Preparation method for producing dialkyl chlorophosphate reagent from polyethylene glycol

Abstract

The present invention provides a preparation method for producing a dialkyl chlorophosphate reagent from polyethylene glycol. The preparation method comprises: adding a preset amount of polyethylene glycol to a reaction bottle, replacing the air in the reaction bottle with an inert gas, cooling to a preset temperature, adding trisodium phosphate to the reaction bottle in a dropwise manner, diluting with a preset amount of an anhydrous solvent when the reaction is completed, filtering the product, and concentrating the product to obtain the dialkyl chlorophosphoric acid. According to the present invention, the reaction can be completely performed without any solvents in the dialkyl chlorophosphate preparation process, the reaction time is short, and the liquid waste cannot be generated; and the obtained product has the sufficient purity under the normal circumstance, the general organic synthesis requirement can be met, and the further distillation can be performed if the purity does not meet the requirement.

Description

technical field [0001] The invention relates to a preparation method, in particular to a preparation method for preparing dihydrocarbyl chlorophosphate reagent from polyethylene glycol. Background technique [0002] Dihydrocarbyl chlorophosphate is an important reagent for the synthesis of organophosphorus compounds, especially phosphoric acid mixed ester compounds. Dihydrocarbyl chlorophosphate is prepared by reacting phosphite with gaseous chlorine sources such as chlorine and phosgene. After the reaction, it is necessary to use dry air and lead carbonate to remove the dissolved gas and acid in the product. Generate solid waste that pollutes the environment. In the prior art, nitrogen-chloro-succinimide or trichloroisocyanuric acid is used as the chlorine source. [0003] In the process of realizing the present invention, the inventor finds that there are at least the following problems in the prior art: [0004] The preparation method of prior art uses acetonitrile or ...

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Problems solved by technology

[0004] The preparation method of prior art uses acetonitrile or toluene as solvent, produces unnecessary liquid waste; The reaction process needs to be heated, and the reaction time is long; The number of carbon atoms in the hydrocarbon group increases, the yield of the product decreases, the reaction is incomplete, and the product is difficult to purify

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