以莰烯和甲基丙烯酸为原料,采用直接加成酯化法合成甲基丙烯酸异冰片酯(IBOMA)。分析了反应时间、反应温度、莰烯与甲基丙烯酸的物质的量之比、催化剂种类及用量、阻聚剂种类及用量等对产物得率和反应选择性的影响,并采用正交试验对反应条件进行了优化,确定了适宜的合成工艺条件:以10%的Amberlyst 15作催化剂、0.03%的吩噻嗪作阻聚剂、甲基丙烯酸与莰烯物质的量之比为1.3∶1、酯化温度为60℃、反应时间为8~9 h,在此工艺条件下,产物甲基丙烯酸异冰片酯的平均得率为80.2%,平均选择性为95.3%,酯含量大于99.2%。采用GC-MS、FT-IR等分析技术对产物性能进行了表征。
Isobornyl methacrylate was synthesized by direct esterification of camphene and methacrylic acid. The synthe- sis conditions of isobornyl methacrylate were discussed. Effects including reaction time, reaction temperature, molar ra- tio of eamphene to methacrylie acid, types of catalysts and their dosage, types of antipolymerization inhibitors and their dosage on yield and selectivity were investigated. The optimum conditions were obtained by orthogonal test. The optimum conditions were 10% Amberlyst 15 as the catalyst (based on total mass of reactants percent) , 0.03% phenothiazine as the polymerization inhibitor, the molar ratio of methaerylic acid to camphene 1.3: 1, esterification temperature 60 ℃ , reaction time 8 - 9 h. The average yield and the selectivity of isobornyl methacrylate under the optimum conditions were 80.2% and 95.3% respectively, and the ester content was more than 99.2%. The structure of the isobornyl acrylate was analyzed by GC - MS, FT - IR and so on.