Method for disproportionating methyl chlorosilane

A technology of methyl chlorosilane and methyl trichlorosilane, applied in the field of methyl chlorosilane disproportionation, can solve the problems of high reaction temperature and pressure, difficult separation, increased trimethyl output, etc., and achieves easy control of conditions and high conversion rate of raw materials , good catalytic activity

Inactive Publication Date: 2011-08-03
JIANGSU UNIV
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AI Technical Summary

Problems solved by technology

Since methylchlorosilane is a polar compound containing chlorine atoms, it is very easy to react with moisture in the air during storage and discharge to produce corrosive gases such as hydrogen chloride, which poses a great safety hazard and causes environmental pollution.
At present, China mainly uses Yijia to prepare low-end products such as silane crosslinking agent, methyl silicone resin and waterproofing agent, but these products are of low value and the market demand is limited, which is not enough to form a large-scale treatment of Yijia
[0003] Dimethyl is the main raw material in the silicone industry, with a wide range of uses and a large market demand. In addition, it also has a certain demand as a polymeric silane protective agent. S

Method used

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  • Method for disproportionating methyl chlorosilane
  • Method for disproportionating methyl chlorosilane
  • Method for disproportionating methyl chlorosilane

Examples

Experimental program
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Effect test

Example Embodiment

[0030] Preparation of chloroaluminate ionic liquid catalyst

[0031] N -Butylpyridine chloroaluminate [BPy]Cl-nAlCl 3 (n=2-6) Preparation method of ionic liquid: under the protection of nitrogen, 1.50 mol (119 g) pyridine and 1.7 mol (158 g) chloro-n-butane are placed in a 500 mL three-necked flask with reflux condenser. Stir and mix well, warm up to 100 ℃ in the dark, and cause gentle reflux, and react at this temperature for 72 h. Stop heating, cool to below 10 ℃, white crystals precipitated, suction filter and wash the crude product with ethyl acetate, the product was vacuum dried at 70 ℃ for 48 h to remove residual ethyl acetate. The yield of [BPy]Cl is about 55%, and it should be stored in a dry inert atmosphere for later use.

[0032] Fill the glove box with nitrogen, and slowly add different amounts of anhydrous AlCl to the quantitative above intermediate [BPy]Cl at room temperature. 3 During the feeding process, keep stirring to avoid local high temperature until the soli...

Example Embodiment

[0033] Example 1:

[0034] The disproportionation reaction of methyltrichlorosilane and low boilers to prepare dimethyldichlorosilane:

[0035] In the autoclave, add methyltrichlorosilane and low-boiling substances with a mass ratio of 1.5:1, a total of 150 g of the reaction mixture and 16.7% (25 g) aluminum trichloride and chlorination N -Butylpyridine molar ratio 6:1 N -Butylpyridine chloroaluminate is [BPy]Cl-6AlCl 3 Ionic liquid catalyst, sealed, introduced nitrogen to replace the air in the kettle, kept fully stirring (500 rpm), heated to 150 ℃, and reacted for 5 h. After the reaction is over, after the temperature of the reactor is lowered to room temperature, the reaction product is taken out, the product is separated from the ionic liquid, and then the product is sampled and the product composition is immediately analyzed by gas chromatography.

[0036] The gas chromatography analysis conditions are:

[0037] Chromatographic column: OV-1701 capillary column; detector type; F...

Example Embodiment

[0045] Example 2

[0046] Same as Example 1, but keeping the mass ratio of methyl trichlorosilane and low boiling substance at 1.5:1, only changing the aluminum trichloride and chlorination in the ionic liquid N -The molar ratio of butylpyridine is 2:1, 3:1, 4:1, 5:1, and the results are shown in image 3 .

[0047] by image 3 It can be seen that with [BPy]Cl-nAlCl 3 AlCl in ionic liquid catalyst 3 With the continuous increase of the molar ratio of [BPy]Cl, the conversion rate of tetramethylsilane in low boilers increased rapidly to 100%, and the conversion rate of methyltrichlorosilane and the yield of dimethyldichlorosilane showed a significant increase trend . When AlCl 3 When the molar ratio of [BPy]Cl is 6:1, the conversion rate of methyltrichlorosilane reaches 88.21%, the yield of dimethyldichlorosilane reaches 69.40%; the yield of trimethylchlorosilane is Continuous decline. Therefore, increase [BPy]Cl-nAlCl 3 AlCl in ionic liquid catalyst 3 The content has a significant...

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Abstract

The invention relates to a method for disproportionating methyl chlorosilane, belonging to the field of ion liquid catalysis, and discloses a method for preparing dimethyl dichlorosilane or trimethyl chlorosilane by catalyzing the disproportionating reaction between methyl trichlorosilane and a low-boiling-point substance with N-butyl pyridine chloroaluminate ionic liquid serving as a catalyst. The method for catalyzing the disproportionating reaction between the methyl trichlorosilane and the low-boiling-point substance has the advantages of simple and convenient process, high raw material conversion ratio, high product yield, low reaction temperature, short time, easily-controlled condition, catalyst reusability realized by simple liquid separation, and the like.

Description

technical field [0001] The invention relates to a method for the disproportionation reaction of by-product methyltrichlorosilane and low boilers in the process of producing dimethyldichlorosilane monomer by "direct method", specifically referring to: 1. using N -Butylpyridinechloroaluminate[BPy]Cl-nAlCl 3 (n=2-6) The ionic liquid is used as a catalyst to catalyze the disproportionation reaction of methyltrichlorosilane and low boilers to prepare dimethyldichlorosilane; 2. use N -Butylpyridinechloroaluminate[BPy]Cl-nAlCl 3 (n=1.5-3) A new method for preparing trimethylchlorosilane by catalyzing the disproportionation reaction of methyltrichlorosilane and low boilers with ionic liquid as catalyst. Background technique [0002] In the process of Rochow's direct synthesis of methylchlorosilane monomers, in addition to the target product dimethyldichlorosilane (abbreviated as dimethyl or M2), it also includes methyltrichlorosilane (abbreviated as monomethyl or M1), trimethyl B...

Claims

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Application Information

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IPC IPC(8): C07F7/12B01J31/14
Inventor 殷恒波陈维广王爱丽姜逸倩沈玉堂柳艳君卢章准张运生
Owner JIANGSU UNIV
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