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 difficult control of reaction end point, complicated process, inability to fully recover triethylamine and the like

Inactive Publication Date: 2017-05-24
QINGDAO SENMEIKE CHEM TECH CO LTD
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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

[0023] 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

[0025] 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 relates to a method for producing glycine by using an organic solvent, and provides a clean production technology of the glycine. According to the method, the glycine is prepared by using a glycols solvent (such as ethylene glycol, propylene glycol or butanediol), or a glycol derivative solvent (such as ethylene glycol monomethyl ether, ethylene glycol monoethyl ether or ethylene glycol monobutyl ether) and a methyl alcohol (or ethyl alcohol) organic solvent. The method comprises the steps of adding the organic solvent and a catalyst-urotropine into a reactor used for producing the glycine, then adding chloroacetic acid into the reactor, slowly replenishing the reactor with ammonia, and carrying out a reaction for synthesizing the glycine; after the reaction is finished, filtering out glycine crystals at the temperature of 50-75 DEG C, washing the glycine crystals with methyl alcohol (or ethyl alcohol), filtering, and drying to obtain a glycine product; cooling filtrate by freezing, then filtering to obtain mixed crystal solid of ammonium chloride and a small amount of glycine, and washing to obtain an ammonium chloride product, wherein the reaction solvents can be reused.

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 ana...

Claims

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Application Information

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IPC IPC(8): C07C227/08C07C229/08C01C1/16
Inventor 李春梅
Owner QINGDAO SENMEIKE CHEM TECH CO LTD
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