阳离子交换树脂催化合成草酸葑醇酯

Synthesis of fenchyl oxalate catalyzed by cation exchange resin

阳离子交换树脂作为绿色环保型催化剂广泛应用于有机化合物的合成,通过催化反应,以葑醇和草酸为原料,合成草酸葑醇酯。考察催化剂类型、催化剂用量、反应温度、反应时间以及原料物质的量比对葑醇酯化反应的影响,通过单因素实验确定了酯化反应的最佳条件:催化剂为阳离子交换树脂NKC-9,催化剂用量为葑醇质量的50%,反应温度55℃,反应时间96 h,n(草酸)∶n(葑醇)=4∶1。在该条件下,葑醇平均转化率为92.06%,草酸葑醇酯平均选择性为93.51%,平均收率为86.07%。催化剂重复使用7次后,葑醇转化率为87.15%,草酸葑醇酯选择性为89.44%,收率为77.95%。NKC-9催化剂可以取代酰氯法合成草酸葑醇酯,具有环保和经济等优点。

Cation exchange resin as green catalysts is widely used to synthesize organic compounds. Using fenchyl alcohol and oxalic acid as the raw materials, fenchyl oxalate was synthesized by the catalytic reaction. The effects of the types and dosage of the catalysts, reaction temperatures, reaction time and molar ratio of oxalic acid to fenchyl alcohol on esterification were investigated by single factor experiments. The optimum reaction condition was determined as follows：the best catalyst cation exchange resin NKC-9, catalyst dosage 50% of fenchyl alcohol mass, reaction temperature 55 ℃ ,reaction time 96 h, molar ratio of oxalic acid to fenchyl alcohol 4： 1. Under the optimum condition ,the average conversion of fenchyl alcohol of 92.06%, the average selectivity to fenchyl oxalate of 93.51%, and the average yield of fenchyl oxalate of 86.07% were attained. After the catalyst was reused for 7 times, the conversion of fenchyl alcohol was 87.15 %, the selectivity to and the yield of fenchyl oxalate were 89.44% and 77.95 %, respectively. The catalyst NKC-9 had the advantages of environmental protection and economy, and could be used as the replacement of acyl chloride method to synthesize fenchyl oxalate.