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Organic catalyst for synthesis of glyphosate and glyphosate synthesizing process

An organic catalyst, glyphosate technology, applied in the direction of organic compound/hydride/coordination complex catalyst, organic chemistry, physical/chemical process catalyst, etc., can solve the problem of increasing the production of mother liquor, increasing environmental protection pressure, impact Economic benefits and other issues, to achieve the effect of quality advantages, small exhaust gas, and complete depolymerization reaction

Active Publication Date: 2020-03-06
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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  • Organic catalyst for synthesis of glyphosate and glyphosate synthesizing process
  • Organic catalyst for synthesis of glyphosate and glyphosate synthesizing process
  • Organic catalyst for synthesis of glyphosate and glyphosate synthesizing process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] 1. Depolymerization reaction: first put paraformaldehyde into the depolymerization kettle (the degree of polymerization of paraformaldehyde is 38), open the valve of the pipeline connecting the depolymerization kettle to the tail gas system, pass steam through the jacket, and heat and dehydrate at 60°C for 2 minutes . After the dehydration is completed, add methanol (the molar ratio of methanol to paraformaldehyde is controlled at 0.5:1), stir evenly, add a methanol solution of sodium methoxide to the mixed solution, and depolymerize quickly at room temperature in 30 seconds to form high Active methanol solution of anhydrous formaldehyde, after depolymerization is completed, add methanol until the molar ratio of paraformaldehyde to alcohol is 1:6.

[0046] The molar ratio control of lithium methylate and formaldehyde (the molar number of paraformaldehyde is calculated as formaldehyde): 5 parts per million.

[0047] 2. Addition reaction: After the depolymerization is co...

Embodiment 2

[0053] 1. Depolymerization reaction:

[0054] First put paraformaldehyde into the depolymerization kettle (the degree of polymerization of paraformaldehyde is 50), open the valve of the pipeline connecting the depolymerization kettle to the tail gas system, pass steam through the jacket, heat and dehydrate at 60°C for 3 minutes, and then add Methanol (the molar ratio of methanol to paraformaldehyde is controlled at 0.6:1), stir evenly, add methanol solution of lithium methoxide to the mixed solution, react naturally at 30°C for 20s for depolymerization reaction, and generate highly active anhydrous formaldehyde methanol solution; after depolymerization, add ethanol until the molar ratio of paraformaldehyde to alcohol is 1:7.8.

[0055] The molar ratio control of lithium methylate and formaldehyde (the molar number of paraformaldehyde is calculated as formaldehyde): one part per million.

[0056] 2. Addition reaction:

[0057] After the depolymerization is completed, add trie...

Embodiment 3

[0063] 1. Depolymerization reaction: use the purchased alcohol solution of anhydrous formaldehyde as formaldehyde raw material, add the methanol solution of catalyst potassium methylate into the alcohol solution of anhydrous formaldehyde, and react for 20 seconds; The molar ratio is 1:2.2;

[0064] The molar ratio control of the potassium methylate and formaldehyde: fifty parts per million.

[0065] 2. Addition reaction: After the depolymerization is completed, add triethylamine to the mixed solution, then add glycine, stir evenly, control the reaction temperature at 50°C, and the reaction time for 35 minutes. The addition reaction occurs under the action of nascent alkoxy groups and formaldehyde and hemiacetal molecules. After the addition reaction is over, the mixed solution is rapidly heated to 60°C, kept for 18s, then cooled to about 38°C, and then dimethyl phosphite is added for condensation reaction.

[0066] 3. Condensation reaction: After the addition reaction is com...

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Abstract

The invention discloses an organic catalyst for synthesis of glyphosate. The catalyst is an alkoxy compound including alkali metal in the first main group, also comprises alkoxy metal compounds whichare prepared through a reaction between fresh anhydrous alcohol and anhydrous hydroxides or oxides of the first main-group alkali metal or the alkali metal, and is one or a combination of more of thealkoxy metal compounds in the form of an alcohol solution of the alkoxy metal compounds. The glyphosate synthesizing process comprises the steps: adding the organic catalyst to a methanol solution ofparaformaldehyde or formaldehyde, performing a depolymerization reaction, adding triethylamine and glycine after completion of the reaction, performing stirring for an addition reaction, adding dimethyl phosphite after completion of the reaction, performing a condensation reaction, adding hydrochloric acid for hydrolysis after completion of the reaction, and then performing crystallization, washing and drying so as to obtain glyphosate. The reaction speed and reaction selectivity of glyphosate synthesis can be improved through the specific catalyst, the depolymerization reaction has a high speed and thoroughness, and the addition reaction also has high selectivity, so that the yield of the glyphosate product reaches 3% or above; and the process has the advantages of reactions, energy saving, cost and environmental protection.

Description

technical field [0001] The invention belongs to the technical field of glyphosate production, in particular to a catalytic synthesis method of glyphosate by a glycine method. Background technique [0002] Glyphosate is a high-efficiency, low-toxicity, broad-spectrum, and herbicide of systemic conduction type. There are two mainstream production methods, one is the production method using iminodiacetic acid (IDA) as the raw material, and the other is the production method using The production method of glycine and alkyl phosphite as raw materials. The foreign companies dominated by Monsanto basically adopt the iminodiacetic acid method for production. my country's glyphosate production 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. Calculated) from the initial stable 65% to about 75%. The glycine method glyphosate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07F9/38
CPCB01J31/0212C07F9/3813Y02P20/584
Inventor 胡波黄明华黄丹丹许长泽
Owner HUBEI TAISHENG CHEM
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