微波辐射活性炭负载磷钨酸催化合成丙二酸二乙酯  

Synthesis of diethyl malonate catalyzed by activated carbon supported tungstophosphoric acid under microwave irradiation

作　　者：邓斌[1,2] 张晓军[2] 徐安武[2] 王存嫦[1] 

机构地区：[1]湘南学院化学与生命科学系,湖南郴州423000 [2]中国科技大学合肥微尺度物质科学国家实验室,安徽合肥230026

出　　处：《石油化工应用》2009年第6期8-12,共5页Petrochemical Industry Application

基　　金：湖南省自然科学基金资助项目(07JJ3017);湖南省教育厅重点资助科研项目(08A065)

摘　　要：研究了微波辐射下,利用活性炭负载磷钨酸作催化剂,丙二酸和乙醇为原料,催化合成丙二酸二乙酯,考察了影响反应酯化率的各主要因素其优化反应条件为:当丙二酸用量为0.15mol时,醇酸摩尔比为2.8:1,催化剂用量1.30g(磷钨酸负载量为35%时),微波辐射功率325W,微波辐射反应时间10min,带水剂(环己烷)用量8.00mL,在此条件下反应的酯化率可达97.6%实验结果还表明:在各自优化条件下,利用活性炭负载磷钨酸作催化剂,微波辐射法比常规加热法,反应速度加快了18倍。By using activated carbon supported tungstophosphoric acid as acatalyst, malonic acid and ethyl alcohol reacted to form diethyl malonate under microwave irradiation. The primary factors affecting the yield of esterfication were investigated. Results showed that the optimum conditions were as follows： when malonic acid was 0.15 mol, the molar ratio of ethyl alcohol to malonic acid was 2.8：1, the percentage of activated carbon supported tungstophosphoric acid was 35 % and 1.30 g microwave irradiation 10 min, the agent taking Under these optimum experimental conditions, catalyst was used, microwave power 325 W, of water amount of cyclohexane was 8.00 mL. the yield of esterification reached to 97.6 %.The experiments proved that activated carbon supported tungstophosphoric acid was a high active catalyst for diethyl malonate and could be reused under microwave irradiation. The reaction was 18 times faster under microwave irradiation than conventional heating.

关 键 词：微波 活性炭 磷钨酸 负载催化剂 丙二酸二乙酯 

分 类 号：TQ225.242[化学工程—有机化工]