酸性离子液体[N4H4(CH2)6].4HSO4催化合成氯乙酸乙酯的研究

Synthesis of Ethyl Chloroacetate Catalyzed by Acidic Ionic Liquid [N4H4(CH2)] .4HSO4

摘要:

以六次甲基四胺和浓硫酸为原料制备了酸性离子液体[N4H4(CH2)6].4HSO4，将其应用到氯乙酸乙酯的合成中，并对酯化反应涉及的工艺参数进行了优化，采用核磁共振波谱对产物进行了表征。结果表明：n（氯乙酸）：n（乙醇）=1:1.8，离子液体用量为氯乙酸总质量的30%，反应温度100℃，反应时间3.5h，氯乙酸乙酯收率为93.27%。重复使用6次，氯乙酸酯收率为90.16%。产品易分离，克服了无机酸催化的缺陷。

Abstract:

An acidic ionic liquid [N4H4(CH2)].4HSO4 was prepared with the raw materials of hexamethylenetetramine and concentrated sulfuric acid, and it was applied to the synthesis of ethyl chloroacetate. The technological parameters involved in esterification reation were optimized. Structures of the title compound and the catalyst were confirmed by 1HNMR. The results showed that n(chloroacetic acid):n(ethanol)=1:1.8, the amount of ionic liquid was 30% of the total mass of chloroacetic acid, the reaction temperature was 100℃, the reaction time was 3.5h and the yield of ethyl chloroacetate was 93.27%.When the acidic ionic liquid was repeated 6 times, the yield of ethyl chloroacetate was 90.16%. The product was easy to separate and the acidic ionic liquid overcomed the defects of inorganic acid catalyst.