法合成甲基丙烯酸乙酰乙酰氧基乙酯的工艺研究

Study on Synthesis of Acetoxyethyl Methacrylate by Ester Addition Process

甲基丙烯酸乙酰乙酰氧基乙酯(AAEM)是非常重要的功能性乙烯基不饱和单体,在室温下很容易与固化剂发生反应,广泛用于丙烯酸酯的乳液聚合产品及丙烯酸酯溶液聚合产品的交联固化。本文以甲基丙烯酸羟乙酯和二乙烯酮为原料,研究了酯加成法合成AAEM工艺,考察了原料物质的量比、酯化温度、酯化反应时间、不同催化剂及用量、不同阻聚剂及用量等对反应收率和产品质量的影响,结果表明:最优工艺条件为甲基丙烯酸羟乙酯和二乙烯酮的物质的量比为1∶1.1,加入0.5%的催化剂三乙胺、0.05%的对羟基苯甲醚,升温到50℃反应6 h,反应得到的AAEM产品,反应总收率在90%以上,经GC检测产品主含量在98%以上。

Acetoacetoxy ethyl methacrylate(AAEM)is a very important fuctional vinyl unsaturated monomer,which can easily be reacted with some curing agent at room temperature and often used for crosslinking or curing of latex or solventborne polymers in the fields of coatings and adhesives based on polyacrylates. In this paper,hydroxyethyl methacrylate and diketene were used as raw materials,and a novel process for the synthesis of acetoacetoxy ethyl methacrylate by ester addition process was studied. The influences of the molar ratio of raw materials,reaction temperature,catalysts and their dosages,polymerization inhibitors and dosages as well as post-treatment process on the yield and purity of title product were investigated. Results showed that the optimal process conditions were as follows,the molar ratio of hydroxyethyl methacrylate to diketene was 1∶1. 1,the catalyst triethylamine was 0. 5% of the total materials,the inhibitor MEHQ was 0. 05% to hydroxyethyl methacrylate and thereaction was conducted for 6 hours at 50 ℃. The total yield of reaction was no more less 90%and the purity of the product was over 98%,which was determined by gas chromatography.