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Glyphosate synthesis method for improving utilization rate of dimethyl phosphite

A technology for the synthesis of dimethyl phosphite, which is applied in the field of pesticide chemical industry, can solve the problems of great influence on the recovery rate of glycine, low utilization of dimethyl phosphite, and waste of glycine, etc., so as to reduce production cost, improve utilization rate, The effect of reducing raw material consumption

Pending Publication Date: 2021-07-30
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the moisture in the synthetic liquid has a great influence on the recovery rate of glycine, and glycine cannot be crystallized after the moisture is >5%.
[0008] Due to the low utilization of dimethyl phosphite and the waste of glycine in the current glycine synthesis method of glyphosate

Method used

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  • Glyphosate synthesis method for improving utilization rate of dimethyl phosphite
  • Glyphosate synthesis method for improving utilization rate of dimethyl phosphite
  • Glyphosate synthesis method for improving utilization rate of dimethyl phosphite

Examples

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Effect test

Embodiment 1

[0071] This embodiment provides a figure 1 The glyphosate synthetic method that improves the utilization rate of dimethyl phosphite shown, the glyphosate synthetic method comprises the steps:

[0072] (1) Add 38g of paraformaldehyde, 208g of methanol and 67.6g of triethylamine into a 1000mL four-necked reaction flask, raise the temperature to 47°C, stir for 30 minutes and then cool down to 37°C to complete the depolymerization reaction;

[0073] (2) Add 57.6 g of glycine to the depolymerization reaction product, control the temperature at 42° C., and stir for 60 minutes to complete the addition reaction;

[0074](3) Add 82.4 g of dimethyl phosphite to the addition reaction product, control the temperature at 52°C, and stir for 80 minutes to complete the condensation reaction;

[0075] (4) Pass 15g of hydrogen chloride gas into the product after the condensation reaction, add 18g of water, control the temperature at 40°C, stir for 60 minutes, add 100g of methanol for alcohol a...

Embodiment 2

[0078] This embodiment provides a figure 1 The glyphosate synthetic method that improves the utilization rate of dimethyl phosphite shown, the glyphosate synthetic method comprises the steps:

[0079] (1) Add 38g of paraformaldehyde, 208g of methanol and 67.6g of triethylamine into a 1000mL four-necked reaction flask, raise the temperature to 47°C, stir for 30 minutes and then cool down to 37°C to complete the depolymerization reaction;

[0080] (2) Add 49.2 g of glycine to the depolymerization reaction product, add 8 g of glycine recovered in Example 1, control the temperature at 42° C., and stir for 50 minutes to complete the addition reaction;

[0081] (3) Add 82.4 g of dimethyl phosphite to the addition reaction product, control the temperature at 52°C, and stir for 80 minutes to complete the condensation reaction;

[0082] (4) Add 27.8g of 36% hydrochloric acid to the product after the condensation reaction, control the temperature at 45°C, stir for 30 minutes, add 100g ...

Embodiment 3

[0085] This embodiment provides a figure 1 The glyphosate synthetic method that improves the utilization rate of dimethyl phosphite shown, the glyphosate synthetic method comprises the steps:

[0086] (1) Add 38g of paraformaldehyde, 208g of methanol and 68.6g of triethylamine into a 1000mL four-necked reaction flask, raise the temperature to 47°C, stir for 30 minutes and cool down to 37°C to complete the depolymerization reaction;

[0087] (2) Add 47.6 g of glycine to the depolymerization reaction product, add 5 g of glycine recovered in Example 2, control the temperature at 42° C., and stir for 60 minutes to complete the addition reaction;

[0088] (3) Add 82.4 g of dimethyl phosphite to the addition reaction product, control the temperature at 52°C, and stir for 80 minutes to complete the condensation reaction;

[0089] (4) Add 18g of 36% hydrochloric acid to the product after the condensation reaction, control the temperature at 40°C, stir for 30 minutes, add 50g of metha...

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Abstract

The invention provides a glyphosate synthesis method for improving the utilization rate of dimethyl phosphite. According to the glyphosate synthesis method, dimethyl phosphite, triethylamine, paraformaldehyde and glycine serve as raw materials, the addition amount of triethylamine and glycine in the reaction raw materials is increased to promote complete reaction of a formaldehyde substrate in a reaction system, generation of a by-product glyphosine is reduced, the utilization rate of dimethyl phosphite is increased, and redundant glycine is recycled for mechanical application, so that the purposes of reducing the overall raw material consumption of glyphosate and reducing the production cost are achieved. The molar ratio of the dimethyl phosphite to the triethylamine to the paraformaldehyde to the glycine is 1: (0.82 to 0.99): (1.60 to 1.80): (0.88 to 1.17).

Description

technical field [0001] The invention belongs to the field of pesticide chemical industry, and specifically relates to a synthesis method of glyphosate, in particular to a synthesis method of glyphosate for improving the utilization rate of dimethyl phosphite. Background technique [0002] Glyphosate is a high-efficiency, non-selective, destructive organophosphorus herbicide raw material, absorbed by roots, stems and leaves to all parts of the plant, without adverse effects on crop seeds, fruits, organisms and soil. It is the most widely used in the global market. The most widely used herbicide in the field of crops. [0003] At present, there are two main production routes for glyphosate to achieve industrialization: one is the relatively common domestic production method using glycine as raw material; the other is the production method using iminodiacetic acid (IDA) as raw material. Among them, the glycine production route mainly uses paraformaldehyde, glycine, and dimethy...

Claims

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Application Information

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IPC IPC(8): C07F9/38
CPCC07F9/3813
Inventor 周曙光秦龙詹波钱志刚张斌沈涵李杭斌
Owner ZHEJIANG XINAN CHEM INDAL GROUP
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