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

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.