O,S-dimethyl thiophosphoryl chloride, preparation and uses thereof

A technology of dimethyl thiophosphoryl and methamidophos, which is applied in chemical instruments and methods, organic chemistry, compounds of Group 5/15 elements of the periodic table, etc. Problems such as poor quality of amide and low yield of transisomerism

Inactive Publication Date: 2009-05-13
李坚
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are big defects in the original process, the transposition isomerization yield of 93-95% of O, O-dimethylphosphorothioate is low, less than 80%, and the generated O, S-dimethylphosphorothioate The quality is poor, the content is less than 73% to 75%, and the content has been reduced by 20%. So far, the content of O, S-dimethylphosphorophosphoramide products launched by domestic manufacturers is generally around 73%. The product produces chloramidophos and acephate, and its subsequent production process increases a lot of environmental governance costs. For example, based on O-methylphosphorothioate dichloride, one ton of O, O-dimethyl Thiophosphoramide, with at least 1.5 tons of NaCl and NH 4 CL waste brine, because O, O-dimethylthiophosphoramide is an important foreign exchange earning species for export, the total output of this species in my country is more than 50,000 tons / year, and it has a tendency to expand year by year. Therefore, every year At least 80,000 tons of waste salt water flow into rivers, seas, lakes and rivers. This kind of production process can no longer meet the basic requirements of the Chinese government for environmental protection in the future.

Method used

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  • O,S-dimethyl thiophosphoryl chloride, preparation and uses thereof
  • O,S-dimethyl thiophosphoryl chloride, preparation and uses thereof
  • O,S-dimethyl thiophosphoryl chloride, preparation and uses thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Put 100 grams of anhydrous O, S-dimethylphosphorothiochloride with a content of 97% into a 500ml three-necked flask, and then put in 100 grams of benzene or toluene as a solvent, start stirring, slowly heat up to 65-80°C, drop Add 2 to 6 grams of CH 3 I reagent, or pass through dry CH 3 CL gas, stirred and reacted for 6 to 8 hours, then, maintained the temperature at 70°C to 77°C, slowly added 20 grams of anhydrous methanol reagent dropwise, and continued to stir and react for 8 hours until the HCL gas did not continue to overflow, that is It is the end point of the reaction, then lower the temperature to 20-40°C, stop stirring, put the reaction material liquid into the separatory funnel, let it stand for 30 minutes, and separate the lower liquid, which is O, S-dimethylphosphoryl thiochloride product , had a weight of 94 grams, and a content of 92% to 95%.

Embodiment 2

[0029] Put 100 grams of anhydrous O, O-dimethylphosphorylthiochloride with a content of 91% into a 500ml three-necked flask, and put 100 grams of toluene as a solvent, start stirring, slowly heat up to 75-90°C, and drop 2 ~6 grams (CH 3 ) 2 SO 4 , stirred and reacted for 6-8 hours, cooled to 20-40°C, allowed to stand for 30 minutes to separate layers, and separated the lower liquid, which was O, S-dimethylphosphoryl thiochloride, with a weight of 86 grams and a content of 85%- 90%.

Embodiment 3

[0031] Put 100 grams of 95% anhydrous O, S-dimethylphosphoryl thiochloride into a 500ml three-necked flask, add 100 to 200 grams of dichloroethane as a solvent, start stirring, and 0 Slowly feed ammonia gas at ~40°C, analyze by gas chromatography, test that the content of O, S-dimethylphosphoryl thiochloride in the test reaction system is less than 0.5%, which is the end of the reaction, and filter out NH at room temperature 4 Cl is solid, then the mother liquor is evaporated to remove the dichloroethane solvent, evaporated to dryness as much as possible, and the distillation bottom is cooled to below 10°C to obtain a solid of methamidophos (chemical name O, S-dimethylphosphorothioate), It weighs 92 grams and has a content of 92%.

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Abstract

The invention relates to a novel compound of O, S-dimethyl thiophosphoryl chloride, a preparation method and application as intermediate or raw material of pesticide thereof. The novel compound can be used to prepare pesticide products, such as acephatemet, orthene and chloramine phosphorus. Compared with the prior process for preparing the acephatemet and the orthene, the method has the advantages that dislocation isomerism yield is improved by 15 percent; production cost is reduced by 10 percent and 20 percent; waste water discharge is reduced by 80 percent; and the cost for environmental protection and control is reduced by 60 percent.

Description

technical field [0001] The present invention relates to a new compound of O, S-dimethylphosphoryl thiochloride and its preparation and application, in particular to a new compound of O, S-dimethylphosphoryl thiochloride or O, O-dimethyl Thiophosphoryl chloride through to The transposition isomerization of O, S-dimethylphosphorothioate is generated, and the new compound generated by this is used as an intermediate or raw material, which can be used to prepare insecticides such as chloramidophos, acephate, methamidophos, etc. agent products. Background technique [0002] Chloramidophos, acephate, and methamidophos are all important pesticide products. For decades, it has always been using O, O-dimethylphosphorothioate as the basic raw material, that is, after to The transposition isomerization of O, S-dimethyl thiophosphoramide (ie methamidophos), and then the preparation of chloramidophos and acephate. There are big defects in the original process, the transposition...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/20C07F9/26
Inventor 李坚
Owner 李坚
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