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Process for preparing glyphosate by using glycine

A preparation process and glycine method technology, applied in the field of preparation technology, can solve the problems of complex reaction components, increase the ratio of raw materials, affect product quality, etc. Effect

Inactive Publication Date: 2010-05-12
CAC NANTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to solve this problem, many enterprises add more dimethyl phosphite, expecting to increase the yield of the product, but this process often leads to complex reaction components in the reaction process. For example, dimethyl phosphite is easily hydrolyzed to generate phosphorous acid and Methanol, etc., will eventually affect the quality of the product, and at the same time increase the proportion of raw materials and increase the production cost of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Add 33.6g of paraformaldehyde, 168g of methanol and 40.3g of triethylamine into a three-necked flask with a reflux condenser, a thermometer and a stirring device, keep the reaction temperature at 30°C, and stir to obtain a transparent reaction solution;

[0025] (2) Add 33 g of glycine to the above reaction solution, keep the temperature at 30° C., stir and react for 1 h to obtain a condensation solution;

[0026] (3) Add 68.5 g of dimethyl phosphite to the condensation solution, keep the temperature at 30° C., stir and react for 1 hour to obtain an esterification solution;

[0027] (4) Adding 212 g of hydrochloric acid with a weight percent concentration of 10% to the esterification solution for acidification, keeping the temperature at 20° C., to obtain a hydrolysis solution;

[0028] (5) Under normal pressure conditions, control the temperature at 80°C to carry out desolvation and deacidification, then under a vacuum pressure of 0.2MPa, control the temperature at...

Embodiment 2

[0030] (1) Add 33.6g of paraformaldehyde, 195g of methanol and 52.2g of triethylamine into a three-necked flask equipped with a reflux condenser, a thermometer and a stirring device, keep the reaction temperature at 40°C, and stir to obtain a transparent reaction solution;

[0031] (2) Add 38.3 g of glycine to the above reaction solution, keep the temperature at 40° C., stir and react for 1.5 h to obtain a condensation solution;

[0032] (3) Add 72.1 g of dimethyl phosphite to the condensation solution, keep the temperature at 40° C., stir and react for 1.5 h to obtain an esterification solution;

[0033] (4) Adding 212 g of hydrochloric acid with a weight percent concentration of 30% to the esterification solution for acidification, keeping the temperature at 30° C., to obtain a hydrolysis solution;

[0034] (5) Under normal pressure conditions, control the temperature at 100°C to carry out desolvation and deacidification, then under the vacuum pressure of 0.3MPa, control the...

Embodiment 3

[0036] (1) Add 33.6g of paraformaldehyde, 201.6g of methanol and 67.2g of triethylamine into a three-necked flask equipped with a reflux condenser, a thermometer and a stirring device, keep the reaction temperature at 50°C, and stir to obtain a transparent reaction solution;

[0037] (2) Add 50.4 g of glycine to the above reaction solution, keep the temperature at 45° C., stir and react for 2 hours to obtain a condensation solution;

[0038] (3) Add 84 g of dimethyl phosphite to the condensation solution, keep the temperature at 60° C., stir and react for 1.5 h to obtain an esterification solution;

[0039] (4) Adding 228.5 g of hydrochloric acid with a weight percent concentration of 35% to the esterification solution for acidification, keeping the temperature at 40° C., to obtain a hydrolysis solution;

[0040] (5) Under normal pressure conditions, control the temperature at 100°C to carry out desolvation and deacidification, then under the vacuum pressure of 0.4MPa, control...

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PUM

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Abstract

The invention relates to a process for preparing glyphosate by using glycine, which comprises the following steps: (1) putting paraformaldehyde, methanol and triethylamine in a reaction vessel, maintaining the reaction temperature to be 30-50 DEG C and stirring until the mixture is transparent; (2) adding the glycine to the reaction solution, and reacting to obtain condensation solution; (3) adding diisopropyl phosphate to the condensation solution, and reacting to obtain esterification solution; (4) adding hydrochloric acid to the esterification solution for acidification treatment to obtain hydrolysis solution; and (5) under the condition of normal pressure, controlling the temperature to be 80-130 DEG C for desolvation and deacidification, then under vacuum pressure, controlling the temperature to be 80-130 DEG C for deacidification by adding water two times, and finally adding deionized water and stirring for crystallization and leaching to obtain solid glyphosate. Compared with the prior art, the process has higher yield and convenient operation, saves the cost, and is suitable for industrial production due to production repeatability.

Description

technical field [0001] The invention relates to a preparation process, in particular to a preparation process of glyphosate by glycine method. Background technique [0002] Glyphosate, whose chemical name is N-(phosphonic acid methyl) glycine, is a broad-spectrum organic phosphorus systemic herbicide. In 1971, it was successfully developed by Monsanto Company of the United States for the first time. Due to its excellent performance, high efficiency, broad spectrum, low toxicity, environmental safety, etc., and other superior biological characteristics, it is currently the world's largest herbicide. One of the pesticides, enduring for more than 30 years. In recent years, with the promotion of genetically modified crops around the world, it has developed more rapidly, and it is currently the largest herbicide variety in the world. [0003] There are many patent reports on the synthesis methods of glyphosate at home and abroad, and the synthesis methods are rare among pestici...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38A01P13/00
Inventor 王方惠郑留清朱正江胡晓明郑锦彪田晓宏
Owner CAC NANTONG CHEM
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