以离子液体[HSO3-pmim]^+[HSO4]^-为催化剂,马来酸酐和甲醇为原料,硫脲为异构化试剂,在微波条件下,通过酯化反应催化合成富马酸二甲酯。通过单因素实验和正交试验考察了马来酸酐与甲醇物质的量比、催化剂用量、微波功率和微波时间对富马酸二甲酯产率的影响。实验结果表明,合成富马酸二甲酯最佳条件为:马来酸酐与甲醇物质的量比为1∶6,催化剂离子液体[HSO3-pmim]^+[HSO4]^-用量为2.5g,微波功率为400 W,微波时间为7min,富马酸二甲酯的产率可达95.3%。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,富马酸二甲酯产率仍高于90%,表明该催化剂具有较好的反应活性和稳定性。
The dimethyl fumarate was synthesized using maleic anhydride and methanol with mi-crowave-assisted in presence of ionic liquid [HSO3-pmim]^+[HSO4]^- as catalyst and sulfocarbam-ide as isomerization agent.The molar ratio of maleic anhydride to methanol,the amount of cata-lyst,microwave power and microwave time were explored by single factor experiment and orthog-onal experiment.The results show that under optimal conditions for the synthesis of dimethyl fu-marate,the molar ratio of maleic anhydride to methanol being 1∶6,the amount of catalyst being 2.5 g,the microwave power being 400 W,and microwave time being 7 min,the dimethyl fumar-ate yield was up to 95.3%.In microwave irradiation,the ionic liquid [HSO3-pmim]^+[HSO4]^-exhibited excellent stability and catalytic activity,and it can be reused seven times without consid-erable loss of activity and still makes the conversion rate reach to above 90%.