大孔树脂固载Ce~（4＋）催化合成薄荷酯的研究

目的]探索薄荷酯的最佳合成工艺。方法]以大孔树脂固载Ce4＋为催化剂,甲酸、乙酸和薄荷醇为原料合成甲酸薄荷酯和乙酸薄荷酯,采用正交试验优化2种薄荷酯的合成工艺。结果]醇酸摩尔比为1.0∶（1.4～1.6）,反应温度为125～135℃,反应时间为4～8h,催化剂用量为醇酸总质量的1%～2%时,乙酸薄荷酯的产率较高;醇酸摩尔比为1.0∶1.6,反应温度为120℃左右,反应时间为4h,催化剂用量为醇酸总质量的2%时,甲酸薄荷酯的产率最高。2种薄荷酯的最佳合成工艺为：醇酸摩尔比1.0∶1.6,催化剂用量为醇酸总质量的1.5%～2.0%,反应时间为4h,反应温度分别为120和135℃。结论]在最佳反应条件下,甲酸薄荷酯和乙酸薄荷酯的产率分别达到72.6%和60.0%。

Study on Menthyl Ester Synthesis Catalyzed by Immobilized Ce4+ on Macroporous Resin

Objective] The aim was to explore the optimum synthesis technology of menthyl ester.Method] With immobilized Ce4+ on macroporous resin as catalyst,the menthyl formate and menthyl acetate were synthesized with formic acid,acetic acid and menthyl ester as raw materials.Then their synthesis technologies were optimized through orthogonal test.Result] When the mol ratio of alcohols-acids was 1.0∶(1.4-1.6),the reaction temperature was 125-135 ℃,the reaction time was 4-8 h and the dosage of catalyst was 1%-2% of total mass of alcohols-acids,the yield rate of menthyl acetate was higher.When the mol ratio of alcohols-acids was 1.0∶1.6,the reaction temperature was about 120 ℃,the reaction time was 4 h and the dosage of catalyst was 2% of total mass of alcohols-acids,the yield rate of menthyl formate was the highest.The optimum synthesis technology of the 2 menthyl ester was as follows:the mol ratio of alcohols-acids was 1.0∶1.6,the dosage of catalyst was 1.5%-2.0% of total mass of alcohols-acids,the reaction time was 4 h and the reaction temperatures were 120 and 135 ℃ resp.Conclusion] Under the optimum reaction condition,the yield rates of menthyl formate and menthyl acetate reached 72.6% and 60.0% resp.