微波辐射下活性炭固载固体酸催化合成草酸二丁酯  

SYNTHESIS OF DIBUTYL OXALATE CATALYZED BY ACTIVATED CARBON SUPPORTED TUNGSTOSILICIC ACID UNDER MICROWAVE IRRADIATION

作　　者：邓斌[1] 陈劲翔[2] 

机构地区：[1]湘南学院化学与生命科学系,湖南郴州423000 [2]中国矿业大学化学与环境工程学院,北京100083

出　　处：《精细石油化工》2010年第6期30-33,共4页Speciality Petrochemicals

基　　金：国家自然科学基金项目(20971118);湖南省教育厅重点科研项目(10A113);湘南学院重点科研课题(09Z010)

摘　　要：实验以草酸和正丁醇为原料,以活性炭负载钨硅酸为催化剂,在微波辐射下合成草酸二丁酯。通过正交实验,探讨了各因素对酯化率的影响,结果表明:活性炭固载钨硅酸催化活性良好。在草酸用量0.05 mol,n(正丁醇):n(草酸)为2.6:1,w(催化剂)=8.0%,微波输出功率325 W,辐射时间10 min,带水剂环己烷8mL条件下,反应的酯化率可达96.8%。该催化剂易回收并可重复使用。Dibutyl oxalate was synthesized with oxalic acid and butyl alcohol as raw materials and acti- vated carbon supported tungstosilicic acid as catalyst under microwave irradiation. The product was confirmed by infrared spectroscopy, gas chromatography and elemental analysis. The factors influencing the synthesis were discussed. The results by the orthogonally arranged experiments showed that the activated carbon supported tungstosilicic acid was an excellent catalyst for the synthesis of dibutyl oxalate. The optimal conditions were found as follows. 0.05 mol oxalic acid, molar ratio of butyl alcohol to oxalic acid 2.6 ： 1, 8.0% catalyst based on the total feed stock, microwave power 325 W, microwave irradiation time 10 rain, and the water-carrying agent cyclohexane 8 mL. Under these conditions, the esterification extent could reach 96.8%. In addition, the catalyst could be easily recov- ered and reused, and had characteristics of low cost, high catalytic efficiency, wide availability, easy operation, and environmental friendliness.

关 键 词：微波辐射 活性炭负载钨硅酸 草酸二丁酯 催化酯化 

分 类 号：TQ225.242[化学工程—有机化工] TQ426.91