Setup of glycine continuous synthesis by ammonolysis of monochloroacetic acid

Catherine Couriol, Henri Fauduet, Catherine Porte, Alain Delacroix
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引用次数: 8

Abstract

This article describes the continuous production of glycine by catalytic ammonolysis of monochloroacetic acid in an aqueous medium. The synthesis and crystallization of glycine are carried out in a battery of three stirred double-jacketed reactors while temperature and pH values are controlled. The results of the kinetic study allow one to calculate the residence time in each tank for a desired conversion ratio and are first checked with the setup. Then, some parameters (concentration of reagents, regulation of pH, residence time, catalyst) are modified to improve the final yield in crystallized glycine. The best yield resulting from a flow process (96.6%) is better than that resulting from a batch process (93%) and is obtained in the following conditions: the first step is performed at 75°C and pH 5.4 with a 10 mol L−1 monochloroacetic acid solution and a 17 mol L−1 ammonia aqueous one with a 0.2 molar ratio of hexamethylenetetramine; the second step is carried out at 75°C and pH 8.0; the optimal residence times are respectively 1 and 4 hours. Replacement of hexamethylenetetramine by formaldehyde can also be considered even if the yield is slightly lower. © 1999 John Wiley & Sons, Inc. Lab Robotics and Automation 11: 29–35, 1999

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一氯乙酸氨解法连续合成甘氨酸的研究
介绍了一氯乙酸在水介质中催化氨解连续生产甘氨酸的方法。在控制温度和pH值的条件下,甘氨酸的合成和结晶在一个由三个搅拌双夹套反应器组成的电池中进行。动力学研究的结果允许人们计算所需转化率在每个水箱中的停留时间,并首先与设置进行检查。然后,通过对试剂浓度、pH调节、停留时间、催化剂等参数的修改,提高了甘氨酸结晶的最终收率。在75℃、pH 5.4条件下,以10 mol L−1的一氯乙酸溶液和17 mol L−1的氨水溶液为原料,以0.2摩尔比的六亚甲基四胺为原料,得到最佳收率(96.6%),优于间歇法(93%);第二步在75℃和pH 8.0下进行;最佳停留时间分别为1小时和4小时。即使收率略低,也可以考虑用甲醛代替六亚甲基四胺。©1999 John Wiley &儿子,Inc。实验室机器人与自动化(11):29-35,1999
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