微波辐射纳米稀土复合固体超强酸催化合成草酸二丁酯  

Synthesis of Bibutyl Oxalate by Catalysis of Nanosized Rare Earth Composite Solid Superacid under Microwave Radiation

作　　者：邓斌[1,2] 章爱华[3] 徐安武[2] 

机构地区：[1]湘南学院化学与生命科学系,郴州423000 [2]中国科技大学合肥微尺度物质科学国家实验室,合肥230026 [3]吉首大学化学化工学院,吉首416000

出　　处：《精细石油化工进展》2008年第5期31-34,共4页Advances in Fine Petrochemicals

基　　金：湖南省教育厅优秀青年科研基金项目(06B089)。

摘　　要：采用微波辐射技术,以纳米稀土复合固体超强酸SO_4^(2-)/ZrO_2-2%Nd_2O_3为催化剂,以草酸与正丁醇为原料合成草酸二丁酯。通过正交实验,探讨了诸因素对酯化率的影响,结果表明,纳米稀土复合固体超强酸So_4^(2-)/ZrO_2-2%Nd_2O_3催化剂具有良好的催化活性,当草酸用量为0.1 mol,醇酸摩尔比为3.0:1,催化剂用量为反应物总质量的1.6%,微波输出功率468 W,辐射时间14 min时反应的酯化率可达97%以上。该催化剂易于回收且可重复使用,具有价廉易得、催化效果好、操作简单、无环境污染等优点。Bibutyl oxalate was synthesized with oxalic acid and butyl alcohol as raw materials and nanosized rare earth composite solid superacid SO4^2-/ZrO2-2%Nd2O3 as catalyzer under microwave radiation. The factors influencing the synthesis were discussed. The results by orthogonal experiments showed that nanosized rare earth composite solid superacid SO4^2-/ZrO2-2%Nd2O3 was an excellent catalyst for synthesizing bibutyl oxalate. When the dosage of oxalic acid was 0. lmol, molar ratio of butyl alcohol to oxalic acid was 3.0： 1, the dosage of catalyst was equal to 1.6% （based on the total mass of feed stock）, microwave power was 468W, microwave radiation time was 14 min, the esterification ratio was more than 97%. Moreover,the catalyst could be easily recovered 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 纳米稀土复合固体超强酸SO4^2-/ZrO2-2%Nd2O3 草酸二丁酯 催化酯化 

分 类 号：TQ225.1[化学工程—有机化工]