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A method for comprehensively treating organosilicon by-products

A comprehensive treatment and organosilicon technology, applied in the direction of organic chemistry, chemical instruments and methods, compounds of group 4/14 elements of the periodic table, etc., can solve problems such as expensive ethanol reagents

Active Publication Date: 2016-02-24
内蒙古恒业成有机硅有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the ethanol reagent is relatively expensive, and the formed silicon tetrachloride partial ester substitute becomes a new by-product, which requires additional treatment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Put 250ml of high boilers into a 1L autoclave, the catalyst AlCl 3 10g (mass accounts for about 4% of the total amount of high boiling), the temperature of the reactor is raised to 300 ° C, and the pressure is about 4.2 MPa after 6 hours of reaction. After the reaction is completed, the temperature of the reactor is cooled to room temperature, and the material after the reaction is distilled , Determine the composition of the material after rearrangement by gas chromatography analysis. In the table, M2 is dimethyldichlorosilane, M1 is methyltrichlorosilane, MH is methyldichlorosilane, and M3 is trimethylchlorosilane.

[0022] Material composition and selectivity after rearrangement reaction:

[0023] M2: 49.0%; M1: 19.1%; M3: 2.1%; MH: 2.2%; Residual high boilers: 26.3%;

[0024] The remaining components in this embodiment are substances with low boiling points, such as dimethyl monochlorosilane, tetramethylsilane, isopentane and the like.

[0025] From the above dat...

Embodiment 2

[0027] Put 250mL of high boilers, 25mL of azeotropes, 25mL of low boilers, and 25mL of methyltrichlorosilane into a 1L autoclave, and add 6% of the total amount of the mixture as catalyst AlCl 3 , reacted at 280°C for 5 hours, and the final pressure was 3.2Mpa. After the reaction, the temperature of the reactor was cooled to room temperature, the material after the reaction was distilled, and the composition of the rearranged material was determined by gas chromatography analysis:

[0028] Material composition after rearrangement reaction

[0029] The remaining components in this embodiment are substances with low boiling points, such as dimethyl monochlorosilane, tetramethylsilane, isopentane and the like.

Embodiment 3

[0031] Put 80mL of high boilers, 80mL of azeotropes, 80mL of low boilers, and 80mL of methyltrichlorosilane into a 1L autoclave, and add 3% of the total amount of the mixture as catalyst AlCl 3 , reacted at 350°C for 5 hours, and the final pressure was 9Mpa. After the reaction, the temperature of the reactor was cooled to room temperature, the material after the reaction was distilled, and the composition of the rearranged material was determined by gas chromatography analysis:

[0032] Material composition after rearrangement reaction

[0033] The remaining components in this embodiment are substances with low boiling points, such as dimethyl monochlorosilane, tetramethylsilane, isopentane and the like.

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Abstract

The invention relates to a method for comprehensively treating organosilicon by-products. The organosilicon by-products, high boilers, azeotropes, low boilers, and methyltrichlorosilane are mixed in a volume ratio of 1: (0.1~1): (0.1~ 1): (0.1~1), after mixing, it is integrated into dimethyldichlorosilane through disproportionation reaction under the Lewis catalyst; the reaction temperature is 280~350°C, and the reaction time is 1~6h , and during the reaction process, the pressure is 3-10Mpa as the filling amount of the material, the temperature rise and the composition of the organochlorosilane change. The invention is simple and easy to implement, has a high dimethyl selectivity, and converts by-products that cause hidden dangers to safety and the environment into dimethyldichlorosilane through a rearrangement reaction, thereby generating both economic value and social benefits.

Description

technical field [0001] The invention belongs to the technical field of comprehensive utilization of organosilicon by-products, and specifically relates to organic silicon by-products such as high boilers, low boilers, azeotropes and methyl trichlorosilane are mixed and then integrated into dimethyl dichlorosilane through disproportionation reaction. Chlorosilane method. Background technique [0002] A large number of by-products will be produced in the production process of direct synthesis of dimethyldichlorosilane, among which methyltrichlorosilane is the most, accounting for 10-15% of the total product, followed by high boiling substances accounting for about 5%. (Boiling point higher than 70°C, mainly containing Si-Si bond, Si-O-Si bond, Si-C-Si bond compound), low boilers accounted for about 1% (boiling point lower than 41°C, mainly containing dimethyl Monochlorosilane, tetramethylsilane, methyldichlorosilane, etc.), the azeotrope accounts for about 1% (mainly 60% trim...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/12
Inventor 孙峰吴忆南
Owner 内蒙古恒业成有机硅有限公司
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