Production method of O, O-dialkyl thiophosphoryl chloride

A technology of alkyl phosphorothioate and dimethyl phosphorothioate, applied in the production field of O, O-dialkyl phosphorothioate chloride, which can solve the problems of many by-products, large environmental pollution, and only , to achieve the effect of large cooling consumption and large heat release

Active Publication Date: 2009-07-22
荆州市沙市东方有机化工研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, it can be seen from the above reaction formula that a large amount of HCl and SO are produced by the reaction. 2 , S and NaCl, which cause great difficulties for recycling and post-proces

Method used

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

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Embodiment 1

[0055] Embodiment 1: The raw materials used in the synthesis of this product are phosphorus trichloride, anhydrous methanol, sulfur, first use phosphorus trichloride and anhydrous methanol in the presence of solvent benzene and acid-binding agent triethylamine in trialkyl synthesis The reaction in the kettle generates trimethyl phosphite, and the trimethyl phosphite reacts with phosphorus trichloride in the chlorinator to generate O, O-dimethyl phosphorus monochloride, and then O, O-dimethyl-phosphorous monochloride Phosphorus chloride and sulfur react in the sulfide to produce crude O, O-dimethylphosphoryl thiochloride, and after post-treatment, the fine product of O, O-dimethylphosphoryl thiochloride can be obtained.

[0056] The input amount of phosphorus trichloride in the present embodiment is 1037kg, methyl alcohol 483kg, sodium hydroxide 603kg, sulfur 242kg, the product O produced, the product amount of O-dimethylphosphoryl thiochloride is 1000kg. The total yield to pho...

Embodiment 2

[0057] Embodiment 2: The used raw material of this product synthesis is phosphorus trichloride, dehydrated alcohol, sulfur. First use phosphorus trichloride and absolute ethanol to react in a trialkyl synthesis kettle in the presence of solvent benzene and acid-binding agent triethylamine to generate triethyl phosphite. Triethyl phosphite reacts with phosphorus trichloride in the chlorinator to generate O, O-diethyl phosphorus monochloride, and then reacts O, O-diethyl phosphorus monochloride with sulfur in the vulcanizer Produce O, O-diethylthiophosphoryl chloride crude product; after post-treatment, O, O-diethylthiophosphoryl chloride is obtained.

[0058] The input amount of phosphorus trichloride in the present embodiment is 770kg, ethanol 519kg, sodium hydroxide 472kg, sulfur 181kg, and the product O produced, O-diethylthiophosphoryl chloride is 1000kg, and this product is to phosphorus trichloride The total yield is 94%, and its content is 99%.

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Abstract

The invention discloses a manufacturing method of O, O-dialkyl thiophosphoryl chloride; the manufacturing method comprises the steps that phosphorus trichloride, alcohol, sulfur and the like are taken as raw materials, wherein, the phosphorus trichloride reacts with alcohol in a trialkyl synthesis kettle to produce phosphorous acid trialkyl ester; then, the phosphorous acid trialkyl ester reacts with the phosphorus trichloride in a chlorinator to produce O, O-dialkyl phosphorus chloride; and the O, O-dialkyl phosphorus chloride reacts with sulfur in a vulcanizing apparatus to produce the crude products of O, O-dialkyl thiophosphoryl chloride which then is processed to obtained the refined products of the O, O-dialkyl thiophosphoryl chloride. The overall yield of the manufacturing method can be up to 94 percent, the content of the O, O-dialkyl thiophosphoryl chloride can reach 99 percent, and the manufacturing method is characterized by safe production, low energy consumption and no pollution.

Description

Technical field: [0001] The present invention relates to the chemical production of O,O-dialkylphosphorylthiochlorides, such as O,O-dimethylphosphorylchloride and O,O-diethylphosphorylchloride. 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 reacts with excess methanol to generate O-methylphosphoryl thiochloride (referred to as dichloride); dichloride reacts with excess methanol in the presence of a base to generate O, O-dimethylphosphoryl thiochloride (abbreviated as monochlorine). [0003] During production, sulfur reacts with phosphorus trichloride, and its yield and content can reach 97%. [0004] When phosphorus trichloride reacts with methanol to generate 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 reaction will generate ...

Claims

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Application Information

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