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Method for pyrolysis of organosilicone high-boiling substance under catalysis of solid alkali

A catalytic cracking, high boiler technology, applied in chemical instruments and methods, organic chemistry, chemical/physical processes, etc., can solve the problems of non-reusability, increase production costs, etc., achieve less by-products, improve conversion rate, catalyst active effect

Active Publication Date: 2014-11-05
山东时代新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Most of the catalysts used in existing patents and literature technologies are soluble catalysts, which cannot be reused and increase the production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Step (1) in 500L reactor, add tri-n-butylamine 100Kg, dioctadecyl secondary amine 0.1Kg, perfluorotriethylamine 0.1Kg and macroporous cross-linked polyhydroxyethyl methacrylate resin 80Kg respectively, in React at 70°C for 10 h to obtain a composite catalyst, which is ready for use.

[0021] Step (2) Add 100Kg of organosilicon high boilers after impurity removal and 8Kg of high boiler composite catalysts in a 500L cracking kettle with a fractionation tower, then feed hydrogen chloride gas to control the molar ratio of high boilers and hydrogen chloride feed The ratio is 1:1.25, the temperature is raised to 110°C, and after 40 hours of constant temperature under normal pressure, the reaction produces four monochlorosilanes: dimethyldichlorosilane, trimethylchlorosilane, monomethyldichlorosilane, and monomethyltrichlorosilane. The solid-based mixed product is condensed and collected by the overhead condenser of the fractionation column. The conversion rate and the conten...

Embodiment 2

[0023] (1) Add tri-n-butylamine 100Kg, dioctadecyl secondary amine 0.05Kg, perfluorotriethylamine 0.05Kg and macroporous cross-linked polyhydroxyethyl methacrylate resin 50Kg respectively in 500L reactor. React at 30°C for 20 hours to obtain a composite catalyst, which is ready for use.

[0024] (2) Add 100Kg of organosilicon high boilers and 8Kg of composite catalyst after impurity removal in a 500L cracking kettle with a fractionation tower, then feed hydrogen chloride gas, and control the molar ratio of high boilers and hydrogen chloride feed to be 1: 1.05 , heated up to 100°C, and kept at constant temperature for 50 hours under normal pressure, the reaction produced dimethyldichlorosilane, trimethylmonochlorosilane, monomethyldichlorosilane, and monomethyltrichlorosilane. The mixed products are condensed and collected by the overhead condenser of the fractionation column. The conversion rate and the content of dimethyldichlorosilane are shown in Table 1.

Embodiment 3

[0026] 1) In a 500L reactor, add 100Kg of tri-n-butylamine, 0.2Kg of dioctadecyl secondary amine, 0.5Kg of perfluorotriethylamine and macroporous cross-linked polyhydroxyethyl methacrylate resin by mass ratio of 100Kg, React at 100° C. for 5 h to obtain a composite catalyst for future use.

[0027] (2) Add 100Kg of organosilicon high boilers after impurity removal and 8Kg of composite catalyst in a 500L cracking kettle with a fractionation tower, then feed hydrogen chloride gas, and control the molar ratio of high boilers and hydrogen chloride feed to be 1: 1.4 , heated up to 120°C, and kept at constant temperature for 30 hours under normal pressure, the reaction produced dimethyldichlorosilane, trimethylmonochlorosilane, monomethyldichlorosilane, and monomethyltrichlorosilane. The mixed products are condensed and collected by the overhead condenser of the fractionation column. The conversion rate and the content of dimethyldichlorosilane are shown in Table 1.

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PUM

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Abstract

The invention discloses a method for pyrolysis of organosilicone high boiling substance under catalysis of solid alkali. The method comprises the steps of subjecting tri-n-butylamine, dioctadecyl amine, perfluorotriethylamine and macroporous crosslinked poly(hydroxyethyl methacrylate) resin to a load reaction so as to obtain a compound catalyst after the load reaction is finished; adding the organosilicone high-boiling substance and compound catalyst with impurities removed in a pyrolysis kettle with a fractionating tower; then introducing hydrogen chloride gas into the pyrolysis kettle; reacting to generate mixed products mainly including four monomers such as dimethyldichlorosilane, trimethylchlorosilane, methyldichlorosilane and methyltrichlorosilane; and condensing and collecting the above mixed products through a condenser at the top of the fractioning tower. The catalyst has good activity and can be used circularly, and the method has few three wastes (waste gas, waste water and industrial residue) and is environment-friendly.

Description

technical field [0001] The invention relates to a method for preparing an organosilicon product, in particular to a method for catalyzing and cracking organosilicon high boilers with a solid base. Background technique [0002] The by-product of methylchlorosilane is industrially produced by "direct method" (CH 3 ) 2 SiCl 2 A by-product of the monomer process. In the "direct method" industrial production, due to the constraints of catalysts, process conditions and other factors, the target product (CH 3 ) 2 SiCl 2 In addition, there are 5-10wt% high-boiling polysilane mixtures with a boiling range of 70-215°C, mainly silicon-silicon bonds, silicon-oxygen-silicon bonds, and silicon-carbon-silicon bonds, referred to as high boilers. Its main components are 1,2-dimethyl-1,1,2,2-tetrachlorodisilane, 1,1,2 trichloro-1,2,2-trimethyldisilane, 1,2 -Dichloro-1,1,2,2-tetramethyldisilane, organosilicon high boiler is a mixed liquid with caramel color, pungent smell and strong cor...

Claims

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Application Information

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IPC IPC(8): C07F7/12B01J31/06
Inventor 张玲王新
Owner 山东时代新材料科技有限公司
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