柠檬酸单月桂醇酯二钠盐的合成过程及光谱分析

Synthesis and Infared Spectral Analysis of Disodium Monolauryl Citrate

简述了柠檬酸月桂醇单酯二钠盐的合成过程。以乙酸酐、柠檬酸为原料 ,合成柠檬酸酐中间体 :柠檬酸∶乙酸酐 =2 0∶1 0 ,温度 36℃～ 37℃ ,反应时间 18h ,产率为 71 0 % ;酯化反应 :柠檬酸酐∶月桂酸=1 0∶1 1,温度 85℃～ 90℃ ,反应时间 2 0h ,单酯的产率为 83%～ 84 %。并采用红外光谱对合成过程中的原料、中间体及产物进行了研究。通过柠檬酸 ,柠檬酸酐及柠檬酸单酯二钠盐的红外光谱比较分析 ,证实了环状柠檬酸酐的形成。证明了直接制备高纯度的柠檬酸单月桂醇酯二钠盐工艺路线的合理性及可行性。同时表明可以用红外光谱对反应的中间体及产物进行验证。

The synthetic process of disodium lauryl monocitrate has been introduced. The optimum conditions of the citric anhydride were that the molar ratio of citric acid to acetic anhydride was 2.0:1.0, the reaction temperature was 36degreesC - 37degreesC, and the reaction time was 18 h. The yield of citric anhydride was 71.0%; the optimum conditions of esterification were that the molar ratio of citric anhydride to laury alcohol was 1.0:1.1, the reaction temperature was 85degreesC - 90degreesC, and the reaction time was 2.0 h. The yield of monocitrate was 83% - 84%. The raw material, intermediate and product were studied with infrared spectra. Comparing the results from citric acid, citric anhydride and disodium lauryl monocitrate, it was confirmed that the cyclo-anhydride was synthesized. The highly purified disodium monolauryl citrate has been directly prepared using this method. The technology is reasonable and feasible.