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Continuous glycine synthesis method

A synthesis method, glycine technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as quality not up to product standards, high consumption, difficult ammonium chloride treatment, etc., and achieve environmental protection in production Problems, the effect of unit consumption reduction

Active Publication Date: 2020-05-22
TIANJIN TIANDI CHUANGZHI TECH DEV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) High catalyst consumption
The catalyst urotropine is a one-time use, it will not be recycled after being added, and will eventually enter the waste water and products, which not only leads to excessive consumption, but also causes subsequent environmental protection problems
[0005] (2) Environmental issues
There are three aspects of environmental protection problems: ① "red water" is difficult to deal with
② It is difficult to deal with "yellow" ammonium chloride, because glycine, urotropine, reaction by-products and impurities are all in the ammonium chloride mother liquor, resulting in 60~70% ammonium chloride obtained by concentration can meet the product standard, and the remaining 30~40% of the ammonium chloride is yellow and sticky, the quality is not up to the product standard and needs to be reprocessed
Formaldehyde-containing wastewater treatment problems

Method used

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  • Continuous glycine synthesis method
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Such as Figure 2-3 Shown is the production process diagram and product diagram of glycine of the present invention. (1) Dissolve chloroacetic acid in the mixed crystal mother liquor (in the beginning of production, replace the mixed crystal mother liquor with water) to make a chloroacetic acid solution with a mass concentration of 50%.

[0037] (2) Dissolve liquid ammonia in mixed crystal mother liquor to prepare ammonia water with a mass concentration of 15%, and the temperature of the ammonia water is not higher than 30°C.

[0038] (3) Chloroacetic acid solution and a part of ammonia water undergo a salt-forming reaction in the salt-forming reactor. In the salt-forming reaction, the molar ratio of chloroacetic acid to ammonia is 1.0 to obtain solution A; the reaction temperature is controlled at 30°C, and the reaction pH is controlled at 5.0.

[0039] (4) Dissolve a certain amount of urotropine solution in the remaining ammonia water, so that the total mass concentr...

Embodiment 2

[0043] (1) Dissolve chloroacetic acid in the mixed crystal mother liquor (in the beginning of production, replace the mixed crystal mother liquor with water) to make a chloroacetic acid solution with a mass concentration of 65%.

[0044](2) Dissolve liquid ammonia in the mixed crystal mother liquor to prepare ammonia water with a mass concentration of 25%; the temperature of the ammonia water is not higher than that of 30°C.

[0045] (3) Chloroacetic acid solution and a part of ammonia water undergo a salt-forming reaction in the salt-forming reactor. In the salt-forming reaction, the molar ratio of chloroacetic acid to ammonia is 2 to obtain solution A. The reaction temperature is controlled at 45°C and the reaction pH is controlled at 7.0.

[0046] (4) Dissolve a certain amount of urotropine solution in the remaining ammonia water, so that the total mass concentration of urotropine is 23%; the molar ratio of urotropine to ammonia is 0.3.

[0047] (5) The ammonia water contai...

Embodiment 3

[0050] (1) Dissolve chloroacetic acid in the mixed crystal mother liquor (in the beginning of production, replace the mixed crystal mother liquor with water) to make a chloroacetic acid solution with a mass concentration of 55%.

[0051] (2) Dissolve liquid ammonia in mixed crystal mother liquor to prepare ammonia water with a mass concentration of 20%, and the temperature of the ammonia water is not higher than 30°C.

[0052] (3) Chloroacetic acid solution and a part of ammonia water undergo a salt-forming reaction in the salt-forming reactor. In the salt-forming reaction, the molar ratio of chloroacetic acid to ammonia is 0.8 to obtain solution A. The reaction temperature is controlled at 40°C and the reaction pH is controlled at 6.0.

[0053] (4) Dissolve a certain amount of urotropine solution in the remaining ammonia water, so that the total mass concentration of urotropine is 20%; the molar ratio of urotropine to ammonia is 0.1.

[0054] (5) The ammonia water containing ...

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Abstract

The invention relates to a continuous glycine synthesis method. The method comprises the following steps: preparing ammonia water; then mixing a chloroacetic acid solution with the ammonia water for asalifying reaction to obtain a solution A; dividing a mixed solution containing urotropin and ammonia water into a plurality of parts, separately adding the plurality of parts of the mixed solution into the solution A, carrying out an ammoniation reaction, and then performing cooling, crystallizing, and separating to obtain a mixed crystal of glycine and ammonium chloride and a mixed crystal mother liquor; taking the mixed crystal mother liquor as a solvent for preparing the ammonia water used in the step (1) or the chloroacetic acid solution used in the step (2); and continuing the reactionto realize continuous synthesis of glycine. According to the invention, a conventional one-step method is divided into three parts, i.e., ammonia dissolution, a salifying reaction and the ammoniationreaction, so a required amount of the ammonia water can be uniformly mixed with feed liquid, the problem of generation of many byproducts caused by local overheating due to ammonia absorption or a toohigh pH value of local feed liquid is avoided, the defects of conventional processes are effectively avoided, glycine yield is increased, and urotropine consumption is reduced.

Description

technical field [0001] The invention belongs to the technical field of glycine production, and in particular relates to a continuous glycine synthesis method. Background technique [0002] Such as figure 1 As shown, at present, the chloroacetic acid route adopts a batch method process, and the reactor adopts a batch stirring tank. After the catalyst hexamethamine is made into an aqueous solution, it is first added to the reactor, and then the chloroacetic acid solution and ammonia gas are respectively fed into the reactor at a certain flow rate. The ammonification reaction occurs in the kettle, and then a large amount of methanol is added to the feed liquid (synthesis liquid) for alcohol analysis, and then the crude product of glycine (containing glycine, a small amount of ammonium chloride and urotropine) and the mother liquor of glycine are obtained by centrifugation. The glycine crude product is washed, centrifuged and dried to obtain the glycine product; the glycine mot...

Claims

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Application Information

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IPC IPC(8): C07C227/08C07C227/40C07C227/42C07C229/08
CPCC07C227/08C07C227/40C07C227/42C07C229/08Y02P20/584
Inventor 张敏卿胡辉黄鑫刘秉言温洪鹏郑鑫黃邵峰
Owner TIANJIN TIANDI CHUANGZHI TECH DEV
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