固载磷钨酸催化氯乙酸母液合成氯乙酸甲酯合成条件的优化

以氯乙酸母液和甲醇为基本原料,固载磷钨酸为催化剂,通过连续酯化的方法制备了氯乙酸甲酯;以氯乙酸甲酯的质量收率为基准,采用三因素三水平正交实验的方法对酯合成的条件进行了优化。实验结果表明氯乙酸母液与甲醇质量比对反应的影响最大,其次是母液与催化剂的质量比,而回流时间对反应的影响较小。正交实验得到的适宜反应条件为:母液与甲醇的质量比为10/7,母液与催化剂的质量比为10/1,回流时间为1.5h;在此条件下氯乙酸甲酯的质量收率为46.9%。

Optimization of Synthesized Condition of Methyl Chloroacetate through Mother Liquor of Chloroacetic Acid with Immobilized phosphotungstic Acid as Catalyst

Methyl monochloroacetate was prepared through continuous esternization method with mother liquor of chloroacetic acid and methanol as raw material and immobilized phosphotungstic acid as catalyst. With the yield of methyl monochloroacetate as evaluating standard,the synthesized condition of methyl chloroacetate was optimized through orthogonal experiment. The experimental results indicated the mass quantity ratio of the mother liquor to methanol or to catalyst had great influence on the yield of methyl monochloroacetate. The optimum condition as follows:the of mass quantity ratio of the mother liquor to methanol and catalyst was 10/7 and 10/1 respectively,the reflux time was 1.0 h. The yield of methyl monochloroacetate was 46.9% under these condition.