Method for producing glycine by mixed solvent method

A technology of mixed solvent and glycine, applied in the field of clean production technology of glycine, can solve the problems of no separation method, large energy, complicated process, etc.

Inactive Publication Date: 2016-08-17
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

[0022] Put 473g of chloroacetic acid, 1900ml of methanol, 50ml of ethylene glycol, and 125g of urotropine into a four-necked 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 50°C. 85 g of liquid ammonia was introduced within one hour. Then continue to pass ammonia, the temperature is controlled between 60°C and 70°C, and 100 g of ammonia is passed within 1 hour. Heat preservation reaction for 0.5 hours. Glycine and ammonium chloride mixed crystalline solids were filtered out at 60°C. The mixed crystalline solids were washed with 100 ml of methanol, filtered with suction, and the washing solution was added to the filtered reaction mother liquor. After weighing, 749.64g of glycine and ammonium chloride mixed crystal solid was obtained, with a moisture content of 25.35%.

Embodiment 2

[0024] Add 473 g of chloroacetic acid to the mother liquor filtered out in Example 1, stir and dissolve, keep the temperature below 50° C., and feed 85 g of liquid ammonia within one hour. Then continue to pass ammonia, the temperature is controlled between 60°C and 70°C, and 100g of ammonia is passed within 1 hour. Heat preservation reaction for 0.5 hours. Glycine and ammonium chloride mixed crystalline solids were filtered out at 60°C. The mixed crystalline solids were washed with 100ml of methanol, filtered with suction, and the washing solution was added to the filtered reaction mother liquor. After weighing, 816.24 g of glycine and ammonium chloride mixed crystal solid were obtained, with a moisture content of 25.79%.

Embodiment 3

[0026] Take 140 g of the wet glycine and ammonium chloride mixed crystal solid in Example 1, add it to a mixed solvent consisting of 800 ml ethylene glycol and 300 ml methanol, stir, heat to 65° C., and filter out the glycine crystals. Glycine crystals were washed with 100ml of methanol, suction filtered and dried to obtain 39.13 g of crude glycine. After analysis, the glycine content is 97.13%. Filter out the mixed solvent of glycine, cool down to 10°C, and filter out solid ammonium chloride. The solid ammonium chloride was washed with 100ml of methanol, and suction-filtered to obtain 16.12g of crude ammonium chloride.

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PUM

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Abstract

The invention provides a clean production process of glycine. An organic mixed solvent is used for producing glycine and a by-product ammonium chloride by combined production. The organic mixed solvent comprises methanol, ethanol, and dihydric alcohol solvents or dihydric alcohol derivative solvents. The mixed solvent is added into a glycine synthesis reactor, urotropine and chloroacetic acid are added, ammonia is added, and a mixed crystal solid of glycine and ammonium chloride is obtained. The mixed crystal solid is added into a mixed solvent for separation, the mixed solvent for separation is heated to 60-80 DEG C, after glycine crystal is filtered, the mixed solvent for separation is cooled to 0-20 DEG C, and an ammonium chloride solid is separated by centrifugation.

Description

Technical field [0001] The present invention involves a cleaning production technology of a glycine, and the use of organic hybrid solvents to produce glycine is a chemical production technology field. Background technique [0002] Glycine is an important raw material for products such as glycut, glycopine ethyl hydrochloride, and can also be refined into food -grade glycine.The traditional domestic chlorohydrin amin amino acid production process is as follows: Add a catalyst olotine with a catalyst with a catalyst of about 25%of the water solution of about 25%of the catalyst.Active reaction is performed under the conditions of about 7 at a pH value of about 7 and the reaction temperature of about 80 ° C.After the reaction is over, the ammonia resolution reaction liquid containing glycine and ammonium chloride is separated by methanol alcohol to obtain glycine products.To produce a ton of glycine, it is generated to produce a methanol-containing parent liquid with a methanol of a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/08C07C227/08C07C227/40C01C1/16
Inventor 刘长飞
Owner 刘长飞
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