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Production method for O,O-dialkyl thiophosphoryl chloride

A technology for the production of alkylphosphorylthioxate, which is applied in the field of producing O,O-dialkylphosphorylthiochloride by chemical method, can solve the problems of difficult process control, complex process, and many raw materials, and achieve high power consumption , dark color, less environmental pollution effect

Inactive Publication Date: 2017-01-18
荆州市沙市东方有机化工研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0022] 3. The publication number "CN101486729A" discloses "a production method of O, O-dialkylphosphoryl thiochloride", which uses trimethyl phosphite, phosphorus pentasulfide, phosphorus trichloride, and chlorine as raw materials to produce O , O-dialkylphosphoryl thiochloride, although some shortcomings of the above two methods have been overcome, a large amount of hydrogen chloride, hydrogen sulfide, waste sulfur residue and sewage are still produced in the production process, and the raw materials used are many and the process is complicated , process control is difficult

Method used

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  • Production method for O,O-dialkyl thiophosphoryl chloride
  • Production method for O,O-dialkyl thiophosphoryl chloride
  • Production method for O,O-dialkyl thiophosphoryl chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Put dimethyl phosphite and sulfur into the reaction kettle, raise the temperature to 70°C, keep the temperature for 2 hours, then cool down to 20°C, then slowly add the measured chlorine into the reaction kettle, after the chlorine is added, put the measured Add water into the kettle and continue to stir for one hour. After layering, the lower layer is high-quality O,O-dimethylphosphorothioate monochloride. After analysis, the product content is 99.1%, and 158.8 grams of the product are obtained. The yield 98.1% (calculated as dimethyl phosphite).

[0043] The material feeding amount in this example is as follows:

[0044] Dimethyl phosphite: 112 grams, sulfur: 33.2 grams, chlorine: 74 grams, water: 145 grams.

Embodiment 2

[0046]Put diethyl phosphite and sulfur into the reaction kettle, raise the temperature to 75°C, keep it warm for 2 hours, then cool down to 20°C, then slowly add the metered chlorine into the reaction kettle, after the chlorine is added, add the metered water Put it into the kettle, continue to stir for one hour, and after layering, the lower layer is high-quality O, O-diethylphosphorothioate monochloride. After analysis, the product content is 99.6%, and 185.6 grams of the product are obtained, with a yield of 99.0%. (calculated as diethyl phosphite).

[0047] The material feeding amount in this example is as follows:

[0048] Diethyl phosphite: 140 grams, sulfur: 33.2, chlorine: 74 grams, water 175 grams.

Embodiment 3

[0050] Put dimethyl phosphite into the reaction kettle, raise the temperature to 40°C, slowly drop sulfur chloride into the reaction kettle, keep the temperature at 40°C and finish dropping the sulfur chloride; It is passed into the material under certain conditions; after the completion of chlorine passage, a certain amount of water is added, and the layers are washed with water, and the lower layer is O, O-dimethylphosphorylthiochloride. After analysis, the product content is 99.5%, and the product is obtained 316.2 grams, yield 98.6% (calculated as dimethyl phosphite).

[0051] The material feeding amount in this example is as follows:

[0052] Dimethyl phosphite: 224 grams, sulfur chloride: 138 grams, chlorine: 72 grams, water: 365 grams.

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Abstract

The invention relates to a production method for O,O-dialkyl thiophosphoryl chloride, and belongs to the field of manufacturing of O,O-dialkyl thiophosphoryl chloride through a chemical method. Raw materials comprise dialkyl phosphite, sulfur or sulfide, chlorine or a chlorinating agent and the like. The production method comprises the steps: carrying out a reaction of dialkyl phosphite and sulfur or sulfide in a synthesis kettle for 2 hours, then chloridizing by chlorine or the chlorinating agent to obtain an O,O-dialkyl thiophosphoryl chloride crude product, and then washing with water to obtain the product O,O-dialkyl thiophosphoryl chloride. The total yield can reach 98%-99%, the content of O,O-dialkyl thiophosphoryl chloride can reach more than or equal to 99.5%, the product quality is good, and the purity of the product can reach 99-99.9%; and the production method has the advantages of simple production process, safe production, low energy consumption, and no pollution. The problems in the prior art that a large amount of alcohol is needed to be recycled, consumption of steam is high and energy consumption is high are solved; and the problems that all the process routes need freezing, a large amount of freezing energy and circulating water is needed and the electric energy consumption is high are solved.

Description

technical field [0001] The invention relates to a production method of O, O-dialkylphosphoryl thiochloride, which belongs to the technical field of producing O, O-dialkylphosphoryl thiochloride by chemical method. Background technique [0002] 1. At present, the production of O, O-dimethylphosphoryl thiochloride in China adopts the reaction of phosphorus trichloride and sulfur to generate phosphorus trichloride, and then reacts with excess methanol to generate O-methylphosphoryl thiochloride ( Referred to as dichloride); dichloride reacts with excess methanol under alkali catalysis to generate O, O-dimethylphosphoryl thiochloride (referred to as monochloride). [0003] During production, sulfur reacts with phosphorus trichloride, and the yield and content can reach 97%. However, when phosphorus trichloride reacts with methanol to form dichloride, methanol must be in excess, and the molar ratio is 1:5. The reaction temperature must be maintained at about 0°C, and the reacti...

Claims

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Application Information

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IPC IPC(8): C07F9/20
CPCC07F9/20
Inventor 刘国罗方明罗朝龙罗朝林苏玲
Owner 荆州市沙市东方有机化工研究所
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