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29.
离子液体催化合成丁二酸二甲酯
赵地顺1,刘猛帅1,徐智策1,张娟1,张笛1,付江涛1,任培兵1,2
化工学报
2012, 63 (4):
1089-1094.
DOI: 10.3969/j.issn.0438-1157.2012.04.015
Seven kinds of ionic liquids, N-methyl-imidazolium bisulfate([Hmim]HSO4),1-butyl-3-methyl imidazole phosphate([Bmim]H2PO4), 1-butyl-3-methyl imidazole bisulfate([Bmim]HSO4), 1-butyl-3-methyl imidazole tetrafluoroborate([Bmim]BF4), N-butyl-pyridine bisulfate([Bpy]HSO4), N-butyl-pyridine phosphate([Bpy]H2PO4), N-ethyl-pyridine bisulfate([Epy]HSO4), were designed and synthesized.The synthesis of dimethyl succinate catalyzed by ionic liquids was studied for the first time.It was shown that[Epy]HSO4 had the best catalytic performance, and optimal conditions for the synthesis of dimethyl succinate were obtained, succinic acid and methanol molar ratio 1∶3.0, amount of catalyst 5%(g/g)of succinic acid, reaction temperature 70℃ and reaction time 2 h.Under the optimal conditions, the yield of dimethyl succinate was up to 91.83%, esterification rate was 96.32%.The catalyst was recycled 7 times without substantial decrease in activity.Moreover, compared to conventional industrial catalysts, ionic liquid catalyst had the superiority of smaller catalyst dosage, less by-product, mild reaction conditions, high yield, and recycled catalyst usage.Finally, the mechanism of esterification catalyzed by ionic liquids was discussed.
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