Preparation method of O, O '-dimethyl thiophosphamide

A technology of dimethyl thiophosphoramide and dimethyl thiophosphoryl, which is applied in the field of preparation of O,O'-dimethyl thiophosphorylamide, can solve the problem that sewage is difficult to treat, discharge is difficult to meet standards, and ammonia concentration is difficult to achieve. low problems, to achieve the effect of fast response, low cost and improved economic benefits

Pending Publication Date: 2020-09-29
杭州润盛科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the biggest disadvantage of this process is that the concentration of ammonia water is low (17%-20%), which will produce a large amount of sewage containing chlorine, nitrogen and phosphorus
The amount of sewage is large, the COD is extremely high, the sewage is difficult to treat, the cost is high, and the discharge is difficult to meet the standards, which has caused great pressure on environmental protection

Method used

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  • Preparation method of O, O '-dimethyl thiophosphamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Put 210 kg of water and 1050 kg of O, O'-dimethylphosphorothioate (content 92.5%) into a 3000-liter glass-lined reaction pot, start the stirring blade and directly feed liquid ammonia at a temperature of 15 ° C, and pass the ammonia pressure It is 0.15kPa, and the ammonia ratio is controlled to be 30%. When the pH value of the reaction solution reaches 8-9, the ammonia flow is stopped until the end point. The ammonia reaction time is 2 hours, and then the discharge is centrifuged, and the solid ammonium chloride is rinsed with cold water at 0-5°C; the liquid part is the organic phase mainly composed of O,O'-dimethylthiophosphoramide and the ammonium chloride solution. A mixed liquid formed from an aqueous phase. The mixed liquid is transferred to the separator for separation, and the water phase is sent to the reaction pot for continued production and use. After being recycled and supersaturated, the solid ammonium chloride is recovered by filtration, and the water phas...

Embodiment 2

[0028] Put 1300 kg of water and 800 kg of O, O'-dimethyl thiophosphoryl chloride (92.5% content) into a 3000-liter glass-lined reaction pot, start the stirring paddle at a temperature of 40°C and directly feed ammonia to the ammonia pressure It is 0.17kPa, and the ammonia ratio is controlled to be 32%. When the pH value of the reaction solution reaches 8-9, the ammonia flow is stopped until the end point. The ammonia reaction time is 2.5 hours, and then the material is centrifuged, and the liquid part is a mixed liquid formed by an organic phase mainly composed of O, O'-dimethylphosphorothioate and an aqueous phase of an ammonium chloride solution. The mixed liquid is transferred to the separator for separation, and the water phase is sent to the reaction pot for continued production and use. After being recycled and supersaturated, the solid ammonium chloride is recovered by filtration, and the water phase is continued for production and use. After the organic phase is post-t...

Embodiment 3

[0030] Put 520 kg of water into a 3000-liter glass-lined reaction pot, then add 1300 kg of O, O'-dimethylphosphoryl thiochloride (content 99.5%), start the stirring blade and directly feed ammonia at 0°C. The ammonia pressure is 0.18kPa, and the ammonia ratio is controlled to be 35%. When the pH value of the reaction solution reaches 8-9, the ammonia flow is stopped until the end point. The ammonia reaction time is 2.5 hours, and then the material is centrifuged, and the liquid part is a mixed liquid formed by an organic phase mainly composed of O, O'-dimethylphosphorothioate and an aqueous phase of an ammonium chloride solution. The mixed liquid is transferred to the separator for separation, and the water phase is sent to the reaction pot for continued production and use. After being recycled and supersaturated, the solid ammonium chloride is recovered by filtration, and the water phase is continued for production and use. After the organic phase is post-treated, it is refin...

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Abstract

The invention discloses a preparation method of O, O '-dimethyl thiophosphoric amide. The method comprises the following steps: adding water and O, O '-dimethyl thiophosphoryl chloride into a reactioncontainer, stirring, introducing liquid ammonia at a set temperature to enable the mass ratio of the water in the reaction container to the introduced liquid ammonia to be 1: (0.30-0.35) for ammoniation reaction, and stopping introducing the liquid ammonia when the pH value of reaction liquid reaches 8-9; after the reaction is finished, carrying out liquid-solid separation, separating out a water-phase liquid, an organic-phase liquid and a white ammonium chloride solid, and introducing the separated water-phase liquid into a reaction container for cyclic utilization; and distilling the organic phase liquid to recover the solvent, thereby obtaining O, O '-dimethyl thiophosphoric amide. According to the method, the ammonia ratio of a reaction system is increased, the speed is high, the reaction is complete, no wastewater is discharged, the yield is high and the quality is good.

Description

technical field [0001] The invention relates to a preparation method of O, O'-dimethylphosphorothioate, belonging to the technical field of chemical manufacturing. Background technique [0002] O, O'-dimethylphosphorothioate is an important intermediate in the production of methamidophos series of high-efficiency and low-toxicity pesticides. [0003] O,O'-dimethylphosphorothioate is obtained from O,O'-dimethylphosphorothiochloride (abbreviated as monochloride) through ammonolysis reaction, and its synthesis methods mainly include the following: [0004] For example, "Feng Jitao, Li Ruzhi. Fine and Specialty Chemicals, 2003, 11(22): 13-14", "Zhang Yongqin, Yuan Hua, Yu Zongyuan. Hubei Chemical Industry, 1997, 14(3): 7-10" published O, O'-dimethylphosphoryl thiochloride and 16% to 18% ammonia water are used as raw materials, dichloroethane, benzene, etc. are used as solvents, and O, O'-dimethoxy Methyl phosphorothioate. This method has the disadvantages of consuming a large...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/24
CPCC07F9/2408
Inventor 金士庆
Owner 杭州润盛科技有限公司
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