微波辐射活性炭负载钨硅酸催化合成乙二酸二丁酯

Synthesis of dibutyl oxalate catalyzed by activated carbon supported tungstosilicic acid under microwave irradiation

借助微波辐射技术,以活性炭负载钨硅酸为催化剂,以乙二酸和正丁醇为原料合成乙二酸二丁酯.通过正交实验,探讨了诸因素对酯化率的影响,结果表明:活性炭负载钨硅酸具有良好的催化活性,当乙二酸用量为0.05 mol,醇酸摩尔比为2.6∶1,催化剂用量为反应物总质量的8.0%,微波输出功率为325 W,辐射时间为10 min,带水剂环己烷8 mL,在此优化条件下,反应的酯化率可达96.8%.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.

Dibutyl oxalate was synthesized with oxalic acid and butyl alcohol as raw materials and activated carbon supported tungstosilicic acid as catalyzer under microwave irradiation.The factors influencing the synthesis were discussed.The results by orthogonal experiments showed that activated carbon supported tungstosilicic acid was an excellent catalyst for synthesizing dibutyl oxalate.If the dosage of oxalic acid was 0.05 mol,molar ratio of butyl alcohol to oxalic acid was 2.6：1,the quantity of catalyst was equal to 8.0 %（based on the total feed stock）,microwave power was 325 W,microwave irradiation time was 10 min,the use level of water-carring agent cyclohexane was 8 mL.Under these optimum experimental conditions,the esterification ratio could reach 96.8 %.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.