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Novel process for preparing glyphosate by glycin method

A technology of glycine and glyphosate, applied in herbicides and algicides, chemical instruments and methods, chemicals for biological control, etc., to achieve the effects of reducing pollution, reducing loss, and reducing material consumption

Active Publication Date: 2009-12-02
BEIJING ZIGUANG YINGLI CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few research reports on the dialkyl phosphite route. The invention patent with application number 85102988 discloses a glyphosate preparation process using dialkyl phosphite as raw material; the invention patent with application number 00125933 discloses An improvement to the process of dialkyl phosphite, which does not use paraformaldehyde but utilizes its own by-product methylal to synthesize glyphosate; in addition, "Research on the process of synthesizing glyphosate from trimethyl phosphite" ( "PESTICIDES" 1999.Vol.38No.6P8) has introduced the method that trimethyl phosphite and glycine synthesize glyphosate in aqueous phase; Method for synthesizing glyphosate from starting material

Method used

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  • Novel process for preparing glyphosate by glycin method

Examples

Experimental program
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Effect test

Embodiment 1

[0033]15.63g (0.5mol) of paraformaldehyde, 25.6g (0.253mol) of triethylamine, 19g (0.25mol) of glycine and 120ml of methanol were simultaneously placed in a 500mL four-necked flask with a reflux condenser, a thermometer and stirring, and stirred until After becoming transparent, the temperature was raised to 45°C, 30.90 g (0.30 mol) of dimethyl phosphite was added, and the reaction was maintained at 45-65°C until the reaction was completed. 45-70°C blow air analysis to recover methanol and triethylamine, after no obvious liquid outflow, naturally cool down to about 40°C, slowly add hydrochloric acid (30%) 38.00g (0.313mol) dropwise, keep warm at 50-75°C until reaction Completely, at the same time blow air to analyze and remove formaldehyde until the end of acidolysis, then deacidify under reduced pressure, stop the reduced pressure when the temperature reaches 110°C, add 40.00g of water, cool and crystallize, filter and dry to obtain 34.78g of glyphosate raw powder (content 97...

Embodiment 2

[0035] 11.72g (0.375mol) of paraformaldehyde, 25.6g (0.253mol) of triethylamine, 19g (0.25mol) of glycine and 120ml of methanol were simultaneously placed in a 500mL four-necked flask with a reflux condenser, a thermometer and stirring, and stirred until After becoming transparent, the temperature was raised to 45°C, 29.66g (0.288mol) of dimethyl phosphite was added, and the reaction was maintained at 45-65°C until the reaction was completed. Distill at 90-110°C under atmospheric pressure to separate and recover methanol and triethylamine. After no obvious liquid flows out, cool down naturally to about 40°C. Slowly add 38.00g (0.313mol) of hydrochloric acid (30%), and keep warm for acidolysis at 50-75°C until The reaction is complete, and at the same time blow air to analyze and remove formaldehyde until the end of acidolysis, deacidify under reduced pressure at the reaction temperature, add 20.00g of water, then use NaOH (30%) to adjust the pH to about 1.5, filter and dry to o...

Embodiment 3

[0037] 14.47g (0.463mol) of paraformaldehyde, 25.6g (0.253mol) of triethylamine, 19g (0.25mol) of glycine and 120ml of methanol were simultaneously placed in a 500mL four-necked flask with a reflux condenser, a thermometer and stirring, and stirred until After becoming transparent, the temperature was raised to 45°C, 25.75g (0.25mol) of dimethyl phosphite was added, and the reaction was maintained at 45-65°C until the reaction was completed. Recover methanol and triethylamine by distillation under reduced pressure at 40-70°C. After no obvious liquid flows out, the temperature is naturally lowered to about 40°C, and 51.71g (0.425mol) of hydrochloric acid (30%) is slowly added dropwise, and the pressure is reduced at 50-75°C (P = -0.01 to -0.03MPa) acidolysis until the reaction is complete, then adjust the pH to about 1.5 with NaOH (30%), filter and dry to obtain 34.02g (content 97%) of glyphosate former powder, the former powder yield 80.5%, The total yield is 85.5%.

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Abstract

The invention relates to a method for preparing glyphosate, which comprises the following steps: according to certain mixture ratio, putting glycin and paraformaldehyde into a monacid alcohol / tertiary amine system together for depolymerization condensation; then, after the mixture and dialkyl phosphate in mixing amount undergo condensation reaction, directly reclaiming monacid alcohol and tertiary amine; then, controlling temperature for acidolysis; in the acidolysis or after the acidolysis, removing and oxidizing formaldehyde; and deacidifying and neutralizing the reactant to prepare the glyphosate. The method adopts a plurality of methods such as reduction of the mixture ratio of the paraformaldehyde, direct exsolution and application, low-temperature acidolysis after the exsolution and the like to remove the influence of the formaldehyde, reduce consumption and stabilize the yield and the quality of the glyphosate.

Description

field of invention [0001] The present invention relates to a kind of method that is raw material preparation herbicide glyphosate (N-phosphonomethylglycine) with phosphite alkyl ester, specifically, the method of the present invention comprises the following steps: glycine and paraformaldehyde according to certain The proportioning ratio is put into the depolymerization and condensation reaction of the monohydric alcohol / tertiary amine system at the same time. At this time, the volatile components such as alcohol and amine can be recovered by means of normal pressure, reduced pressure or air analysis, and then mixed with the proportioning amount of dialkyl phosphite Condensation reaction of ester, then recovery of alcohol and amine by means of normal pressure, reduced pressure or air analysis, then temperature-controlled acidolysis, and removal or oxidation of formaldehyde during acidolysis, and then deacidification or neutralization to prepare glyphosate phosphine. Backgrou...

Claims

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Application Information

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IPC IPC(8): C07F9/38A01P13/00
Inventor 查正炯尹应武郭钰来谢增勇杨立雯易飞
Owner BEIJING ZIGUANG YINGLI CHEM TECH CO LTD
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