以马来酸酐和正丁醇为原料,用微波协同离子液体[ HSO3-pmim]+[ HSO4]-催化合成了马来酸二丁酯。通过单因素实验和正交试验考察催化剂种类、催化剂用量、马来酸酐与正丁醇物质的量比、微波功率、微波时间对马来酸二丁酯产率的影响。实验结果表明,马来酸二丁酯最佳合成条件为:马来酸酐与正丁醇物质的量比1∶4,以离子液体[HSO3-pmim]+[HSO4]-为催化剂,其用量为2.0g,微波功率为600W,微波时间为15min,马来酸二丁酯产率可达到99.36%。在微波辐射下,催化剂离子液体[ HSO3-pmim]+[ HSO4]-重复使用7次后活性没有明显降低,马来酸二丁酯产率仍高于96%,表明该催化剂具有较好的反应活性和稳定性。与常规加热方式相比,微波加热提高了反应效率,缩短了反应时间。
Dibutyl maleate was synthesized from maleic anhydride and n-butanol using ionic liquid[ HSO3-pmim]+[ HSO4 ]-as cat-alyst under microwave irradiation. The molar ratio of maleic anhydride and n-butanol,the type of catalysts and dosage,microwave power and irradiated time were explored by single factor experiment and orthogonal experiment. The results showed that optimal con-ditions were the molar ratio of maleic anhydride and n-butanol was 1∶4,dosage of ionic liquid[HSO3-pmim]+[HSO4]-catalyst was 2. 0g,microwave power was 600W,and microwave irradiated time was 15min. The yield of dibutyl maleate was up to 99. 36%under the optimized condition. The ionic liquid[ HSO3-pmim]+[ HSO4 ]-exhibited excellent stability and catalytic activity under the reac-tion conditions. Moreover, it could be reused seven times without considerable loss of activity with at least 96% conver-sion. Compared with conventional heating,microwave irradiation enhanced catalytic efficiency,as well as reduced reaction time.