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Raw material components and production method of diphenyl phosphorus chloride

A technology of diphenylphosphorus chloride and production method, which is applied in chemical instruments and methods, organic chemistry, compounds of Group 5/15 elements of the periodic table, etc. Long time and other problems, to achieve the effect of reducing raw material consumption, shortening reaction time, and reducing the discharge of three wastes

Inactive Publication Date: 2009-07-15
ZHAOYUAN SONGHE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] A large amount of aluminum trichloride is used in the reaction process, which causes environmental pollution. In addition, the post-processing of the product is difficult, and it is not easy to filter, which causes difficulties in large-scale industrial production. The product yield is low, the cost is high, and the reaction time is long.

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  • Raw material components and production method of diphenyl phosphorus chloride
  • Raw material components and production method of diphenyl phosphorus chloride

Examples

Experimental program
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Embodiment 1

[0027] The raw material component of a kind of diphenylphosphorus chloride of this embodiment, comprises the halide of active metal, benzene, phosphorus trichloride, organic solvent, catalyst, wherein by mass parts, active metal sodium 0.8 part, benzene 1 part of halide, 1 part of phosphorus trichloride, 1 part of organic solvent, 0.03 part of catalyst;

[0028] The production method of present embodiment diphenyl phosphorus chloride is as follows:

[0029] In the production method of the following examples, take the example of active metal sodium, benzene halide chlorobenzene, organic solvent xylene, and catalyst aluminum trichloride;

[0030] 1. Under the protection conditions of anhydrous, anaerobic and nitrogen, put 1 part of xylene and 0.8 part of metal sodium into the dispersion kettle according to the mass parts, close the pot mouth, open the jacket and steam to 90-130 ℃, stir and disperse sodium metal at 300-2500 rpm for 2-40 minutes to disperse the sodium into partic...

Embodiment 2

[0037] Embodiment 2 The difference between a kind of diphenyl phosphorus chloride of this embodiment and embodiment 1 is that,

[0038] The raw material component of a kind of diphenylphosphorous chloride of this embodiment, comprises the halide of active metal, benzene, phosphorus trichloride, organic solvent, catalyst, wherein according to mass parts, active metal 1.5 parts, halogenated benzene 4 parts of compound, 3 parts of phosphorus trichloride, 8 parts of organic solvent, 0.1 part of catalyst;

[0039] The difference between the production method of the present embodiment diphenyl phosphorus chloride and embodiment 1 is,

[0040] 1. Under the protection conditions of anhydrous, oxygen and nitrogen, mix 8 parts of xylene and 1.5 parts of sodium metal into the dispersion kettle according to the mass parts, heat to 90-130 ℃, and use 300-2500 rpm Stir and disperse the sodium metal at a high stirring speed for 2 to 40 minutes to disperse the sodium into particles below 120 ...

Embodiment 3

[0044] Embodiment 3: The difference between a kind of diphenyl phosphorus chloride of the present embodiment and embodiment 1 is,

[0045] The raw material component of a kind of diphenylphosphorous chloride of this embodiment, comprises the halide of active metal, benzene, phosphorus trichloride, organic solvent, catalyst, wherein according to mass parts, active metal 1.0 parts, halogenated benzene 2 parts of compound, 1.5 parts of phosphorus trichloride, 2 parts of organic solvent, 0.05 part of catalyst;

[0046] The difference between the production method of the present embodiment diphenyl phosphorus chloride and embodiment 1 is,

[0047] 1. Under the protection conditions of anhydrous, oxygen and nitrogen, mix 2 parts of xylene and 1.0 part of metal sodium into the dispersion kettle according to the mass parts, heat to 90-130 ℃, and use 300-2500 rpm Stir and disperse the sodium metal at a high stirring speed for 2 to 40 minutes to disperse the sodium into particles below...

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Abstract

The invention relates to raw material components and a production method of chlorodiphenylphosphine, and belongs to the technical field of chemical product formulas and production methods. Based on mass part, the raw material components are as follows: 0.8-1.5 parts of an active metal, 1-4 parts of benzene halide, 1-3 parts of phosphorus trichloride, 1-8 parts of an organic solvent and 0.03-0.1 part of a catalyst. The production method comprises the following steps: 1. mixing and adding the organic solvent and the active metal to a dispersing kettle based on the mass part, heating and stirring to disperse the active metal, and adding the benzene halide for a first initiation; 2. cooling the materials after dispersion, adding the same amount of the benzene halide for a second initiation, cooling and adding the remaining benzene halide and the phosphorus trichloride; 3. allowing reaction, adding the catalyst, and heating for reaction; 4. filtering through a press filter cone when the materials are hot; and 5. putting the filter pressed materials in a rectifying still and stirring, distilling off the solvent at normal pressure, rectifying a finished chlorodiphenylphosphine product at negative pressure, checking and packaging. The raw material components and the production method have the advantages of 1. shortening the reaction time, reducing the side reaction and improving the yield; and 2. avoiding a hydrolysis procedure, eliminating sewage discharge and reducing the raw material consumption.

Description

1. Technical field [0001] The invention relates to a raw material component and a production method of diphenylphosphorous chloride, and belongs to the technical field of chemical product formulations and production methods. 2. Background technology [0002] The prior art diphenyl phosphorus chloride production method is that benzene and phosphorus trichloride are synthesized under the catalysis of aluminum trichloride: [0003] 2C 6 h 6 +PCl 3 +AlCl 3 ----→Ph 2 PCl+2HCl [0004] A large amount of aluminum trichloride is used in the reaction process, causing environmental pollution. In addition, the post-processing of the product is difficult, and it is not easy to filter, which causes difficulties in large-scale industrial production. The product yield is low, the cost is high, and the reaction time is long. 3. Contents of the invention [0005] The object of the present invention is to overcome the defect that the above-mentioned prior art diphenylphosphorous chlor...

Claims

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Application Information

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IPC IPC(8): C07F9/52
Inventor 孙登利王春玉宫生铭孙胜文
Owner ZHAOYUAN SONGHE CHEM
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