A kind of method that calcium hydride reduces chlorosilane to prepare hydrosilane

A technology of calcium hydride and chlorosilane, which is applied in the field of reduction of chlorosilane, can solve the problems of high temperature of the reaction system, narrow application range, and inability to obtain the target product, and achieve the effect of increasing the reaction speed and yield, and rapid reduction

Active Publication Date: 2019-06-11
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 1971, R.Calas et al. reported adding CaH 2 The amount of 5% (mol fraction) AlCl 3 can make CaH 2 Restore Me 3 The yield of SiCl can reach more than 80%; but the catalyst cycle can only be realized when it is higher than 270°C, and the temperature of the reaction system is very high
In 2007, A. Tsuhako et al. found that ZnCl 2 When present, CaH 2 Phenyldimethylsilane can be reduced, and the yield of product phenyldimethylsilane is 83%; ZnCl-free 2 When the reaction does not occur, it is confirmed that the ZnCl 2 However, the application of this catalytic reduction system is relatively narrow, such as for ClCH 2 SiMeCl 2 , ClCH 2 SiCl 3 Then there is no effect and the target product cannot be obtained
GotzKoerner et al. reported that ball milling, ultrasonic and other mechanical activation methods can be used to reduce organopolysiloxanes containing terminal Si-Cl to Si-H-containing organopolysiloxanes under relatively mild conditions of cheap metal hydrides. It does have a better effect on LiH, but on CaH 2 The effect of using only mechanical activation is often still difficult to reach a practical level

Method used

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  • A kind of method that calcium hydride reduces chlorosilane to prepare hydrosilane
  • A kind of method that calcium hydride reduces chlorosilane to prepare hydrosilane
  • A kind of method that calcium hydride reduces chlorosilane to prepare hydrosilane

Examples

Experimental program
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Effect test

Embodiment 1

[0065] The 100mL three-neck round bottom flask was dried, connected with a mechanical stirrer, spherical condenser, constant pressure funnel and gas guiding device, then evacuated for three times to replace nitrogen, and at the same time baked with a heat gun to remove attached water vapor. Under nitrogen atmosphere, add 9.3g (0.22mol) CaH 2 , 0.38g (0.01mol) lithium aluminum hydride, 25mL diethylene glycol dimethyl ether solvent, 25g ZrO 2 Ceramic ball (φ=0.90mm). Add 25.8g (0.2mol) of Me to the constant pressure funnel 2 SiCl 2 , slowly dropwise into the reaction flask under mechanical stirring. After the dropwise addition was completed, it was heated to 50° C. and reacted for 10 h. The main reduction product obtained is Me 2 SiH 2 , The reaction yield is 97%.

Embodiment 2

[0067] The 250mL three-neck round bottom flask was dried, connected with a spherical condenser, constant pressure funnel and gas guiding device, then evacuated three times to replace nitrogen, and at the same time baked with a hot air gun to remove attached water vapor. Under nitrogen atmosphere, add 9.3g (0.22mol) CaH 2 , 0.38g (0.01mol) lithium aluminum hydride, 35mL diethylene glycol dimethyl ether solvent. Add 23.0g (0.2mol) MeSiHCl to the constant pressure funnel 2 , and slowly dropwise added to the reaction flask under magnetic stirring. After the dropwise addition was completed, heat to 50°C for 7 hours, and the product 9.1g MeSiH was collected in the liquid nitrogen cold trap 3 , the yield is close to 100%.

[0068] figure 1 is the chromatogram of the product, figure 2 for figure 1 The mass spectrum of the middle peak 1 confirms that the main peak 1 is methylsilane, according to figure 1 It can be calculated that the purity of methylsilane in the product reache...

Embodiment 3

[0070] The 250mL three-neck round bottom flask was dried, connected with a spherical condenser, constant pressure funnel and gas guiding device, then evacuated three times to replace nitrogen, and at the same time baked with a hot air gun to remove attached water vapor. Under nitrogen atmosphere, add 9.3g (0.22mol) CaH 2 , 0.38g (0.01mol) lithium aluminum hydride, 35mL butyl ether solvent. Add 23.0g (0.2mol) MeSiHCl to the constant pressure funnel 2 , and slowly dropwise added to the reaction flask under magnetic stirring. After the dropwise addition is completed, heat to 50°C for 7h to obtain the product MeSiH 3 , the product yield reaches 85%.

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Abstract

The invention discloses a method for preparing hydrogen silane by using calcium hydride to conduct reduction on chlorosilane and belongs to the technical field of chlorosilane reduction. The problemsof harsh reaction conditions, low reaction speed and the like of chlorosilane reduction through CaH2 in the prior art are solved. In an organic solvent, under catalysis of a catalyst, calcium hydrideis used as a reducing agent, and chlorosilane is reduced into hydrogen silane; the catalyst is borane or borohydride or lithium aluminum hydride, and the organic solvent is tetrahydrofuran or diethylene glycol dimethyl ether or other ether solvents. The method can be applied to hydrogen silane preparation through chlorosilane reduction.

Description

technical field [0001] The present invention relates to the reduction of a kind of chlorosilane, relate in particular to a kind of calcium hydride (CaH 2 ) method for preparing hydrosilane by reducing chlorosilane. Background technique [0002] Hydrosilane is a silicon compound containing Si-H bonds in its molecule, which is an important functional monomer and has a wide range of uses. [0003] In the prior art, the preparation method of hydrosilane (containing chloroalkylhydrosilane) mainly adopts the reduction method, through the reaction of chlorosilane or alkoxysilane with abundant sources and a strong reducing agent, the chlorosilane or alkoxysilane on the Reduction of chlorine or alkoxy groups in whole or in part to H yields silicon hydrides. The reduction method has abundant raw materials, more types of hydrosilanes, and higher yields, and usually can retain unsaturated groups such as vinyl groups, and has wider adaptability. [0004] In the reduction method, the r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/08C07F7/12C01B33/04
CPCC01B33/04C07F7/083
Inventor 李永明陈义徐彩虹王新良
Owner INST OF CHEM CHINESE ACAD OF SCI
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