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Thermal condensation production method for phenyl chlorosilane

A technology of phenylchlorosilane and a production method, which is applied in the field of production technology of phenylchlorosilane, can solve the problems of low production efficiency, material punching or explosion, stay and the like, and achieves the advantages of reducing energy consumption, reducing pollution and reducing reaction temperature. Effect

Inactive Publication Date: 2012-05-09
ZHEJIANG KAIHUA SYNTHETIC MATERIAL
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The process is simple and the raw materials are easy to obtain; its disadvantages are: the preparation process of the formatted reagent has high requirements, and sometimes improper control during the reaction process may easily cause punching or explosion; the by-product magnesium chloride and solvent treatment are more complicated; the production efficiency is low; With the emergence of the direct method, the format method has basically been eliminated
Its disadvantages: the amount of catalyst copper is 30-50% (mass ratio) of the amount of silicon powder, and the amount of catalyst is relatively large; the by-products contain polychlorinated biphenyls, which are highly toxic and carcinogenic
However, the current technology only stays in the small test stage, and it is difficult to form large-scale industrial production

Method used

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  • Thermal condensation production method for phenyl chlorosilane
  • Thermal condensation production method for phenyl chlorosilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Such as figure 1 As shown, the process flow for preparing phenylchlorosilane is as described in the figure above. Specific steps are as follows:

[0019] step one:

[0020] Synthetic reaction: using raw materials chlorobenzene and trichlorosilane as raw materials, the ratio of the two is 0.7:1 in the molar ratio of chlorobenzene and trichlorosilane, and at the same time under the action of the initiator dibenzoyl peroxide, The temperature is controlled at 300-350°C and the pressure is 0.2-0.8Mpa to carry out the reaction. The amount of initiator dibenzoyl peroxide is 0.1%wt of the total amount of material. The reaction produces phenylchlorosilane mixed monomers.

[0021] Its reaction principle is:

[0022] C 6 h 5 Cl+HSiCl 3 →C 6 h 5 SiCl 3 +HCl(1)

[0023] C 6 h 5 Cl+HSiCl 3 →C 6 h 6 + SiCl 4 (2)

[0024] Step two:

[0025] Condensation of syngas: Use suitable refrigerant (air, circulating water, water at 0°C) to condense syngas to greatly reduce ...

Embodiment 2

[0031] Such as figure 1 As shown, the process flow for preparing phenylchlorosilane is as described in the figure above. Specific steps are as follows:

[0032] step one:

[0033] Synthesis reaction: use chlorobenzene and methyldichlorosilane as raw materials, the ratio of the two is 0.8:1 molar ratio of chlorobenzene and methyldichlorosilane, and at the same time, under the action of the initiator azobisisobutyronitrile Under the control temperature of 350-400°C and the pressure of 0.2-0.8Mpa, the reaction is carried out. The amount of initiator azobisisobutyronitrile is 1.05%wt of the total amount of material. The reaction produces phenylchlorosilane mixed monomers.

[0034] Its reaction principle is:

[0035] C 6 h 5 Cl+HSiCl 3 →C 6 h 5 SiCl 3 +HCl(1)

[0036] C 6 h 5 Cl+HSiCl 3 →C 6 h 6 + SiCl 4 (2)

[0037] Step two:

[0038] Condensation of syngas: Use suitable refrigerant (air, circulating water, water at 0°C) to condense syngas to greatly reduce e...

Embodiment 3

[0044] Such as figure 1 As shown, the process flow for preparing phenylchlorosilane is as described in the figure above. Specific steps are as follows:

[0045] step one:

[0046] Synthetic reaction: use raw materials chlorobenzene and trichlorosilane as raw materials, the ratio of the two is 0.8:1 molar ratio of chlorobenzene and trichlorosilane, and at the same time, under the action of initiator potassium persulfate, the temperature is controlled at React at 400-500°C and pressure 0.2-0.8Mpa. The amount of initiator potassium persulfate is 1.2%wt of the total amount of material. The reaction produces phenylchlorosilane mixed monomers.

[0047] Its reaction principle is:

[0048] C 6 h 5 Cl+HSiCl 3 →C 6 h 5 SiCl 3 +HCl(1)

[0049] C 6 h 5 Cl+HSiCl 3 →C 6 h 6 + SiCl 4 (2)

[0050] Step two:

[0051] Condensation of syngas: Use suitable refrigerant (air, circulating water, water at 0°C) to condense syngas to greatly reduce energy consumption; use three-stag...

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Abstract

The invention discloses a thermal condensation production method for a phenyl chlorosilane; with chlorobenzene and trichlorosilane as raw materials or with chlorobenzene and methyl dichloresilane as raw materials, in the action of an initiator, the raw materials are reacted in a reactor to produce synthetic phenyl chlorosilane gas under the conditions of controlling the temperature to be 300-600 DEG C and the pressure to be 0.2-0.8 MPa; the molar ratio of the chlorobenzene and the trichlorosilane in the raw materials is 0.7: 1 to 1:1; and the molar ratio of the chlorobenzene and the methyl dichloresilane in the raw materials is 0.7:1 to 1:1. The initiator is one of trichloromethane, potassium peroxydisulfate, azodiisobutyronitrile and dibenzoyl peroxide; and the dosage of the initiator is 0.1-2% wt of the total amount of the materials. The thermal condensation production method for the phenyl chlorosilane disclosed by the invention has simple equipment and is high in reaction efficiency, low in cost and easy to form industrial production.

Description

technical field [0001] The invention belongs to the field of chemical technology, and in particular relates to a production technology of phenylchlorosilane. Background technique [0002] At present, there are three methods for producing phenylchlorosilane, which are format method, direct method and condensation method (refer to "Organosilicon Synthesis Process and Product Application" written by Xing Songmin). [0003] Method 1: format method. Using chlorobenzene and trichlorosilane or methyl dichlorosilane as raw materials, using Grignard reagent as catalyst, adding a certain amount of solvent, and controlling a certain temperature and pressure to produce phenylchlorosilane products. The process is simple and the raw materials are easy to obtain; its disadvantages are: the preparation process of the formatted reagent has high requirements, and sometimes improper control during the reaction process may easily cause punching or explosion; the by-product magnesium chloride a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/12
Inventor 魏涛廖端友汪玉林郑云峰
Owner ZHEJIANG KAIHUA SYNTHETIC MATERIAL
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