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Clean production technology for co-production of glycine and calcium chloride

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

Active Publication Date: 2013-12-18
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

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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Put 55.75g of ammonium chloroacetate, 120g of methanol, and 10g of urotropine into a four-necked flask equipped with a stirrer, thermometer and reflux condenser, stir to dissolve, heat up to 65°C and start adding 50.5g of triethylamine dropwise to maintain the temperature 60°C-65°C, complete the addition in one and a half hours, keep the reaction for two and a half hours until the pH value is 7.0-7.5, lower the temperature to 45°C, and filter to obtain glycine crystals. After the glycine crystals were washed with methanol, filtered and dried, 36.7 g of glycine crystals with a content of 97.5% were obtained. The yield of glycine was 95.3% based on ammonium chloroacetate. The reaction solution from which glycine was filtered out was cooled and frozen to -10°C, and 39 g of triethylamine hydrochloride solid was filtered out, and the filtered mother liquor was recycled for use in the next reaction.

Embodiment 2

[0025] Continue to use the mother liquor recovered in Example 1, dissolve 55.75g of ammonium chloroacetate, start to add 50.5g of triethylamine dropwise when the temperature is raised to 65°C, maintain the temperature at 60°C-65°C, complete the addition in one and a half hours, keep the temperature for two and a half hours After hours, the pH value is 7.0-7.5, the temperature is lowered to 45°C, and glycine crystals are obtained by filtration. After the glycine crystals were washed with methanol, filtered and dried, 37.1 g of glycine crystals with a content of 98.1% were obtained, and the glycine yield was 97.1% based on ammonium chloroacetate. The reaction solution from which glycine is filtered out is cooled and frozen to -10°C, and 68.2 g of triethylamine hydrochloride solid is filtered out, and the filtered mother liquor is recycled for use in the next reaction.

Embodiment 3

[0027] Continue to use the mother liquor recovered in Example 2, dissolve 55.75g of ammonium chloroacetate, start adding 50.5g of triethylamine dropwise when the temperature is raised to 65°C, maintain the temperature at 60°C-65°C, complete the addition in one and a half hours, keep the temperature for two and a half hours After hours, the pH value is 7.0-7.5, the temperature is lowered to 45°C, and glycine crystals are obtained by filtration. After the glycine crystals were washed with methanol and filtered and dried, 36.1 g of glycine crystals with a content of 98.3% were obtained. The glycine yield was calculated as 94.6% based on ammonium chloroacetate. The reaction solution from which glycine was filtered out was cooled and frozen to -10°C, and 68.5 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 technology for co-production of glycine and calcium chloride. Calcium chloride byproducts or sodium chloride byproducts can be co-produced while glycine is produced. The clean production technology comprises the following steps of: adding solvent methyl alcohol and a catalyst to a reactor in which glycine ammonolysis reaction is carried out, then adding solid ammonium chloroacetate, heating to 65 DEG C, adding triethylamine, completing the addition of triethylamine within 1.5 hours, carrying out heat preservation reaction for 2.5 hours till the pH value is 7.0-7.5; respectively cooling, freezing, and separating out glycine and triethylamine hydrochloride; recycling triethylamine in triethylamine hydrochloride by using calcium hydroxide, calcium oxide or sodium hydroxide, wherein triethylamine serves as an acid-binding agent to participate in glycine ammonolysis reaction.

Description

Technical field: [0001] The invention relates to a clean production process of glycine, which can co-produce calcium chloride by-product or sodium chloride by-product 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 can also be refined into food-grade glycine for use. The traditional domestic production process of glycine by chloroacetic acid method is as follows: Add an aqueous solution with a catalyst urotropine content of about 25% in a reactor filled with cooling water, and at the same time add dropwise an aqueous solution of chloroacetic acid with a content of about 70% and pass in liquid ammonia. The ammonolysis reaction is carried out at a pH of about 7 and a reaction temperature of about 80°C. The ammonolysis reaction solution containing glycine and ammonium chloride obtained after the reaction i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/08C07C227/08C01F11/28C01D3/04
Inventor 刘长飞阎森林李志伟王云鹤李丽
Owner 北京长邦科技有限公司