Preparation method of diphenyl phosphine chloride

A technology of diphenylphosphine chloride and aluminum chloride, which is applied in chemical instruments and methods, organic chemistry, compounds of Group 5/15 elements of the periodic table, etc., and can solve difficult distillation, environmental pollution, low yield, etc. problem, achieve the effect of increasing the yield and solving the difficulty of distillation

Inactive Publication Date: 2019-12-27
江苏多森新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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 oxychlo...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1 The preparation method of a kind of diphenylphosphine chloride of the present invention comprises the following steps: 455kg (5.82mol) of benzene and 777kg (5.82mol) of aluminum trichloride are dropped into the reactor, and are added into the reactor under stirring 800kg (5.82mol) phosphorus trichloride (that is, the molar ratio of benzene, phosphorus trichloride and aluminum trichloride is 1:1:1), slowly heat up to 120°C, react for 12h; turn off the heating and cool down to 60°C; then Add 625 kg (4.66 mol) of decomplexing agent triethylphosphine oxide to the reactor in batches, wherein the molar percentage of decomplexing agent is 80% of phosphorus trichloride, raise the temperature to 80° C. and stir for 2 hours. Rectification isolates monophenylphosphine dichloride and diphenylphosphine chloride products, and the yield of product is 75%, and purity is 99.1%; Rectification condition is: under the condition of high vacuum (-0.1MPa), Gradually raise the tem...

Embodiment 2

[0022] Embodiment 2 The preparation method of a kind of diphenylphosphine chloride of the present invention comprises the following steps: 455kg (5.82mol) of benzene and 777kg (5.82mol) of aluminum trichloride are dropped into the reactor, and are added into the reactor under stirring 800kg (5.82mol) of phosphorus trichloride (that is, the molar ratio of benzene, phosphorus trichloride and aluminum trichloride is 1:1:1), slowly heated up to 120°C, and reacted for 12 hours. Turn off the heating and cool down to 60°C; then add a decomplexing agent in batches to the reactor, namely 600kg of reclaimed triethylphosphine oxide and new 60kg triethylphosphine oxide, the molar percentage of the decomplexing agent being that of phosphorus trichloride 85%, the ratio between recovered triethylphosphine oxide and new triethylphosphine oxide is 10:1, heat up to 80°C and stir for 2 hours; rectify and separate monophenylphosphine dichloride and diphenylchloride Phosphine product, the yield of...

Embodiment 3

[0023] Embodiment 3 The preparation method of a kind of diphenylphosphine chloride of the present invention comprises the following steps: 455kg (5.82mol) of benzene and 777kg (5.82mol) of aluminum trichloride are dropped into the reactor, and are added into the reactor under stirring 800kg (5.82mol) of phosphorus trichloride (that is, the molar ratio of benzene, phosphorus trichloride and aluminum trichloride is 1:1:1), slowly heated up to 120°C, and reacted for 12 hours. Turn off the heating and cool down to 60°C; then add a decomplexer in batches to the reactor, i.e. 642kg triethylphosphine oxide and new 60kg triethylphosphine oxide recovered in Example 2, the molar percentage of the decomplexer is three 90% of phosphorus chloride, the ratio between the recovered triethylphosphine oxide and the new triethylphosphine oxide is 10.7:1, the temperature is raised to 80°C and stirred for 2 hours; Phenylphosphine chloride product, the yield of the product is 72%, and the purity is...

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PUM

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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...

Claims

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Application Information

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IPC IPC(8): C07F9/52
CPCC07F9/52
Inventor 何子健
Owner 江苏多森新材料科技有限公司
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