Process for producing O, S-dimethyl-N-acetylphosphoramidothioate

A technology of acetyl thiophosphoramidide and dimethyl thiophosphoramidide acetyl, applied in the improved O field, can solve problems such as high production cost, non-biodegradation, harsh operating conditions, etc., achieves improved production operating environment, reduced Production cost, effect of simplifying process facilities

Inactive Publication Date: 2010-04-07
陈兵
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are more than 30 manufacturers of O,S-dimethyl-N-acetylthiophosphoramide in China. Low efficiency, high production cost, etc., especially the post-treatment process mostly adopts ammonia water neutralization method, that is, adding ammonia water to the acylation solution of O, S-dimethyl-N-acetylthiophosphoramide for neutralization reaction, A large amount of industrial wastewater containing ammonium acetate is generated. The wastewater is colorless or light yellow liquid, slightly viscous, has a strong pesticide odor, and is not biodegradable. Therefore, the treatment of this type of wastewater has become a worldwide problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] In a 1000ml three-neck flask equipped with stirring, ice-salt bath, thermometer, and dropping funnel, add 216.9 grams of O, S-dimethylphosphorothioate with a content of 65%, and slowly add 155 grams of ethyl alcohol from the dropping funnel. For acid anhydride, cool down to 10°C with an ice-salt bath, slowly add 2 grams of 98% sulfuric acid dropwise, and control the temperature of dropping sulfuric acid at 20-25°C. Then, change the water bath to heat, react at 55-60°C for 1 hour, cool down to 20°C, add about 230ml of 25% sodium carbonate solution to pH=7-9 through the dropping funnel, and control the neutralization temperature at 20-30°C. Then, stand and separate layers, use 1,2-dichloroethane or trichloromethane to extract the lower oil phase and the upper water phase respectively, combine the extracts, and vacuum precipitation, crystallization or recrystallization, and drying, can be Obtained 197.8 grams of O, S-dimethyl-N-acetylphosphorothioate product. The O, S-dim...

Embodiment 2

[0013] In a 1000ml three-necked flask equipped with stirring, ice-salt bath, thermometer, and dropping funnel, add 100 grams of O, S-dimethylphosphorothioate with a content of 65%, and slowly add 52 grams of B For acid anhydride, cool down to 10°C with an ice-salt bath, slowly add 1 gram of 98% sulfuric acid dropwise, and control the temperature of the dropwise addition of sulfuric acid at 20-25°C. Then, change the water bath to heat, react at 55-60°C for 1 hour, cool down to 20°C, add about 500ml of 8% sodium bicarbonate solution from the dropping funnel to pH = 7-9, and control the neutralization temperature at 20-30°C . Then, stand and separate layers, use 1,2-dichloroethane or trichloromethane to extract the lower oil phase and the upper water phase respectively, combine the extracts, and vacuum precipitation, crystallization or recrystallization, and drying, can be Obtained 84 grams of O, S-dimethyl-N-acetylphosphorothioate product. The O,S-dimethyl-N-acetylthiophosphor...

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PUM

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Abstract

The invention discloses a new process for producing O, S-dimethyl-N-acetylphosphoramidothioate. In the prior neutralizing process for preparing the O, S-dimethyl-N-acetylphosphoramidothioate by adopting acetylation of O, S-dimethyl acetylphosphoramidothioate, the process adopts sodium carbonate solution or sodium bicarbonate solution to carry out neutralizing treatment; the process not only can effectively improve the production operating environment and simplify the process facilities, but also can facilitate the produced wastewater to be treated easily, and can reclaim sodium acetate conveniently with low cost so as to greatly reduce the production cost which can be reduced by about 5,000 yuan for each ton of O, S-dimethyl-N-acetylphosphoramidothioate; and the process is a new process which is economical and environmentally-friendly, is easy to be controlled and can be steadily operated for a long term.

Description

technical field [0001] The invention belongs to a pesticide production process, in particular to an improved O, S-dimethyl-N-acetylthiophosphoramide production process. Background technique [0002] O, S-Dimethyl-N-acetylthiophosphoramide is an acylated derivative of the insecticide methamidophos. It is a broad-spectrum organophosphorus insecticide with high efficiency, low toxicity and low residue. One of the ideal varieties with high toxicity and high residue pesticides. At present, there are more than 30 manufacturers of O,S-dimethyl-N-acetylthiophosphoramide in China. Low efficiency, high production cost, etc., especially the post-treatment process mostly adopts ammonia water neutralization method, that is, adding ammonia water to the acylation solution of O, S-dimethyl-N-acetylthiophosphoramide for neutralization reaction, A large amount of industrial wastewater containing ammonium acetate is generated. The wastewater is colorless or light yellow liquid, slightly visc...

Claims

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Application Information

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IPC IPC(8): C07F9/24
Inventor 陈兵
Owner 陈兵
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