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Method of preparing dimethyl dichloro silicane using organic silicon high boiling point substance

A technology of dimethyldichlorosilane and methylchlorosilane, which is applied in the field of preparing dimethyldichlorosilane by using organosilicon high boilers, can solve the problems of certain difficulty in industrialization, high reactor cost, and high reaction temperature. Achieve the effect of outstanding technical indicators, simple process and high safety

Inactive Publication Date: 2005-03-09
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Aluminum trichloride can be recycled, but the reaction temperature is high
[0016] Aluminum trichloride Hydrogen chloride 10~27% M 2 Low selectivity, high reactor cost (nickel,
[0022] The operating temperature is high, and industrialization is difficult

Method used

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  • Method of preparing dimethyl dichloro silicane using organic silicon high boiling point substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] High boilers (see table for composition) are added to the tower still type cracking reactor at a speed of 40g / h, the hydrogen chloride feed rate is 75ml / min, and the tri-n-butylamine consumption in the gas preheater is the total amount of high boiler monomers 1%, the reaction temperature is 125-130°C, the temperature in the rectification section is 140±2°C, the temperature in the stripping section is 85°C, and it operates under normal pressure. The top product is 43-47g / h, the reaction is carried out for 50h, and the conversion rate is 91.62%. The composition of the lysate is shown in Table 3.

[0055] Table 3 Product Gas Chromatography Analysis

[0056] MeHSiCl 2 MeSiCl 3 Me 2 SiCl 2

[0057] 1~10h 38.18 16.05 42.71

[0058] 11~20h 44.59 20.26 32.66

[0059] 21~30h 43.97 21.20 29.87

[0060] 31~40h 39.00 16.85 41.30

[0061] 41~50h 26.59 26.85 43.45

[0062] 1~50h 39.79 21.03 36.93

Embodiment 2

[0064] The reaction process is the same as in Example 1, the amount of tri-n-butylamine is 1.5% of the total amount of high boiler monomers, the overhead product is 45-48g / h, the reaction is carried out for 50h, and the conversion rate is 92.9%. The composition of the cleavage product is shown in Table 4.

[0065] Table 4 Product Gas Chromatography Analysis

[0066] Reaction time MeHSiCl 2 MeSiCl 3 Me 2 SiCl 2

[0067] 1~10h 38.66 7.84 48.78

[0068] 11~20h 32.56 7.54 56.43

[0069] 21~30h 31.19 27.34 38.43

[0070] 31~40h 19.24 31.11 45.71

[0071] 41~50h 15.66 40.61 40.32

[0072] 1~50h 29.44 20.32 46.41

Embodiment 3

[0074] The reaction process is the same as in Example 2, using methyl chloride as a catalyst, the overhead product is 28-32g / h, the reaction is carried out for 50h, and the conversion rate is 70.47%. The composition of the cleavage product is shown in Table 5.

[0075] Table 5 Product Gas Chromatography Analysis

[0076] Reaction time MeCl 3 MeSiCl 3 Me 2 SiCl 2 high boiler

[0077] 1~10h 5.39 25.31 56.42 11.18

[0078] 11~20h 6.20 34.69 49.93 8.39

[0079] 21~30h 6.02 31.26 54.38 10.28

[0080] 31~40h 5.48 28.79 47.61 9.97

[0081] 41~50h 6.51 29.98 53.19 11.06

[0082] 1~50h 5.78 30.06 52.68 10.01

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Abstract

A process for preparing dimethyl dichlorosilane from the high-boiling-point residue generated in synthesizing methyl chlorosilane includes filling catalyst in gas preheater, passing chloromethane (or hydrogen chloride) gas through it, carrying catalyst into reactor while introducing said residue to it, and separating dimethyl dichlorosilane from the cooled substance at tower top.

Description

technical field [0001] The invention relates to a method for preparing dimethyldichlorosilane from a high-boiling residue of organic silicon through a gas-liquid phase cracking reaction and improving its selectivity. Background technique [0002] Organosilicon high boiling point residue (high boiling point) refers to the high boiling point polysilane with a boiling range of 80-215 °C produced during the synthesis of methyl chlorosilane monomer, mainly composed of silicon-silicon bonds and silicon-carbon-silicon bonds. mixture. With the continuous expansion of the production scale of methyl chlorosilane monomer, the utilization of high boilers accounting for 5% of the monomer composition is becoming more and more important. At present, domestic high boiling substances are mainly used for the production of silicone waterproofing agents and defoaming agents. The market capacity is limited, and only about one-fifth of high boiling substances can be used ...

Claims

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Application Information

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IPC IPC(8): C07F7/12
Inventor 王刚王明成
Owner PETROCHINA CO LTD
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