N-甲基咪唑硫酸氢盐催化合成增塑剂柠檬酸三丁酯

Catalytic synthesis of plasticizer tributyl citrate by N-methyl-imidazolium hydrosulfate

在离子液体N-甲基咪唑硫酸氢盐([Hmim]+[HSO4]-)的催化下,以柠檬酸和正丁醇为原料,合成了无毒增塑剂柠檬酸三丁酯。结果表明,[Hmim]+[HSO4]-催化合成柠檬酸三丁酯的最佳工艺条件为:n(柠檬酸)∶n(正丁醇)=1∶4.5,催化剂用量占反应物料总质量的5%,反应时间3.5 h,在此条件下产品收率97.31%,催化剂重复使用5次,仍保持较好的催化活性。产品经红外光谱、核磁进行定性分析,纯度经气相色谱分析大于99.0%。

Tributyl citrate was synthesized by citric acid and n-butanol with N-methyl-imidazolium hydrosulfate as catalyst.Experiment results indicated that the optimum process conditions were as follows：molar ratio of citric acid to n-butanol 1 ∶ 4.5,the amount of catalyst 5% of the mass of reactants,reaction time 3.5 h,the yield was up to 97.31%.After the catalyst being used for 5 times,activity did not significantly decline.Qualitative analysis of product was carried out by IR and NMR.Purity of product analyzed by GC was over 99.0%.