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Clean production process of glycine in coproduction with ammonium chloride

A clean production and glycine technology, applied in the field of clean production technology of glycine, can solve the problems of complex process and difficult control of reaction end point, etc.

Inactive Publication Date: 2014-02-12
刘长飞
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the process is more complicated, and the reaction end point is also more difficult to control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put 58.3g of ammonium chloroacetate, 250ml of methanol, and 15g of urotropine into a four-neck flask equipped with a stirrer, a thermometer and a reflux condenser, stir and dissolve, raise the temperature to 65°C and start adding 50.5g of triethylamine dropwise, maintaining the temperature 60°C--65°C, the addition is completed in one and a half hours, keep the reaction for two and a half hours until the pH value is 7.0-7.5, cool down to 45°C, and filter to obtain glycine crystals. After the glycine crystals were washed with methanol (100 ml of methanol), filtered and dried, 37.81 g of glycine crystals with a content of 98.01% were obtained, and the yield of glycine was 94.2% based on ammonium chloroacetate. The reaction liquid from which glycine was filtered was cooled and frozen to -20°C, and 25.90 g of triethylamine hydrochloride solid was filtered out, and the filtered mother liquid was recycled for use in the next reaction.

Embodiment 2

[0026] Continue to use the mother liquor recovered in Example 1, dissolve 58.45g of ammonium chloroacetate, add 2g of urotropine, raise the temperature to 65°C and start adding 50.53g of triethylamine dropwise, maintain the temperature at 60°C--65°C for one and a half hours After the addition, keep the reaction for two and a half hours until the pH value is 7.0-7.5, cool down to 45°C, and filter to obtain glycine crystals. After the glycine crystals were washed with methanol and dried by filtration, 38.51 g of glycine crystals with a content of 97.8% were obtained, and the yield of glycine was 95.6% calculated by ammonium chloroacetate. The reaction liquid from which glycine was filtered was cooled and frozen to -20°C, and 59.21 g of triethylamine hydrochloride solid was filtered out, and the filtered mother liquor was recycled for use in the next reaction.

Embodiment 3

[0028] Continue to use the mother liquor recovered in Example 2, dissolve 58.51g of ammonium chloroacetate, add 2g of urotropine, raise the temperature to 65°C and start adding 50.52g of triethylamine dropwise, maintain the temperature at 60°C--65°C for one and a half hours After the addition, keep the reaction for two and a half hours until the pH value is 7.0-7.5, cool down to 45°C, and filter to obtain glycine crystals. After the glycine crystals were washed with methanol and dried by filtration, 38.56 g of glycine crystals with a content of 97.36% were obtained, and the yield of glycine was 95.29% calculated by ammonium chloroacetate. The reaction liquid from which glycine was filtered was cooled and frozen to -20°C, and 67.58 g of triethylamine hydrochloride solid was filtered out, and the filtered mother liquor was recycled for use in the next reaction.

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PUM

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Abstract

The invention provides a clean production process of glycine in coproduction with ammonium chloride, which has the capability of co-producing an ammonium chloride product while producing glycine, and also has the capability of co-producing a triethylamine hydrochloride product while producing the glycine. The clean production process comprises the following steps: after a solvent methanol and a catalyst are added into a reactor for a glycine ammonolysis reaction, adding solid ammonium chloroacetate, starting adding triethylamine when the temperature is increased to 65 DEG C, completely adding the triethylamine within one and a half hours, preserving the heat for reacting to two and a half hours until pH value is 7.5; and respectively cooling and carrying out freeze separation to obtain the glycine and the triethylamine hydrochloride. Triethylamine in the triethylamine hydrochloride is recycled by utilizing an ammonium introducing method, and meanwhile, the ammonium chloride product is co-produced.

Description

Technical field: [0001] The invention relates to a clean production process of glycine, which can co-produce ammonium chloride and triethylamine hydrochloride while producing glycine, and belongs to the technical field of chemical production. Background technique: [0002] Glycine is an important raw material for products such as glyphosate and glycine ethyl ester hydrochloride, and it can also be refined into food-grade glycine for use. The domestic traditional chloroacetic acid method glycine production process is as follows: in the reaction kettle with cooling water, add the aqueous solution of catalyst urotropine content about 25%, and drop the chloroacetic acid aqueous solution of about 70% content at the same time and pass into liquid ammonia, The ammonolysis reaction is carried out at a pH value of about 7 and a reaction temperature of about 80°C. The ammonolysis reaction liquid containing glycine and ammonium chloride obtained after the reaction is separated by meth...

Claims

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Application Information

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IPC IPC(8): C07C229/08C07C227/08C07C211/05C07C209/68C07C209/84C01C1/16
Inventor 刘长飞李志伟王云鹤李可
Owner 刘长飞
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