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Hydrosis process improvement method for synthesizing glyphosate by alkyl ester process

A glyphosate and process technology, applied in the field of glyphosate hydrolysis process for the synthesis of glyphosate by the alkyl ester method, can solve the problems of increasing the cost of glyphosate wastewater treatment, increasing the amount of washing water, and affecting the quality of glyphosate formulation products, etc.

Inactive Publication Date: 2013-12-04
UNIV OF SHANGHAI FOR SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] But the disadvantages of this process are: (1) NaOH is added to adjust the pH value of the material in this process to improve the solid recovery rate of glyphosate, which will introduce a large amount of Na+ in the glyphosate original drug, glyphosate High Na+ content in the original drug will affect the product quality of glyphosate formulations, especially the preparation of high-content glyphosate liquid formulations is prone to crystallization in winter
(2) In order to control the Na+ content in the glyphosate technical, it is necessary to increase the difficulty of the washing process of the technical, especially the increase in the amount of washing water, thereby increasing the discharge of glyphosate mother liquor wastewater and increasing the treatment of glyphosate wastewater cost

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0024] Weigh 24.2g of paraformaldehyde, 136.2g of methanol and 40.8g of triethylamine, add them to a four-necked flask and stir for 30 minutes at a temperature of 40-45°C; after the materials in the reactor become clear, add 30g of glycine and keep the same Stir the temperature for 40 minutes. After the material in the flask becomes clear, add 54g of dimethyl phosphite and raise the temperature to 50-60°C; after keeping the temperature for 50 minutes, the temperature is lowered to 30°C. Under stirring, add the mass fraction of 30% hydrochloric acid 135ml; after stirring for 30 minutes, slowly warm the flask to 75-90°C and distill out methanol; when the methanol has evaporated completely, heat the flask to 115-125°C through a temperature regulator; then add 20g water to cool the flask When the temperature is below 70℃, use cold water to cool the inside of the flask to continue to cool down to below 10℃; slowly add 15g of triethylamine, the temperature is controlled at 15-25℃; the...

Embodiment 2

[0029] Weigh 24.2g of paraformaldehyde, 136.2g of methanol and 40.8g of triethylamine, add them to a four-necked flask and stir for 30 minutes at a temperature of 40-45°C; after the materials in the reactor become clear, add 30g of glycine and keep the same Stir the temperature for 40 minutes. After the material in the flask becomes clear, add 54g of dimethyl phosphite and raise the temperature to 50-60°C; after keeping the temperature for 50 minutes, the temperature is lowered to 30°C. Under stirring, add the mass fraction of 30% hydrochloric acid 135ml; after stirring for 30 minutes, slowly warm the flask to 75-90°C and distill out methanol; when the methanol has evaporated completely, heat the flask to 115-125°C through a temperature regulator; then add 20g water to cool the flask When the temperature is below 70℃, use cold water to cool the inside of the flask to keep the temperature below 10℃; slowly add 23g of triethylamine, the temperature is controlled at 15-25℃, and the...

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Abstract

The invention relates to a hydrosis process improvement method for synthesizing glyphosate by an alkyl ester process. The method comprises the following steps: at the temperature of 40-50 DEG C, feeding paraformaldehyde, methyl alcohol and triethylamine as materials into a reaction kettle, stirring, adding glycine after the materials are clarified, adding dimethyl phosphite after the mixture is clarified, rising the temperature to be 50-60 DEG C, and keeping the temperature for 50 min; reducing the temperature to be 30 DEG C, and adding hydrochloric acid; slowing rising the temperature after stirring for 30 min to evaporate methyl alcohol; rising the temperature to be 110-125 DEG C; adding water into the reaction kettle, reducing the temperature to be below 70 DEG C, and externally cooling with cold water to reduce the temperature of the reaction kettle to be below 10 DEG C; adding triethylamine, controlling the temperature to be 15-25 DEG C, and reaching the reaction endpoint when the pH value in the reaction kettle is 0.5-1.5; transferring the materials to a crystallization kettle, reducing the temperature to be below 10 DEG C to crystallize the materials for a time; filtering, washing and drying the crystal to obtain glyphosate technical.

Description

Technical field [0001] The invention relates to the field of pesticide chemical industry, in particular to an improved method for synthesizing glyphosate by an alkyl ester method. Background technique [0002] Glyphosate herbicide is the world's largest variety of chemical pesticide products, accounting for more than 30% of total pesticide output. The annual production capacity of glyphosate in my country is about 800,000 tons. There are two synthetic methods: the alkyl ester method and the IDA method. The production output of the alkyl ester method accounts for more than 70% of the total output. The currently widely used alkyl ester synthesis process for glyphosate production is based on paraformaldehyde as the starting material, methanol as the solvent, and triethylamine as the catalyst to depolymerize the paraformaldehyde, and then add glycine for addition reaction. Dimethyl phosphite is added for condensation reaction, then hydrochloric acid is added for acidic hydrolysis re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
Inventor 蒋兆台玉红毕茜茜王胜蓝徐高福
Owner UNIV OF SHANGHAI FOR SCI & TECH
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