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Improved producing process of methyl chlorosilane

A technology of methyl chlorosilane and methyl chlorodisilane is applied in the field of improvement of the production method for preparing methyl chlorosilane by cracking, and can solve the problem of high energy consumption and low content of dimethyl dichlorosilane and methyl hydrogen dichlorosilane , long process flow and other problems, to achieve sufficient cracking effect

Inactive Publication Date: 2005-01-05
吉林市凇泰化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The reaction time of this method is only 4-6 hours, but the raw materials need to be pretreated, the process flow is long, the energy consumption is high, and the content of dimethyldichlorosilane and methylhydrogendichlorosilane (hydrogen-containing monomer) is low. and only 48.63-57.59%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 600kg of methyl high boilers and 8kg of catalyst N,N-dimethylaniline are added to the cracking kettle to keep a certain amount of high boilers in it. The still height of this cracking still: still diameter=1-1.4. The cracking kettle is equipped with a packed fractionation tower. Heating to raise the temperature and control the temperature of the material in the kettle to 104±1°C, and 3 Pass hydrogen chloride into the above-mentioned material at a speed of / 1h, and collect the condensate product cooled by the fractionating tower and the condenser. After the reaction was carried out for 0.5h, add 200kg of the above-mentioned methyl high boilers to the kettle, and finish it in 0.5h, and then add it once every 2h, add 200kg each time, and finish adding it in 0.5h; The catalyst is added once every 4 hours, 2kg each time, and the addition is completed in 10 minutes. Such a continuous reaction for 30h, and continuous collection of lysates, liquid products after fractional d...

Embodiment 2

[0046] 600kg of methyl high boilers and 8kg of catalyst N,N-dimethylaniline are added to the cracking kettle to keep a certain amount of high boilers in it. The still height of this cracking still: still diameter=1.5-2.0. The cracking kettle is equipped with a packed fractionation tower. Heating up and controlling the temperature of the material in the kettle to 99±1°C, and 3Pass hydrogen chloride into the above-mentioned material at a speed of / 1h, and collect the condensate product cooled by the fractionating tower and the condenser. After the reaction was carried out for 0.5h, add 200kg of the above-mentioned methyl high-boiler to the kettle, and finish it in 0.5h. After that, add it once every 2h, add 200kg each time, and finish adding it in 0.5h; The catalyst is added once every 4 hours, 2kg each time, and the addition is completed in 10 minutes. Such a continuous reaction for 30h, and continuous collection of lysates, liquid products after fractional distillation and ...

Embodiment 3

[0054] Except reaction temperature is 89 ± 1 ℃, continuous reaction 36h, all the other are the same as Example 2, and its methyl high boiler cracking conversion rate is 80%, and its product composition:

[0055] Methylhydrogendichlorosilane CH 3 HSiCl 2 43.92%

[0056] Dimethyldichlorosilane (CH 3 ) 2 SiCl 2 29.34%

[0057] (the sum of the above two components accounts for 73.36% of the total product)

[0058] Monomethyltrichlorosilane CH 3 SiCl 3 18.47%

[0059] Trimethylchlorosilane (CH 3 ) 3 SiCl 1.24%

[0060] Unconverted high boilers 7.03%

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Abstract

The invention relates to an improvement of the producing method of methylchlorosilane, adding methylchlorodisilane, and a catalyst N, N-dimethylaniline1 accounting for 1-2% of the weight of methylchlorodisilane into a cracking kettle, making the materials a certain quantity, where the kettle is installed with a fractionating tower. It controls temperature at 90-110 deg.C, charging hydrogen chloride into the materials, making the molar ratio of methylchlorodisilane to hydrogen chloride 1 to 0.9-5.5, and its characteristic: the ratio of the height of the crackling kettle to the diameter = 1.0-2.0; the flux of the hydrogen chloride is 16 cu m / h; reacting for 5 hours, and then supplementing methylchlorodisilane into the kettle, and later supplementing once at 2h intervals, supplementing the hydrogen chloride once 200 kg, and completing in 0.5 h; supplementing the catalyst 2 kg at 4h intervals and completing in 10 minutes. It continuously reacts for 28-36 h, and collects condensate. It does not preprocess raw materials, and the sum of methylhydrodichlorosilane and dimethyldichlorosilane higher than that of existing techniques.

Description

technical field [0001] The invention relates to a method for producing methylchlorosilane, in particular to the improvement of the method for producing methylchlorosilane by pyrolysis by using methylchlorodisilane, a by-product high boiler in the production of organosilicon monomer, as a raw material. Background technique [0002] The scientific and technical personnel engaged in the research, development and production of organic silicon are very concerned about the by-product methyl chlorodisilane high boiler (hereinafter referred to as It is called the development and utilization of methyl high boilers). Japanese patent JP Zhao 55-26150 discloses the high boiler by methyl [(CH 3 ) n SiCl 6-n , wherein, n is an integer of 1-5] to prepare methyl (hydrogen) dichlorosilane CH 3 HSiCl 2 Methods. The method uses N,N-dimethylaniline as a catalyst to contain 64% (CH 3 ) 2 Si 2 Cl 4 , 35.9 (CH 3 ) 3 Si 2 Cl 3 The pretreated high boiler is used as raw material to prep...

Claims

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Application Information

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IPC IPC(8): C07F7/12
Inventor 朱维新王立元唐龙强王生全
Owner 吉林市凇泰化工有限责任公司
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