Synthesis method of diphenylphosphine chloride

Abstract

The invention discloses a synthesis method of diphenylphosphine chloride, belongs to that technical field of chemical synthesis and solves the problem of low yield of the prior diphenylphosphoric chloride product. The synthesis method of diphenylphosphine chloride is characterized by comprising the following steps: under that protection of dry nitrogen, opening and stirring, adding benzene, phosphorus trichloride and catalyst to a reactor, and raising the temperature to 50 DEG C-80 DEG C and performing reflux reaction at 50 DEG C-80 DEG C for 2-3 h; after the reaction in step S01 is completed, raising the temperature to 85-200 DEG C and performing reflux reaction at 85-200 DEG C; at that end of step S02, after the reactor is cooled down, adding benzene into the reactor, adding a decomplexing agent, stirring until the decomplexing agent is dissolved and distilling to remove benzol, and then performing vacuum distillation to obtain the front fraction and the rear fraction. The inventionhas the advantages of high product yield.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a synthesis method of diphenylphosphine chloride. Background technique [0002] Diphenylphosphine chloride is an important organophosphorus chemical product, the Ph 2 The P group can be used as a transition metal and metal carbonyl ligand, and is widely used as a catalyst for various reactions such as hydrogenation, carbonylation, and oligomerization. In addition, diphenylphosphine chloride is used in the production of flame retardants, Intermediates of important organophosphorus products such as pesticides, antioxidants, photoinitiators, etc. [0003] The "two-step" synthesis is a traditional method for preparing diphenylphosphine chloride. First, PhPCl is obtained from benzene and phosphorus trichloride through the catalytic reaction of excess aluminum trichloride. 2 , then PhPCl 2 Ph 2 PCl, but the yield of this method is low, and the reaction conditions are har...

AI Technical Summary

Problems solved by technology

[0003] The "two-step" synthesis is a traditional method for preparing diphenylphosphine chloride. First, PhPCl is obtained from benzene and phosphorus trichloride through the catalytic reaction of excess aluminum trichloride. 2 , then PhPCl 2 Ph 2 PCl, but the yield of this method is low, and the reaction conditions are harsh

[0004] There are also some synthetic methods that are different from the traditional ones, such as using Ph 3 P and PCl 3 As a raw material, Ph 2 The yield of PCl is 20%-50%; or use diphenylphosphorous oxychloride and triphenylphosphine as raw materials, and react at 400°C for more than 20h to obtain Ph 2 The yield of PCl is 30%; It has also been reported that a kind of preparation of Ph 2 The method of PCl, but diphenylphosphine oxide is difficult to prepare, and the reaction raw materials cannot be obtained easily

Using these methods to prepare Ph 2 PCl has the defects of high production cost, harsh reaction conditions, and low product yield, and cannot meet environmental protection requirements