Novel process for preparation of glycine by using chloroacetic acid aqueous phase ammoniation method
A technology of glycine and chloroacetic acid, which is applied in the preparation of cyanide reaction, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of difficult methanol mother liquor treatment, large centrifuge processing capacity, high production cost, etc., and reduce dissolution loss , reduce the processing volume and processing difficulty, and improve the yield
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Embodiment 1
[0043] A new process for preparing glycine by chloroacetic acid aqueous phase ammonification method comprises the following steps:
[0044] A. Amination reaction
[0045] 183g (0.35 parts by mass) of urotropine solution with a mass concentration of 25%, and 523g (1 part by mass) of chloroacetic acid solution with a mass concentration of 82% were successively put into a 2L reaction bottle, and the pH value of the reaction solution was 6.8; Ammonia reaction was carried out with ammonia gas; the reaction temperature was controlled at 70°C~90°C, and the ammonia reaction reached the end of the reaction for 100 minutes, and the ammonia flow was stopped to complete the reaction; then the ammoniation reaction liquid was cooled to 25°C and filtered to obtain 413.6g of crude glycine , ammoniated mother liquor 559g.
[0046] The content of the glycine crude product is 60%, enter step B for purification.
[0047] Add 1120g (2 parts by mass) of methanol with a mass concentration of 92% t...
Embodiment 2
[0060] A new process for preparing glycine by chloroacetic acid aqueous phase ammonification method comprises the following steps:
[0061] A. Amination reaction
[0062] 185g (0.35 parts by mass) of urotropine solution with a mass concentration of 25%, and 528g (1 part by mass) of chloroacetic acid solution with a mass concentration of 81.8% were successively put into a 2L reaction bottle, and the pH value of the reaction solution was 7.1; Ammonia reaction was carried out with ammonia gas; the reaction temperature was controlled at 70°C to 90°C, and the ammonia reaction was carried out for 100 minutes to reach the end of the reaction, the ammonia flow was stopped, and the reaction ended; then the ammoniation reaction solution was cooled to 26°C and filtered to obtain 412g of crude glycine, Ammonia mother liquor 569g.
[0063] The content of the glycine crude product is 61%, enter step B for purification.
[0064] Add 1140g (2 parts by mass) of methanol with a mass concentra...
Embodiment 3
[0077] A new process for preparing glycine by chloroacetic acid aqueous phase ammonification method comprises the following steps:
[0078] A. Amination reaction
[0079] 165g (0.35 parts by mass) of urotropine solution with a mass concentration of 25%, and 472.6g (1 part by mass) of chloroacetic acid solution with a mass concentration of 81.8% were dropped into a 2L reaction flask in turn, and the pH value of the reaction solution was 7.5; Enter ammonia gas for ammoniation reaction; the reaction temperature is controlled at 80°C to 90°C, and the ammonia reaction reaches the end point of the reaction for 100 minutes, the ammonia flow is stopped, and the reaction ends; then the ammoniation reaction solution is cooled to 25°C and filtered to obtain crude glycine 368.2 g, ammoniated mother liquor 505g.
[0080]The content of the glycine crude product is 62%, enter step B for purification.
[0081] Add 1010g (2 parts by mass) of methanol with a mass concentration of 92% to 505g ...
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