Process for synthesizing glyphosate by alkyl ester method

A technology of glyphosate and alkyl ester, which is applied in the field of glyphosate production by the alkyl ester method, can solve the problems of increasing the amount of mother liquor, hydrochloric acid and alkyl ester, etc., so as to reduce the amount of mother liquor, shorten the time, reduce The effect of steam elimination

Pending Publication Date: 2021-12-24
HUBEI TAISHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method will increase the amount of hydrochloric acid and alkyl esters, and glyphosate crystals are not easy to wash and need to increase washing water, which will eventually cause an increase in the amount of mother liquor

Method used

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  • Process for synthesizing glyphosate by alkyl ester method
  • Process for synthesizing glyphosate by alkyl ester method
  • Process for synthesizing glyphosate by alkyl ester method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A synthetic method of glyphosate, comprising the steps of:

[0040] (1) Add 117ml of anhydrous methanol, 49g of paraformaldehyde, and 7.2g of caustic soda to a 1000ml four-neck flask, raise the temperature to 50°C and start the holding time. The holding temperature is 58-60°C. After holding for 20 minutes, add 225ml of methanol.

[0041] (2) After cooling down to below 35°C, add 62g of glycine (98.5% content) and 70g of triethylamine, and keep warm at below 40°C for 30min.

[0042] (3) Add 109g of dimethyl phosphite, start timing after heating up to 50°C, add 8g of triethylamine after 10 minutes of heat preservation, and the total heat preservation time is 70 minutes.

[0043] (4) After cooling down to 40°C, add 343g of 30% hydrochloric acid and keep the temperature below 40°C.

[0044] (5) Raise the temperature of the above hydrolyzate to 85°C and control it at 2.0-3.5h, 85-102°C at about 1.5h, at 102°C until the material turns yellow and control it at 1-1.5h, and con...

Embodiment 2

[0047] A synthetic method of glyphosate, comprising the steps of:

[0048] (1) Add 117ml of anhydrous methanol, 49g of paraformaldehyde, and 7.2g of caustic soda to a 1000ml four-neck flask, raise the temperature to 50°C and start the holding time. The holding temperature is 58-60°C. After holding for 20 minutes, add 225ml of methanol.

[0049] (2) After cooling down to below 35°C, add 80g of sodium glycinate (content 99%), add 10g of triethylamine, and keep warm at below 40°C for 30min.

[0050] (3) Add 109g of dimethyl phosphite, start timing after the temperature rises to 50°C, and the total holding time is 70min.

[0051] (4) After cooling down to 40°C, add 254g of 30% hydrochloric acid and keep the temperature below 40°C.

[0052] (5) Raise the temperature of the above hydrolyzate to 85°C and control it at 2.0-3.5h, 85-102°C at about 1.5h, at 102°C until the material turns yellow and control it at 1-1.5h, and control the end point temperature at 117°C. After the solutio...

Embodiment 3

[0055] A synthetic method of glyphosate, comprising the steps of:

[0056] (1) Add 117ml of anhydrous methanol, 49g of paraformaldehyde, and 7.2g of caustic soda to a 1000ml four-neck flask, raise the temperature to 50°C and start the holding time. The holding temperature is 58-60°C. After holding for 20 minutes, add 225ml of methanol.

[0057] (2) Add 80g of sodium glycinate (content 99%) after cooling down to below 35°C, and keep warm for 30min below 40°C.

[0058] (3) Add 100g of dimethyl phosphite, start timing when the temperature rises to 50°C, and the total holding time is 70min.

[0059] (4) After cooling down to 40°C, add 248g of 30% hydrochloric acid and keep the temperature below 40°C.

[0060] (5) Raise the temperature of the above hydrolyzate to 85°C and control it at 2.0-3.5h, 85-102°C at about 1.5h, at 102°C until the material turns yellow and control it at 1-1.5h, and control the end point temperature at 117°C. After the solution turns yellow, keep it warm fo...

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Abstract

The invention relates to a process for synthesizing glyphosate by an alkyl ester method, the method comprises the following steps: heating or alkalifying a methanol solution of paraformaldehyde or formaldehyde to depolymerize, adding glycinate, uniformly stirring to carry out addition reaction, adding no or less triethylamine, adding dimethyl phosphite and a small amount of triethylamine to carry out condensation reaction after the addition reaction, and hydrolyzing with hydrochloric acid, adding alkali to crystallize, washing and drying to obtain the glyphosate. Glycine salt is used for replacing glycine, the glyphosate crystallization yield is not affected, the addition reaction efficiency is higher, the temperature is low, the time is short, the process has the characteristics of being simple to operate, energy-saving, environment-friendly and high in selectivity, the production cost of glyphosate synthesis can be greatly reduced (for example, the use amount of hydrochloric acid, liquid caustic soda and steam is greatly reduced), mother liquor treatment is simple, and the process has the advantages of reaction, cost and environmental protection.

Description

technical field [0001] The invention belongs to the technical field of glyphosate production by alkyl ester method, in particular to a process method for synthesizing glyphosate by using glycinate and alkyl ester as raw materials. Background technique [0002] Glyphosate is a high-efficiency, broad-spectrum, low-toxic and safe herbicide. There are mainly two methods for its industrial production. One is the production method using iminodiacetic acid (IDA) as a raw material, and the other is using glycine, A production method in which alkyl phosphite is used as a raw material. Since the Shenyang Research Institute of Chemical Industry opened up the glycine and alkyl phosphite method to produce glyphosate in 1987, about 80% of the current domestic glyphosate production capacity is produced by the glycine-alkyl phosphite method. After 30 years of development of this method, although glyphosate enterprises have continuously optimized the process, the yield of glyphosate has inc...

Claims

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Application Information

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IPC IPC(8): C07F9/38
CPCC07F9/3813
Inventor 姚红田义群彭春雪
Owner HUBEI TAISHENG CHEM
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