A process for catalyzing synthesis of glyphosate

A glyphosate and process technology, applied in the field of catalytic synthesis of glyphosate by glycine method, can solve the problems of increasing mother liquor production, increasing environmental protection pressure, and affecting economic benefits, achieving quality advantages, small tail gas, and depolymerization The effect of complete response

Active Publication Date: 2022-07-01
HUBEI TAISHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of the traditional process is low, which not only affects the economic benefits, but also increases the production of mother liquor and the pressure on environmental protection

Method used

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  • A process for catalyzing synthesis of glyphosate
  • A process for catalyzing synthesis of glyphosate
  • A process for catalyzing synthesis of glyphosate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044]1. Depolymerization reaction: First, put paraformaldehyde into the depolymerization kettle (the degree of polymerization of paraformaldehyde is 38), open the valve of the depolymerization kettle connected to the exhaust system pipeline, pass steam through the jacket, and heat and dehydrate at 60 ° C for 2 minutes . After dehydration, add methanol (the molar ratio of methanol and paraformaldehyde is controlled at 0.5:1), stir evenly, and add methanol solution of sodium methoxide to the mixed solution, and the depolymerization can be quickly completed in 30 seconds at room temperature. The methanol solution of active anhydrous formaldehyde, after the depolymerization is completed, add methanol until the molar ratio of paraformaldehyde to alcohol is 1:7.

[0045] The molar ratio of sodium methoxide to formaldehyde (the number of moles of paraformaldehyde is calculated as formaldehyde) is controlled: five parts per million.

[0046] 2. Addition reaction: After the depolymer...

Embodiment 2

[0052] 1. Depolymerization reaction:

[0053] First put paraformaldehyde into the depolymerization kettle (the degree of polymerization of paraformaldehyde is 50), open the valve of the pipe connected to the tail gas system of the depolymerization kettle, pass steam through the jacket, heat and dehydrate at 60 ° C for 3 minutes, and then add it after the dehydration is completed. Methanol (the molar ratio of methanol and paraformaldehyde is controlled at 0.6:1), stir evenly, add potassium methoxide solid to the mixed solution, and naturally react at 30 ° C for 20 s for depolymerization to generate highly active anhydrous formaldehyde. methanol solution; after the depolymerization is completed, add ethanol until the molar ratio of paraformaldehyde to alcohol is 1:7.8.

[0054] Molar ratio control of lithium methoxide and formaldehyde (the number of moles of paraformaldehyde is calculated as formaldehyde): 2 parts per million.

[0055] 2. Addition reaction:

[0056] After the ...

Embodiment 3

[0062] 1. Depolymerization reaction: The purchased alcohol solution of anhydrous formaldehyde is used as the raw material of formaldehyde, the methanol solution of catalyst potassium methoxide is added to the alcohol solution of anhydrous formaldehyde, and the reaction is carried out for 20 seconds; after the depolymerization is completed, methanol is added to paraformaldehyde and alcohol. The molar ratio is 1:2.2;

[0063] The molar ratio of the potassium methoxide to formaldehyde is controlled: five parts per million.

[0064] 2. Addition reaction: After the depolymerization is completed, add triethylamine to the mixed solution, then add glycine, and stir evenly. The addition reaction occurs under the action of the new alkoxy group and the molecules of formaldehyde and hemiacetal. After the addition reaction was completed, the mixed solution was rapidly heated to 60° C., maintained at a temperature of 18 s, then cooled to about 38° C., and then dimethyl phosphite was added ...

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Abstract

An organic catalyst for synthesizing glyphosate, the catalyst is an alkoxy compound comprising the first main group alkali metal, and also comprises fresh anhydrous methanol, ethanol and potassium, sodium metal or potassium, sodium anhydrous hydroxide Or a combination of one or more of the alkoxy metal compounds prepared by oxides or prepared by alkali metal reaction, and in the form of alcoholic solutions of the alkoxy metal compounds. In the process of synthesizing glyphosate, paraformaldehyde or methanol solution of formaldehyde is depolymerized after adding organic catalyst, and after the reaction is completed, triethylamine and glycine are added to stir for addition reaction; after the reaction is completed, dimethyl phosphite is added to carry out Condensation reaction, hydrochloric acid is added for hydrolysis after the reaction is completed, and then glyphosate is obtained through crystallization, washing and drying. Using a specific catalyst to improve the reaction speed and reaction selectivity of glyphosate synthesis, the depolymerization reaction speed is fast, the reaction is thorough, the addition reaction selectivity is also high, and the glyphosate product yield is more than 5% higher, which has the advantages of reaction and energy saving. , cost advantage, environmental protection advantage.

Description

technical field [0001] The invention belongs to the technical field of glyphosate production, in particular to a catalytic synthesis method of glyphosate by glycine method. Background technique [0002] Glyphosate is a high-efficiency, low-toxicity, broad-spectrum, and biocidal herbicide of systemic conduction type. There are two mainstream production methods, one is the production method using iminodiacetic acid (IDA) as raw material, the other is A production method using glycine and alkyl phosphite as raw materials. Most foreign companies, mainly Monsanto, use the iminodiacetic acid method to produce them. The production of glyphosate in my country started in the 1980s. In 1987, Shenyang Research Institute of Chemical Industry launched the glycine-alkyl ester method to synthesize glyphosate with glycine and dimethyl phosphite as the main raw materials. ) from the initial steady 65% ​​to about 75%. Glycine method glyphosate process uses methanol as solvent and triethyl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38B01J31/02
CPCC07F9/3813B01J31/0212
Inventor 田义群胡波何贵洲
Owner HUBEI TAISHENG CHEM
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