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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. Since the content of Sanjia in the by-products of the "direct method" is small, its price even exceeds that of Dijia. Therefore, some manufacturers do not hesitate to adjust the "direct method" process to increase the output of top three, which not only interrupts the continuity of normal production, increases production costs, but also easily causes safety hazards
However, the reactions catalyzed by these solid catalysts have high reaction temperature and pressure, and high requirements for equipment. In particular, these catalysts are difficult to separate after the reaction, are difficult to reuse, and cannot be continuously produced, which not only increases the cost, but also causes serious resources. waste and even environmental pollution

Method used

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

Examples

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preparation example Construction

[0030] Preparation of Chloroaluminate Ionic Liquid Catalyst

[0031] N -Butylpyridinechloroaluminate[BPy]Cl-nAlCl 3(n=2-6) Preparation method of ionic liquid: under nitrogen protection, 1.50 mol (119 g) of pyridine, 1.7 mol (158 g) of chlorobutane Stir and mix well, then warm up to 100 °C in the dark to appear a gentle reflux, and react at this temperature for 72 h. Stop heating, cool to below 10 °C, white crystals precipitated, filter with suction and wash the crude product with ethyl acetate, and dry the product in vacuum at 70 °C for 48 h to remove residual ethyl acetate. The yield of the product [BPy]Cl is about 55%, and it is stored in a dry and inert atmosphere for future use.

[0032] The glove box was filled with nitrogen, and different amounts of anhydrous AlCl were slowly added in batches to the quantitative above-mentioned intermediate [BPy]Cl at room temperature. 3 During the feeding process, keep stirring to avoid local high temperature until the solids are ...

Embodiment 1

[0034] Methyltrichlorosilane and low boiler disproportionation reaction to prepare dimethyldichlorosilane:

[0035] Add methyl trichlorosilane and low boiler mass ratio 1.5:1 total 150 g reaction mixture and 16.7% (25 g) aluminum trichloride and chloride in autoclave N -Butylpyridine molar ratio 6:1 N -Butylpyridine chloroaluminate [BPy]Cl-6AlCl 3 The ionic liquid catalyst was sealed, and the air in the kettle was replaced by nitrogen gas, kept fully stirred (500 rpm), heated to 150 °C, and reacted for 5 h. After the reaction is finished, the temperature of the reaction kettle is lowered to room temperature, and the reaction product is taken out, and the product is separated from the ionic liquid, and then the product is sampled and analyzed by gas chromatography immediately.

[0036] The gas chromatography analysis conditions are:

[0037] Chromatographic column: OV-1701 capillary column; detector type; FID; carrier gas: high-purity nitrogen; injector temperature: 180 ℃;...

Embodiment 2

[0046] Same as Example 1 but keep methyltrichlorosilane and low boiler mass ratio 1.5:1, only change aluminum trichloride and chloride in ionic liquid N -Butylpyridine molar ratios are 2:1, 3:1, 4:1, 5:1 respectively, the results are shown in image 3 .

[0047] Depend on 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 an obvious increasing trend . When AlCl 3 When the molar ratio with [BPy]Cl was 6:1, the conversion rate of methyltrichlorosilane reached 88.21%, the yield of dimethyldichlorosilane reached 69.40%; the yield of trimethylchlorosilane was Continuous decline. Therefore, increasing [BPy]Cl-nAlCl 3 AlCl in ionic liquid catalyst 3 The content of has a significant impact on the disproportiona...

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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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