Copper catalyst for direct method synthesis of methylchlorosilane and preparation method thereof

A technology of methylchlorosilane and copper catalyst, which is applied in the fields of chemical instruments and methods, organic chemistry, compounds of group 4/14 elements of the periodic table, etc., can solve the problems of low catalytic activity and insufficient catalyst preparation methods, and achieve The effect of improving catalytic activity, improving mass transfer process, and low content of harmful impurities

Inactive Publication Date: 2016-11-23
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In view of the use of the above three types of catalysts in production, as well as the current low catalytic activity of the ternary copper catalyst and the lack of catalyst preparation methods, the present invention provides a ternary copper catalyst system for the synthesis of methyl...

Method used

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  • Copper catalyst for direct method synthesis of methylchlorosilane and preparation method thereof
  • Copper catalyst for direct method synthesis of methylchlorosilane and preparation method thereof
  • Copper catalyst for direct method synthesis of methylchlorosilane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Dissolve 2.00g of copper nitrate (A.R.) in a mixed solvent of 80.0ml of pure ethanol (A.R.) and 24.0ml of ethylene glycol (A.R.), mix well, then add 60ml of ammonia (25%, A.R.) and 20ml sodium hydroxide solution (1mol L -1 , A.R.), stirred to a clear solution, transferred the obtained clear solution to an autoclave for reaction, sealed and maintained at 130°C for 16 hours, and then cooled to room temperature; the reaction solution was centrifuged to obtain a precipitate, which was washed with distilled water and ethanol in turn, and then vacuum-dried , to obtain CuO metal clusters;

[0033] (2) Dehydrate and dry the CuO obtained in step (1), pass through H 2 Reduction, the reaction temperature is 150-300°C, the system pressure is from normal pressure to 0.1MPa, and Cu metal clusters are obtained;

[0034] (3) Pass the Cu obtained in step (2) into an oxygen-containing gas to oxidize, control the oxygen partial pressure to be lower than 0.02MPa, the oxidation temper...

Embodiment 2

[0037] (1) Dissolve 2.00g of copper nitrate (A.R.) in a mixed solvent of 80.0ml of pure ethanol (A.R.) and 20.0ml of ethylene glycol (A.R.), mix well, then add 60ml of ammonia (25%, A.R.) and 20ml sodium hydroxide solution (1mol L -1 , A.R.), stirred to a clear solution, transferred the obtained clear solution to an autoclave for reaction, sealed and maintained at 130°C for 16 hours, and then cooled to room temperature; the reaction solution was centrifuged to obtain a precipitate, which was washed with distilled water and ethanol in turn, and then vacuum-dried , to obtain CuO metal clusters;

[0038] (2) Dehydrate and dry the CuO obtained in step (1), pass through H 2 Reduction, the reaction temperature is 150-300°C, the system pressure is from normal pressure to 0.1MPa, and Cu metal clusters are obtained;

[0039] (3) Pass the Cu obtained in step (2) into an oxygen-containing gas to oxidize, control the oxygen partial pressure to be lower than 0.02MPa, the oxidation temper...

Embodiment 3

[0042] (1) Dissolve 4.00g of copper nitrate (A.R.) in a mixed solvent of 80.0ml of pure ethanol (A.R.) and 24.0ml of ethylene glycol (A.R.), mix well, then add 60ml of ammonia (25%, A.R.) and 20ml sodium hydroxide solution (1mol L -1 , A.R.), stirred to a clear solution, transferred the obtained clear solution to an autoclave for reaction, sealed and maintained at 130°C for 16 hours, and then cooled to room temperature; the reaction solution was centrifuged to obtain a precipitate, which was washed with distilled water and ethanol in turn, and then vacuum-dried , to obtain CuO metal clusters;

[0043] (2) Dehydrate and dry the CuO obtained in step (1), pass through H 2 Reduction, the reaction temperature is 150-300°C, the system pressure is from normal pressure to 0.1MPa, and Cu metal clusters are obtained;

[0044] (3) Pass the Cu obtained in step (2) into an oxygen-containing gas to oxidize, control the oxygen partial pressure to be lower than 0.02MPa, the oxidation temper...

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Abstract

The invention relates to a preparation method of a ternary copper powder catalyst for synthesis of methylchlorosilane. The method is as follows: preparing a porous CuO metal micro-cluster body with a multilevel dandelion structure by a hydrothermal method, reducing the CuO with H2 to completely obtain a Cu metal micro-cluster body, and partially oxidizing to obtain a Cu2O and Cu mixture metal micro-cluster body; and finally, mixing the CuO metal micro-cluster body, the Cu metal micro-cluster body and the Cu2O and Cu mixture metal micro-cluster body in ratio to obtain the ternary copper powder catalyst. The ternary copper powder catalyst prepared by the method has a specific surface area up to 10-60m<2>/g, and has a hierarchical porous structure, in the reaction process of direct synthesis of the methylchlorosilane, contact interface between a reaction gas and solid silica fume can be increased, the catalytic activity of the catalyst can be improved, especially the three component ratio can be accurately controlled, by collocation of a little of a cocatalyst promoter, the selectivity of dimethyldichlorosilance in the product can reach a high level.

Description

technical field [0001] The invention relates to a preparation method of a ternary copper catalyst used for synthesizing methylchlorosilane, belonging to the technical field of catalysts. Background technique [0002] Organochlorosilanes (methyl chlorosilane, phenyl chlorosilane, vinyl chlorosilane, etc.) are the basis of the entire organosilicon industry, among which, methyl chlorosilane is the backbone of the organosilicon industry. The most important monomer and the basic raw material for the preparation of other silicon-functional silanes. Most silicone polymers are based on polydimethylsiloxane prepared from dimethyldichlorosilane (hereinafter referred to as dimethyl) as the base polymer, and then introduce other groups such as phenyl, vinyl, chlorine Phenyl, cyanoalkyl, fluoroalkyl, etc., to meet special needs. [0003] In 1941, E.G. Rochow first proposed the direct synthesis of methylchlorosilane by reacting methyl chloride and silicon powder under the action of a co...

Claims

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Application Information

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IPC IPC(8): B01J23/72C07F7/16
Inventor 邵月刚付方李叶芳刘继
Owner ZHEJIANG XINAN CHEM INDAL GROUP
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