Method for producing glycine by using organic solvent

A technology of organic solvent and glycine, applied in the field of clean production technology of glycine, can solve the problems of high energy consumption, limited output of by-product ammonium chloride, affecting the output of glycine single kettle and the like

Active Publication Date: 2019-06-04
北京长邦科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the output of the by-product ammonium chloride obtained each time is limited, which also affects the output of glycine single-pot production
In order to obtain as much by-product ammonium chloride as possible in single-pot production, the organic solvent needs to be refrigerated and cooled, which consumes a lot of energy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: compound 600 ml of organic solvent (wherein methanol 100 ml, ethylene glycol 300 ml, dimethylacetamide (DMAC) 200 ml) and 95 g of chloroacetic acid, 30 g of urotropine are loaded with stirrer, thermometer and In a four-neck flask cooled by a reflux condenser and a water bath, stir to dissolve, keep the temperature below 45°C, and feed 17g of liquid ammonia within one hour. Then continue to pass ammonia, the temperature is controlled between 50°C and 65°C, and pass 25g of ammonia within 1 hour until the pH value reaches 7.5 to stop the reaction. The crude glycine crystals were filtered out under the condition of cooling down to 40° C., washed with methanol, filtered and dried to obtain 70.72 g of glycine with a content of 98.16%.

[0018] To the filtered organic solvent for circulating reaction, add 95 g of chloroacetic acid in batches, lower the temperature to 20° C., and filter out the crude ammonium chloride and the organic solvent for circulating reacti...

Embodiment 2

[0019] Embodiment 2: Add the organic solvent containing chloroacetic acid obtained in Embodiment 1 into a four-necked flask for ammonia reaction. Keep the temperature below 45°C, and feed 17g of liquid ammonia within one hour. Then continue to pass ammonia, the temperature is controlled between 50°C and 65°C, and pass 26g of ammonia within 1 hour until the pH value reaches 7.3 to stop the reaction. The crude glycine crystals were filtered out under the condition of cooling down to 40° C., washed with methanol, filtered and dried to obtain 73.51 g of glycine with a content of 98.43%.

[0020] To the filtered organic solvent for circulating reaction, add 95 g of chloroacetic acid in batches, lower the temperature to 20° C., and filter out the crude ammonium chloride and the organic solvent for circulating reaction containing chloroacetic acid. The crude ammonium chloride was washed with methanol, filtered and dried to obtain 52.17 g of ammonium chloride.

Embodiment 3

[0021] Example 3: Compounding 600 ml of organic solvent (including 100 ml of methanol, 250 ml of ethylene glycol, 250 ml of dimethylacetamide (DMAC)) and 112 g of ammonium chloroacetate, 30 g of urotropine is equipped with a stirrer and a thermometer In a four-necked flask cooled by a reflux condenser and a water bath, stir and dissolve, the temperature is controlled between 50°C and 65°C, and 25g of ammonia is passed within 1 hour until the pH value reaches 7.3 to stop the reaction. The crude glycine crystals were filtered out under the condition of cooling down to 40° C., washed with methanol, filtered and dried to obtain 72.37 g of glycine with a content of 98.35%.

[0022] Add 112g of ammonium chloroacetate in batches to the filtered organic solvent for the circulating reaction, cool down to 20°C, filter the crude ammonium chloride and the organic solvent for the circulating reaction containing ammonium chloroacetate. The crude ammonium chloride was washed with methanol, f...

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Abstract

The invention relates to a method for producing glycine and co-producing ammonium chloride by using an organic solvent, wherein the organic solvent comprises: ethylene glycol, propylene glycol, dimethylacetamide (DMAC), and methanol and ethanol capable of being blended in the previous solvents. According to the present invention, a reaction organic solvent and a catalyst urotropine are added to areactor for producing glycine, chloroacetic acid is added, ammonia is introduced to synthesize glycine, and cooling, filtration, washing and drying are sequentially performed to obtain the glycine product; and chloroacetic acid or ammonium chloroacetate is added to the organic solvent, ammonium chloride is precipitated and crystallized, and washing and drying are performed to obtain the ammonium chloride product, wherein the organic solvent is recycled.

Description

technical field [0001] The invention relates to a clean production process of glycine, which uses an organic solvent to produce 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 traditional production process of glycine by aminolysis of chloroacetic acid in China is as follows: Add an aqueous solution with a content of about 25% of urotropine as a catalyst in a reaction kettle with cooling water, and at the same time add an aqueous solution of chloroacetic acid with a content of about 80% dropwise and pass in liquid ammonia , Ammonolysis reaction is carried out under the conditions of pH value of about 7 and reaction temperature of about 70-80°C. The ammonolysis reaction liquid containing glycine and ammonium chloride obtained after the reaction is separated...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/08C07C227/42C07C229/08C01C1/16
CPCY02A40/20
Inventor 刘长飞王云鹤李可
Owner 北京长邦科技有限公司
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