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Method for synthesizing oxydemeton-methyl by taking phosphorus oxychloride as raw material through reaction in one step

A technology for acephate and acetamide is applied in the field of one-step reaction synthesis of acephate using phosphorus oxychloride as a raw material, and can solve the problems of large waste water discharge, high refrigeration energy consumption, high environmental control pressure and the like

Inactive Publication Date: 2012-07-25
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the production of all enterprises still follows the technological route that has been used for nearly 20 years, that is, the basic raw material is phosphorus trichloride, and the preparation process of phosphoryl dichloride and phosphoryl monochloride intermediates continues. It is prepared into spermine and methamidophos, and then acylated. After a total of 5 steps of reaction, it is finally prepared into acephate. This process has a large amount of waste water discharge and high energy consumption for freezing. Trichloride Taking sulfur phosphorus as raw material, producing one ton of acephate will generate at least 14 tons of waste water
The spermine product prepared by the old process route can only be used to produce acephate, because of the large amount of wastewater produced, foreign companies that produce acephate mainly import spermine from my country, and my country has become the world's largest In spermine-producing countries, the environmental governance pressure of spermine production enterprises has been increasing. Therefore, the original acephate production process route can no longer meet the requirements of social and environmental protection in the future. The social environmental protection and the economic benefits of such enterprises Contradictions have become very prominent and urgently need to be resolved

Method used

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  • Method for synthesizing oxydemeton-methyl by taking phosphorus oxychloride as raw material through reaction in one step
  • Method for synthesizing oxydemeton-methyl by taking phosphorus oxychloride as raw material through reaction in one step

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Molecular ratio: PSCl 3 Or O-methylphosphoryl dichloride or O, O-dimethylphosphoryl chloride:methanol:acetamide:sodium hydroxide (or X)=1:2~15:1:1~3

[0018] Put the calculated amount of acetamide, methanol and sodium hydroxide or X into the reaction bottle at one time, start stirring, control the temperature at 30-40°C, and drop the calculated amount of PSCl 3 , heat preservation reaction for 4 to 32 hours, cooling, standing, filtering, removing sodium chloride solid, distilling the filtered mother liquor, distilling off excess methanol solvent, cooling, standing, filtering, and drying to obtain acephate Drug solid, yield 90%, content 97%, filter the mother liquor for mechanical use.

[0019] In Example 1, X represents acid-binding agents such as potassium hydroxide, sodium acetate, sodium benzoate, sodium methoxide, N, N-dimethylformamide, ammonium acetate, or N, N-dimethylaniline.

Embodiment 2

[0021] Molecular ratio: PSCl 3 Or O-methylphosphoryl dichloride or O, O-dimethylphosphoryl chloride: methanol: acetamide: sodium hydroxide (or X) = 1:1~2:1:1~3

[0022] Weight ratio: acetamide: ether (or Y) = 1:9

[0023] Put the calculated amount of acetamide and ether or Y and methanol and sodium hydroxide or X into the reaction bottle at one time, start stirring, control the temperature at about 30°C, and drop the calculated amount of PSCl 3 , heat preservation reaction for 28 hours, lower the temperature, stand still, filter, and dry to obtain a solid mixture of acephate and sodium chloride, filter the mother liquor for mechanical use, dissolve acephate in the mixture solid with methanol, and remove the solid sodium chloride by filtration , and then distill the methanol solvent of the filtered mother liquor, lower the temperature, stand still, filter, and dry to obtain the original drug of acephate, with a content of 98% and a yield of 95%.

[0024] X represents the same...

Embodiment 3

[0026] Molecular ratio: PSCl 3 Or O-methylphosphoryl dichloride or O, O-dimethylphosphoryl chloride:methanol:acetamide=1:1~2:1

[0027] Weight ratio: acetamide: propyl ether (or Y) = 1:9

[0028] Put the calculated amount of acetamide and propyl ether or Y into the reaction flask at one time, start stirring, control the temperature at 30-40°C, and drop the calculated amount of PSCl 3 When the content of acetamide in the reaction system is tested by liquid chromatography normalization method 1≤%, the temperature is raised to control the temperature to reflux, the calculated amount of methanol or sodium methylate is added dropwise, and the methanol content in the reaction system is tested by gas chromatography normalization method≤1% , lower the temperature, stand still, filter, and dry to obtain the original drug of acephate, with a content of 95% and a yield of 90%, and filter the mother liquor for mechanical use.

[0029] The meaning of Y is the same as that of Y in Example...

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Abstract

The invention relates to a new method for synthesizing oxydemeton-methyl by taking combined thiophosphoryl chloride or other phosphorus oxychloride, carbinol and acetamide as raw materials only through one step of serial-connected pericyclic reaction. Compared with the prior art, the preparation cost of the oxydemeton-methyl is reduced by more than 50%, and cleaner production industrial design standards of zero discharging of waste water can be realized.

Description

[0001] The invention relates to a new method for synthesizing acephate through one-step serial pericyclic reaction by combining phosphorus trichloride or other phosphorus oxychlorides, methanol and acetamide as raw materials. Compared with the existing production process, acephate The preparation cost is reduced by more than 50%, and at the same time, the clean production industrial design standard of zero discharge of waste water is achieved. Background technique [0002] Acephate has been produced in my country for more than 20 years, and has developed into an important export-earning pesticide variety. Since the government banned the use and production of highly toxic pesticides such as methamidophos in 2007, due to acetyl With the advantages of low toxicity, wide insecticidal spectrum, low residue and good environmental compatibility, methamidophos has developed into one of the largest tonnage pesticide products in the market; in the international market, its sales volume of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/24
Inventor 李坚
Owner WUHAN INSTITUTE OF TECHNOLOGY
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