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New synthesizing method of chlorodiphenylphosphine

A technology of diphenylphosphine chloride and phenylphosphine dichloride, which is applied in the synthesis field of diphenylphosphine chloride, can solve the problems of environmental protection, product yield and purity need to be improved, and high cost, and can speed up the reaction rate , The effect of simplifying production operation and low cost

Inactive Publication Date: 2019-04-05
刘碧见
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method removes the hydrolysis process and directly converts the raw material into diphenylphosphine chloride by one-step disproportionation, which can improve the utilization rate of the raw material and the yield of the product to a certain extent, but because a large amount of by-product table salt and salt will be generated in the reaction process slag, the yield and purity of the product still need to be improved. In addition, the use of organic solvents and catalysts makes this method still have high cost and environmental protection problems

Method used

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  • New synthesizing method of chlorodiphenylphosphine
  • New synthesizing method of chlorodiphenylphosphine

Examples

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Effect test

Embodiment 1

[0027] A new synthetic method of diphenylphosphine chloride, comprising the following steps:

[0028] (1) Raw material preparation: add 13 mol chlorobenzene to the gasification tank with the temperature set at 290°C to vaporize the chlorobenzene for later use; add 2 mol chlorobenzene and 1 mol phosphorus to the mixing tank with the temperature set at 125°C to make them fully mixed Get the mixture and set aside;

[0029] (2) Reaction in the tubular reactor: the gasified chlorobenzene is introduced into the tubular reactor, and the flow rate is controlled by a gas flow meter so that the flow rate of gaseous chlorobenzene in the tubular reactor is 4L / min, and the gaseous chlorine The residence time of benzene in the tubular reactor is 8s, and the mixed solution is injected into the tubular reactor with a metering pump, and the flow rate is controlled by a liquid flow meter so that the flow rate of the mixed solution in the tubular reactor is 4ml / min. The residence time of the mi...

Embodiment 2

[0033] A new synthetic method of diphenylphosphine chloride, comprising the following steps:

[0034] (1) Raw material preparation: add 4mol chlorobenzene to the gasification tank with the temperature set at 280°C to vaporize the chlorobenzene for later use; add 1mol chlorobenzene and 1mol phosphorus to the mixing tank with the temperature set at 120°C to make them fully mixed Get the mixture and set aside;

[0035] (2) Reaction in the tubular reactor: the gasified chlorobenzene is introduced into the tubular reactor, and the flow rate is controlled by a gas flow meter so that the flow rate of gaseous chlorobenzene in the tubular reactor is 3L / min, and the gaseous chlorine The residence time of benzene in the tubular reactor is 5s, and the mixed solution is pumped into the tubular reactor with a metering pump, and the flow rate is controlled by a liquid flow meter so that the flow rate of the mixed solution in the tubular reactor is 2ml / min. The residence time of the mixed so...

Embodiment 3

[0038] A new synthetic method of diphenylphosphine chloride, comprising the following steps:

[0039] (1) Raw material preparation: add 20mol chlorobenzene to the gasification tank with the temperature set at 300°C to vaporize the chlorobenzene for later use; add 5mol chlorobenzene and 1mol phosphorus to the mixing tank with the temperature set at 130°C to make them fully mixed Get the mixture and set aside;

[0040] (2) Reaction in the tubular reactor: the gasified chlorobenzene is introduced into the tubular reactor, and the flow rate is controlled by a gas flow meter so that the flow rate of gaseous chlorobenzene in the tubular reactor is 7L / min, and the gaseous chlorine The residence time of benzene in the tubular reactor is 10s, and the mixed solution is injected into the tubular reactor with a metering pump, and the flow rate is controlled by a liquid flow meter so that the flow rate of the mixed solution in the tubular reactor is 6ml / min. The residence time of the mixt...

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Abstract

The invention discloses a new synthesizing method of chlorodiphenylphosphine and belongs to the field of synthesizing technology. The method comprises the following steps of filling chlorobenzene intoa gasification tank for gasification, then uniformly mixing chlorobenzene and phosphorous into a mixing tank to obtain a mixed solution; guiding the gasified chlorobenzene into a tubular reactor, pumping the mixed solution into the tubular reactor through a metering pump for normal-temperature contact reaction between the chlorobenzene and the phosphorous in the tubular reactor at 580-610 DEG C;condensing and crudely distilling the reacted materials to separate chlorobenzene, chlorophenylphosphine and chlorodiphenylphosphine; recycling the separated chlorobenzene, and performing reduced pressure rectification on the mixture of the chlorophenylphosphine and the chlorodiphenylphosphine to obtain the products of chlorodiphenylphosphine and the chlorophenylphosphine. The new synthesizing method of the chlorodiphenylphosphine achieves continuous reaction and simple operation with a raw material utilization rate up to 100%, saves solvent and catalyst and is high in yield and purity of products.

Description

technical field [0001] The invention relates to a synthesis method of diphenylphosphine chloride, which belongs to the technical field of synthesis. Background technique [0002] Diphenylphosphine chloride is a kind of important organophosphorus chemical product at present, can be used for producing photoinitiator TPO, diphenylphosphine oxide, catalyst etc. industrially. At present, the traditional synthetic method of diphenylphosphine chloride is to take benzene and phosphorus trichloride as raw materials, react under the catalysis of anhydrous aluminum trichloride, and the diphenylphosphine chloride generated is complexed with aluminum trichloride, Diphenylphosphine chloride is dissociated by adding phosphorus oxychloride, dioxane, crushed sodium chloride or potassium chloride and reacting with aluminum chloride. This kind method needs to consume a large amount of raw materials and catalyst, and the utilization ratio of raw materials is low, and the decomplexation process...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/52
CPCC07F9/52
Inventor 李坤武
Owner 刘碧见
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