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Method for producing glycine through organic solvent

A technology of organic solvent and glycine, applied in the field of clean production technology of glycine, can solve the problems of large energy, complex process, difficult control of reaction end point and so on

Inactive Publication Date: 2015-04-01
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
When using ammonia to recover triethylamine hydrochloride, triethylamine cannot be recovered completely, and at the same time, a small amount of mixed crystals of glycine and ammonium chloride are produced during the production process, and further separation is required
Patent CN1176062C introduces a method for producing glycine by the alcohol phase method. Although the catalyst can be recycled, the mixed crystal solid of glycine and ammonium chloride obtained by the reaction has no good separation method, and only electrodialysis or alcohol can be used. separation by means of analysis consumes a large amount of energy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Put 473g of chloroacetic acid, 1600ml of ethylene glycol, and 100g of urotropine into a four-neck flask equipped with a stirrer, a thermometer, a reflux condenser and a water bath to cool down, stir and dissolve, keep the temperature below 45°C, and feed it within one hour Liquid ammonia 85g. Then continue to pass ammonia, the temperature is controlled between 60°C--70°C, and 90g of ammonia is passed within 2 hours. Insulate and react for 1 hour. The crude glycine crystals were filtered out at 60°C, washed with methanol, filtered and dried to obtain 319.7g of glycine with a content of 98.7%. The filtered circulating mother liquor was frozen and cooled to 0° C., filtered out ammonium chloride mixed crystals, washed with methanol and filtered to obtain 217.7 g of ammonium chloride mixed crystals. Add 100ml of water to the ammonium chloride mixed crystal to wash, filter and dry to obtain 151.2g of ammonium chloride with a content of 98.1%.

Embodiment 2

[0029] Put 473g of chloroacetic acid, 1600ml of ethylene glycol, 400ml of methanol, and 120g of urotropine into a four-neck flask equipped with a stirrer, a thermometer, a reflux condenser and a water bath to cool down, stir and dissolve, and keep the temperature below 45°C for one hour Pass into liquid ammonia 85g. Then continue to pass ammonia, the temperature is controlled between 60°C--70°C, and 90g of ammonia is passed within 2 hours. Insulate and react for 1 hour. The crude glycine crystals were filtered out at 60°C, washed with methanol, filtered and dried to obtain 321.6g of glycine with a content of 99.1%. The filtered circulating mother liquor was frozen and cooled to 0° C., filtered out ammonium chloride mixed crystals, washed with methanol and filtered to obtain 208.1 g of ammonium chloride mixed crystals. Add 100ml of water to the ammonium chloride mixed crystal to wash, filter and dry to obtain 144.3g of ammonium chloride with a content of 98.5%.

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Abstract

The invention provides a cleaning production technology of glycine. The glycine is produced through glycols solvents (ethylene glycol, propylene glycol and butyl glycol) or diol derivative solvents (ethylene glycol monomethyl ether, ethylene glycol monoethyl ether and ethylene glycol monobutyl ether) and methanol (or ethanol) organic solvents. After the organic solvents and catalyst methenamine are added in a reactor for producing the glycine, chloroacetic acid is added, then, nitrogen is slowly fed in, and a reaction for synthesizing the glycine is performed. After the reaction ends, glycine crystals are filtered out at the temperature ranging from 50 DEG C to 75 DEG C, and glycine products are obtained after methanol (or ethanol) washing, filtering and drying. After filtering liquid is cooled, ammonium chloride and mixed crystal solids including a small amount of glycine are obtained through filtration, and ammonium chloride products are obtained through washing. The reaction solvents are cyclically used.

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 domestic production process of chloroacetic acid aminolysis method for glycine is as follows: in the reaction kettle with cooling water, add an aqueous solution with a catalyst hexatropine content of about 25%, and at the same time add a chloroacetic acid aqueous solution with a content of about 80% dropwise and pass in liquid ammonia , carry out the ammonolysis reaction 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 methanol alcohol a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/08C07C227/08C01C1/16
Inventor 刘长飞王云鹤李志伟刘丽翠李可
Owner 刘长飞
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