Preparation method of diphenyl phosphine chloride

Abstract

The invention relates to a preparation method of diphenyl phosphine chloride, which belongs to the technical field of chemical synthesis, and comprises the following steps: adding benzene and aluminumtrichloride into a reaction kettle, adding phosphorus trichloride into the kettle while stirring, slowly heating the mixture to 120 DEG C, and carrying out a reaction for 12 hours; stopping heating,cooling the reaction product to 60 DEG C, adding a decomplexing agent in batches, heating the reaction product to 80 DEG C, and stirring the reaction product for 2 hours; desolventizing the reaction product, and rectifying the reaction product to separate out phenyl phosphine dichloride and diphenyl phosphine chloride; after the rectification, the product is properly cooled, then slowly adding residual liquid into a 20% hydrochloric acid solution, stirring the mixture for 2 hours, centrifuging the mixture to obtain a wet decomplexing agent product and an aluminum chloride solution, drying thewet decomplexing agent product, and recycling the dried wet decomplexing agent product, and using the aluminum chloride solution for preparing a flocculating agent. According to the method, a new decomplexing agent is used, so that the solid waste problem of diphenyl phosphine chloride production is solved, the production cost is reduced, and the product has market competitiveness.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a preparation method of diphenylphosphine chloride. Background technique [0002] Diphenylphosphine chloride is an important intermediate for the production of photoinitiator TPO. At present, the method for industrial synthesis of diphenylphosphine chloride is to use benzene and phosphorus trichloride to generate phenyl diphenyl dichloride under the action of Lewis acid. Phosphine chloride, then through disproportionation reaction, and then use potassium chloride, sodium chloride, cyclic ether, phosphorus oxychloride, etc. as decomplexing agents to decomplex to obtain diphenylphosphine chloride. This method has low yield and is difficult to distill At the same time, a large amount of solid waste is produced, which seriously pollutes the environment. [0003] In order to solve the above-mentioned problems, in the current research, it is generally used to replace the ca...

AI Technical Summary

Problems solved by technology

[0002] Diphenylphosphine chloride is an important intermediate for the production of photoinitiator TPO. At present, the method for industrial synthesis of diphenylphosphine chloride is to use benzene and phosphorus trichloride to generate phenyl diphenyl dichloride under the action of Lewis acid. Phosphine chloride, then through disproportionation reaction, and then use potassium chloride, sodium chloride, cyclic ether, phosphorus oxychloride, etc. as decomplexing agents to decomplex to obtain diphenylphosphine chloride. This method has low yield and is difficult to distill At the same time, a large amount of solid waste is produced, which seriously pollutes the environment

The decomplexed substances of this decomplexing agent are separated by liquid separation, but a large amount of organic solvents are used in the synthesis process, and the decomplexing agent cannot be recovered