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Process for preparing allyl chlorosilane

A technology of allyl chlorosilane and chlorosilane, which can be applied to chemical instruments and methods, compounds of elements of Group 4/14 of the periodic table, and metal/metal oxide/metal hydroxide catalysts, etc. The chlorosilane technology is not too mature, the reaction temperature is high, and the separation of the main product is difficult.

Inactive Publication Date: 2006-12-20
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, method a) often obtains mixed hydrocarbyl silanes, and uses a large amount of solvents, which is inflammable and explosive; b) method needs to use precious transition metal platinum, palladium, etc.; A certain proportion of by-products are often generated, and the separation of the main product is difficult; the d) method plays an important role in the synthesis of ethyl chlorosilane and aryl chlorosilane, but the technology for synthesizing allyl chlorosilane is not too mature

Method used

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  • Process for preparing allyl chlorosilane
  • Process for preparing allyl chlorosilane
  • Process for preparing allyl chlorosilane

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Place (0.1 mol) rare earth metal samarium in a 100 mL three-necked round bottom flask equipped with a magnetic stirrer, a constant pressure dropping funnel, a reflux condenser, and a gas guide device. Then inject 40 mL of freshly distilled toluene solution, and under the protection of nitrogen, add a slight excess of allyl bromide (0.11 mol) and diphenyldichlorosilane (0.1 mol) to the reaction flask. Stir at room temperature, the solution turns purple-red after 10 minutes, and then react at constant temperature (25°C) for 2 hours. When the solution turns light yellow, stop the reaction. filter. Distill under reduced pressure to obtain colorless allyldiphenylchlorosilane (yield: 98%). Some physical data of the compound are as follows: IR: v max (liquid film)3070.6, 2969.1, 1630.0, 1427.9, 1112.5cm -1 ; 1 H NMR(400MHz, CDCl 3 ): 7.28-7.72 (5H, m, ArH), 5.73-5.83 (1H, m, CH), 5.05-5.09 (2H, t, CH) 2 =), 2.30-2.32(2H, d, CH 2 CH=CH 2 ); 13 C NMR(100MHz, CDCl 3 ): 133.96, 131.77...

Embodiment 2

[0026] Place (0.1 mol) rare earth metal cerium in a 100 mL three-necked round bottom flask equipped with a magnetic stirrer, a constant pressure dropping funnel, a reflux condenser, and an air guide device. Then inject 40 mL of freshly distilled tetrahydrofuran solution, under the protection of nitrogen, add allyl bromide (0.11 mol) and phenyltrichlorosilane (0.05 mol) into the reaction flask. Stir at room temperature, the solution turns purple-red after 10 minutes, and then react at constant temperature (25°C) for 2 hours. When the solution turns light yellow, stop the reaction. filter. Distill under reduced pressure to obtain colorless phenyldiallylchlorosilane (yield: 95%).

Embodiment 3

[0028] Place (0.1 mol) rare earth metal samarium in a 100 mL three-necked round bottom flask equipped with a magnetic stirrer, a constant pressure dropping funnel, a reflux condenser, and a gas guide device. Then inject 40 mL of freshly distilled xylene solution, under the protection of nitrogen, add allyl bromide (0.11 mol) and methyl trichlorosilane (0.1 mol) into the reaction flask. Stir at room temperature, the solution turned purple-red after 10 minutes, and then heated to reflux (110°C) for 12 hours. When the solution turns light yellow, stop the reaction. filter. Distill under reduced pressure to obtain colorless methallyldichlorosilane (yield: 98%).

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Abstract

This invention relates to a method for producing allyl chloro-silicane using rare-earth metal catalyst, comprising: under the catalyzing of rare-earth metal, dichlorosilane or trichlorosilane performs coupling reaction with allyl bromide to synthesize allyl chloro-silicane, which well solves some problems in current technology. The producing process characterizes: under the protection of nitrogen, dissolve the chloro-silicane and allyl bromide in organic solvent, and then add in rare-earth metal as catalyst, thoroughly stir and react, filtrate by stewing; vacuum distill the filtrate so as to obtain the allyl chloro-silicane monomer, with the formula(I): R(Allyl)xSi(Cl)y (1).

Description

Technical field [0001] The invention relates to the field of organic chemistry, in particular to a method for preparing allyl chlorosilane by using a rare earth metal catalyst. Background technique [0002] Organohalosilane, R n SiX 4-n (R=Me, Et, Vi, Allyl, Pr, Ph, etc.; X=F, Cl, Br, I; n=1-3), especially allyl chlorosilanes containing unsaturated double bonds, which are used to prepare organic Important raw materials for silicone polymers (such as silicone oil, silicone rubber, silicone resin) and other silicon-functional and carbon-functional silanes. [0003] However, the preparation method of allyl chlorosilane is very limited. The existing synthesis methods mainly include: a) metal organic compound method (US 2698333, 19540); b) hydrosilation addition method (JP 2-290886.1990); c) heat shrinkage method (CCCP OXH, 1956: 630) ); d) Direct synthesis method (DD 5348.1942) and so on. However, method a) often obtains mixed hydrocarbyl silanes, and uses a large amount of solvents,...

Claims

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Application Information

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IPC IPC(8): C07F7/12B01J23/12
Inventor 李志芳来国桥邱化玉蒋可志曹肖君
Owner HANGZHOU NORMAL UNIVERSITY
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