Preparation method for benzyltriphenylphospho

A technology of benzyl triphenyl phosphine chloride and triphenyl phosphine is applied in the preparation of fluororubber cross-linking accelerator and the preparation field of benzyl triphenyl phosphine chloride, which can solve the problem of hazardous solid waste polluting the environment, Difficulty separating products from raw materials, solvent and benzyl chloride escape, etc., to achieve the effects of improving production and operation environment, shortening reaction time, and low product cost

Active Publication Date: 2019-06-21
自贡天龙化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, its main synthesis method is mainly the direct synthesis method of benzyltriphenylphosphine chloride in an organic solvent. This method reacts violently and easily causes the dissipation of solvent and benzyl chloride. It is difficult to separate the product from the raw material and requires multiple recrystallizations to improve purity, produce hazardous solid waste to pollute the environment, and have the disadvantages of high energy consumption and low yield
A utility model patent CN201621275573.6 discloses a reflux device for benzyltriphenylphosphorous chloride. The setting of the reflux box can effectively alleviate the problem of excessive steam in the reactor and cause excessive pressure inside the reactor, but for Other issues in react but not resolved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A preparation method of benzyltriphenylphosphine chloride, which comprises the following steps:

[0031] In a 1000L enamel reactor with a jacket heating and a low-temperature cooling return pipe, initially charge 400.0 kg of water (recycled mother liquor) and 200.0 kg of benzyl chloride (excess 314%); start stirring, jacket heating, and After the solution temperature in the kettle was heated to 85°C, the jacket stopped heating. Then start to add a total of 100.0 kg granular triphenylphosphine, add slowly through a vibrating feeder, rapidly dissolve and react to release heat, and the water phase reflux controls the temperature in the kettle to generate benzyltriphenylphosphine chloride. The total addition time is about 60 minute. For complete conversion, turn on the jacket to heat, keep the liquid temperature in the reactor at 80-85°C and continue to stir for 30 minutes, then stop stirring and continue to keep the liquid temperature in the kettle at 80-85°C for 30 minut...

Embodiment 2

[0033]Adopt the same method as Example 1 to carry out the preparation of benzyltriphenylphosphine chloride, the difference is that the amount of initially metered water is 500 kg (recycled mother liquor). After the specified reaction process and conditions in Example 1, 144.86 kilograms of finished products were obtained from the reaction, and the yield of the benzyltriphenylphosphine chloride product was 98.08%, and the purity was 99.61%.

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Abstract

The invention belongs to the technical field of fine chemical engineering, and specifically discloses a preparation method for benzyltriphenylphospho. The preparation method comprises the following steps: performing reflux reaction by utilizing reaction exotherm at a certain initial temperature in a mixed solution of water and benzyl chloride by taking triphenylphosphine and the benzyl chloride asraw materials; allowing standing still for layering, preserving heat and separating liquid, performing micro-membrane filtering, cooling and crystallizing, performing centrifugal separation and performing vacuum drying to obtain the benzyltriphenylphospho. The preparation method provided by the invention is simple in process, quick in reaction, mild in conditions, high in purity and high in yield. According to the preparation method, the water serving as the solvent and excessive benzyl chloride are recycled for utilizing; the reaction is accelerated by utilizing the reaction exotherm, so that energy conservation and emission reduction are realized; the cost is reduced; industrial production is facilitated better. The content of the benzyltriphenylphospho synthesized by the preparation method is 99% or higher, and the reaction yield is up to 98%.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and relates to a preparation process of a fluororubber crosslinking accelerator, in particular to a preparation method of benzyltriphenylphosphine chloride. Background technique [0002] Benzyltriphenylphosphine chloride is an organic chemical substance, mainly used as a fluorine rubber vulcanization accelerator, a phase transfer catalyst, and can also be used as an intermediate in medicine and organic synthesis. In recent years, its new uses are constantly being developed, and its demand is also increasing year by year. [0003] At present, its main synthesis method is mainly the direct synthesis method of benzyltriphenylphosphine chloride in an organic solvent. This method reacts violently and easily causes the dissipation of solvent and benzyl chloride. It is difficult to separate the product from the raw material and requires multiple recrystallizations to improve purity, produce ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/54
CPCY02P20/10
Inventor 黄勇程大军程杰
Owner 自贡天龙化工有限公司
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