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Preparation method of glyphosate

A technology of glyphosate and glycine, which is applied in the field of preparation of glyphosate, can solve the problems of long production process, cumbersome and various types of use, etc., and achieves the effects of low cost, short reaction process and short production process.

Active Publication Date: 2013-04-03
SHANDONG WEIFANG RAINBOW CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention aims at the problems that the existing dialkyl phosphite method uses many types of raw materials, and the production process is long and cumbersome. The process is improved, and glyphosate is synthesized by a one-pot method. , Less wastewater discharge, high product yield, more convenient for industrialized production, and strong economic value

Method used

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  • Preparation method of glyphosate

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Effect test

Embodiment 1

[0026] Dissolve 75g of glycine and 90g of phosphorous acid in 300g of water, stir at room temperature for 30min, and set aside. Put 125g of 36.5% formaldehyde, 150g of 30% hydrochloric acid and 300g of water into the autoclave, heat up to 60-65°C while stirring, slowly add glycine phosphorous acid solution, and seal the autoclave after adding. Slowly raise the temperature to 140°C, and react at 140°C and 6.2MPa for 10 hours. After the heat preservation is completed, deacidify under reduced pressure until a large amount of solids are precipitated, then lower the temperature, add a small amount of liquid caustic soda, adjust the pH of the system to 1-1.5, filter, and dry. 149.6g of glyphosate technical substance was obtained, the detection content was 96.2%, and the yield was 86.4%.

Embodiment 2

[0028] Dissolve 100g of glycine and 120g of phosphorous acid in 400g of water, stir at room temperature for 60min, and set aside. Put 170g of 36.5% formaldehyde, 200g of 30% hydrochloric acid and 400g of water into the autoclave, heat up to 70-75°C while stirring, slowly add glycine phosphorous acid solution, and seal the autoclave after adding. Slowly raise the temperature to 160°C, and react at 160°C and 7.9MPa for 8 hours. After the heat preservation is completed, deacidify under reduced pressure until a large amount of solids are precipitated, then lower the temperature, add a small amount of liquid caustic soda, adjust the pH of the system to 1-1.5, filter, and dry. 198.5g of the original glyphosate was obtained, the detection content was 96.5%, and the yield was 86.3%.

Embodiment 3

[0030] Dissolve 75g of glycine and 90g of phosphorous acid in 300g of water, stir at room temperature for 60min, and set aside. Put 130g of 36.5% formaldehyde, 400g of 50% sulfuric acid and 400g of water into the autoclave, heat up to 70-75°C while stirring, slowly add glycine phosphorous acid solution, and seal the autoclave after adding. Slowly raise the temperature to 180°C, and react at 180°C and 9.9MPa for 7 hours. After the heat preservation is completed, lower the temperature, add a small amount of liquid caustic soda, and adjust the pH of the system to 1-1.5. The original drug is 141.1g, the detected content is 95.8%, and the yield is 81.2%.

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Abstract

The invention discloses a preparation method of glyphosate, which comprises the following steps: adding a glycine and phosphite mixed solution into a formaldehyde acidic solution, reacting at 80-190 DEG C under 0.5-10 MPa after finishing the addition, and carrying out after-treatment on the reaction solution to obtain the glyphosate. The invention adopts the one-pot method to synthesize the glyphosate, has the advantages of short process, high glyphosate yield, low raw material consumption, no consumption of catalyst triethylamine, low cost and less wastewater (the wastewater generation amount can be reduced by about 30-50%), and is simple to operate.

Description

technical field [0001] The invention relates to a preparation method of glyphosate, in particular to a new method for preparing glyphosate under high temperature conditions with glycine as a starting material. Background technique [0002] Glyphosate, the chemical name is N-phosphonomethylglycine (PMG), and its molecular formula is: . [0003] [0004] Glyphosate, as a high-efficiency, broad-spectrum, low-toxicity, and safe organic phosphine post-emergence herbicide, is very effective in the control of perennial deep-rooted weeds, and has important roles in agriculture, forestry, animal husbandry, and horticulture. It is one of the most widely used herbicides at present. Its application path has been continuously broadened by means of cultivating various glyphosate-resistant transgenic crop varieties. In recent years, glyphosate has maintained a high growth rate of use. It is currently the most widely used herbicide in the world. [0005] At present, there are many glypho...

Claims

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Application Information

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IPC IPC(8): C07F9/38
Inventor 孙国庆侯永生牛月利李志清
Owner SHANDONG WEIFANG RAINBOW CHEM