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Process for synthesizing (CH3)2 SiCl2 by utilizing CH3 SiCl2

A CH3, alkylation technology, applied in chemical instruments and methods, compounds of Group 4/14 elements of the periodic table, organic chemistry, etc., can solve the problems of low yield, poor safety, large amount of catalyst, etc. The effect of good safety, full and reasonable utilization, and easy control

Inactive Publication Date: 2004-01-07
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0021] The problem with this method is that the amount of catalyst required for the reaction is very large, generally 10%-20% of the reactant;
[0029] (1) The conversion rate of the alkylation reaction between monomethyltrichlorosilane and methyl chloride and the yield of the target product are all low, CH 3 SiCl 3 Conversion rate is generally between 20-40%, (CH 3 ) 2 SiCl 2 The yield is generally between 10-40%, and the reaction is not easy to control, etc.
[0030] (2) The low-pressure disproportionation reaction of monomethyltrichlorosilane is also difficult to control, and the yield is low, generally below 20%.
[0031] (3) Although the high-pressure disproportionation reaction has a high yield, which can reach 40%, the requirements for the reaction equipment are relatively harsh and the safety is poor

Method used

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  • Process for synthesizing (CH3)2 SiCl2 by utilizing CH3 SiCl2

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0041] Add 1KgAl ball into the stirred bed reactor, stir, pass N 2 Raise the temperature to 240-260°C, and feed CH into the reactor 3 SiCl 3 and CH 3 Cl, CH 3 SiCl 3 :CH 3 Cl=1:1:(mol), control the reaction temperature at 240-300°C, and stop passing CH after 4 hours of reaction 3 SiCl 3 and CH 3 Cl, through N 2 Cool down, when down to room temperature, get liquid sample and analyze by gas chromatography, its composition is 49.7% (CH 3 ) 2 SiCl 2 and 8.9% (CH 3 ) 3 SiCl. CH 3 SiCl 3 Conversion rate is 67.2%, (CH 3 ) 2 SiCl 2 and (CH 3 ) 3 The total yield of SiCl per pass is 58.6%. Example two:

example 2

[0042] Reaction method is the same as Example 1, CH 3 SiCl 3 :CH 3 Cl=1: 1: (mol), Al: 1Kg, NaCl: 500g, the reaction time is 4 hours, and the liquid product of gained is analyzed by gas chromatography, and its composition is 38.2% (CH 3 ) 2 SiCl 2 and 17.5% (CH 3 ) 3 SiCl. CH 3 SiCl 3 Conversion rate is 65.2%, (CH 3 ) 2 SiCl 2 and (CH 3 ) 3 The total yield of SiCl per pass is 60.1%. Example three:

example 3

[0043] Reaction method is the same as Example 1, CH 3 SiCl 3 :CH 3 Cl=1: 0.6 (mol), the reaction time is 4 hours, and the liquid product of gained is analyzed by gas chromatography, and its composition is 40.6% (CH 3 ) 2 SiCl 2 and 2.4% (CH 3 ) 3 SiCl. CH 3 SiCl 3 Conversion rate is 58.7%, (CH 3 ) 2 SiCl 2 and (CH 3 ) 3 The total yield of SiCl per pass is 50.4%. Example four:

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PUM

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Abstract

The method for synthesizing (CH3)2SiCl2 by utilizing CH3SiCl2 uses methyl trichlorosilane whose purity is greater than 99% and chloromethane whose purity is greater than 98% as raw material, makes them produce gas-phase alkylation reaction, adopts spherical aluminium catalyst whose purity is greater than or equal to 97%, and whose average grain size is 1 mm, and its reactant composite CH3SiCl3:CH3Cl=1:1-1:0.4(mol), controlled reaction temp. is 200-300 deg.C, reaction time is 4-5 hr., CH3SiCl3 conversion rate can be up to above 50%, and per pass total yield rate of (CH3)2SiCl2 and (CH3)3SiCl2 can be up to above 50%.

Description

[0001] Involved areas: [0002] The present invention relates to the synthesis of dimethyldichlorosilane {(CH 3 ) 2 SiCl 2} and trimethylchlorosilane ((CH 3 ) 3 SiCl) method. Background technique: [0003] CH 3 SiCl 3 Can be produced by alkylation (CH 3 ) 2 SiCl 2 , the alkylation reaction generally uses an organoaluminum compound as a catalyst [1] , organoaluminum compounds have a history of more than 100 years, but it was used to synthesize organochlorosilanes after 1983, that is, V.Hnizda (V.Hnizda) and Claus (E.Krans) found that metal aluminum can It starts after directly reacting with halogenated hydrocarbons to form hydrocarbyl aluminum halides. In the 1950s, because Ziegler (K.Ziegler) proposed the industrial production method of alkylaluminum, the development of organosilane synthesis by organoaluminum method was more effectively promoted. The synthesis of organosilane by organoaluminum method can be represented by the following general formula: [0004] ...

Claims

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Application Information

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IPC IPC(8): C07F7/12
Inventor 齐姝婧张国良金美仙李洪福殷绪明张月霞许荣王梅
Owner PETROCHINA CO LTD
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