Ternary copper catalyst used in synthesis of dimethyl dichlorosilane and preparation method of ternary copper catalyst

A technology of dimethyldichlorosilane and catalyst, applied in the field of ternary copper catalyst and its preparation, to achieve the effects of easy control, prevention of volatilization, and convenient operation

Inactive Publication Date: 2012-08-29
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation of CuO-Cu by solvothermal method 2 O-Cu has not been reported yet, and it is of great significance to carry out research and invention in this area

Method used

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  • Ternary copper catalyst used in synthesis of dimethyl dichlorosilane and preparation method of ternary copper catalyst
  • Ternary copper catalyst used in synthesis of dimethyl dichlorosilane and preparation method of ternary copper catalyst
  • Ternary copper catalyst used in synthesis of dimethyl dichlorosilane and preparation method of ternary copper catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Weigh 0.5g Cu(CH 3 COO) 2 , Dissolved in 40mL of 15% (volume ratio) glycerol aqueous solution, added the prepared 1M sodium hydroxide solution, adjusted the pH value to 6, placed in a polytetrafluoroethylene lined reactor at 120℃ and reacted for 15h. After the end, the product was filtered, washed with water and absolute ethanol 5 times each, and dried in a vacuum drying cabinet at 60°C for 8 hours. The obtained copper catalyst has the following composition after chemical analysis: 28% Cu (weight percentage, the same below), 49% Cu 2 O and 23% CuO.

[0041] The ternary copper catalyst material prepared above was tested by X'PertPRO MPD multifunctional X-ray diffractometer produced by Panalytical Company (Panalytical) in the Netherlands.

[0042] The ternary copper catalyst material prepared above was analyzed by the Dandong Baxter BT-9300Z laser particle size distribution analyzer.

[0043] The surface morphology of the ternary copper catalyst material prepared above was obse...

Embodiment 2

[0050] Weigh 1g Cu(NO 3 ) 2 , Dissolved in 40mL of 40% (volume ratio) glycerol aqueous solution, add the prepared 3M sodium hydroxide solution, adjust the pH to 9, and place it in a polytetrafluoroethylene lined reactor at 180℃ to react for 24h. After the end, the product was filtered, washed with water and absolute ethanol 5 times each, and dried in a vacuum drying cabinet at 60°C for 8 hours. The obtained copper catalyst has the following composition after chemical analysis: 11% Cu, 68% Cu 2 O and 21% CuO.

[0051] Figure 5 Is the XRD pattern of the copper catalyst obtained in Example 2, where 2θ=36.4° is Cu 2 The characteristic peak of O, the shoulder peak composed of 2θ=35.5° and 2θ=38.7° is the characteristic peak of CuO, and 2θ=43.3° is the characteristic peak of Cu. It can be seen that the catalyst synthesized by this method is composed of CuO, Cu 2 A ternary copper catalyst composed of O and Cu.

[0052] Image 6 In order to analyze the particle size of the copper catalyst...

Embodiment 3

[0054] Weigh 2g CuSO 4 , Dissolved in 40mL of 75% (volume ratio) butanediol aqueous solution, added the prepared 5M sodium hydroxide solution, adjusted the pH value to 13, placed in a polytetrafluoroethylene lined reactor at 250℃ and reacted for 30h. After the end, the product was filtered, washed with water and absolute ethanol 5 times each, and dried in a vacuum drying cabinet at 60°C for 8 hours. The obtained copper catalyst has the following composition after chemical analysis: 43% Cu, 44% Cu 2 O and 13% CuO. Figure 5 Is the XRD diagram of the product, Image 6 For particle size analysis.

[0055] Figure 7 XRD pattern of the copper catalyst obtained in Example 3, where 2θ=36.4° is Cu 2 The characteristic peak of O, the shoulder peak composed of 2θ=35.5° and 2θ=38.7° is the characteristic peak of CuO, and 2θ=43.3° is the characteristic peak of Cu. It can be seen that the catalyst synthesized by this method is composed of CuO, Cu 2 A ternary copper catalyst composed of O and C...

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Abstract

The invention relates to the field of a catalyst used in synthesis of dimethyl dichlorosilane, in particular to a ternary copper catalyst used in synthesis of the dimethyl dichlorosilane and a preparation method of the ternary copper catalyst. The preparation method according to the invention comprises the following steps of: (1) dissolving a copper salt into a mixed solvent of polybasic alcohol and water to obtain solution with copper ion concentration of 0.0025-0.25 g/mL; and (2) dropwise adding pH regulator aqueous solution into the solution obtained by the step (1) under a stirring condition, transferring the solution into a reaction kettle after the pH value of the solution is 6-13, reacting at 100-250 DEG C for 2-30 hours to obtain brown precipitate, and washing and drying the precipitate to obtain the ternary copper catalyst. The ternary copper catalyst prepared by the invention has the advantages of simple experimental process route, convenience in operation, entire process performed in the reaction kettle, no need of any complex experimental equipment, high reaction speed, easiness for large-scale production and capability of showing higher selectivity for the dimethyl dichlorosilane and higher conversion rate for a silicon powder raw material.

Description

Technical field [0001] The invention relates to the field of catalysts for synthesizing dimethyldichlorosilane, in particular to a ternary copper catalyst for synthesizing dimethyldichlorosilane and a preparation method thereof. Background technique [0002] Silicone materials have the dual properties of both inorganic and organic materials. They are resistant to high and low temperatures, electrical insulation, weather resistance, corrosion resistance, non-toxic and odorless, and are widely used in electronics, automobiles, petroleum, chemical, construction, aerospace and other fields . Methylchlorosilane is the most important and the most used organosilicon monomer for preparing organosilicon materials, and it is the foundation and pillar of the entire organosilicon industry. The direct synthesis of methylchlorosilane technology invented by EGRochow in 1940 is still the only industrial production of methylchlorosilane due to its simple process, high yield, no solvent, low risk...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72C07F7/16
Inventor 苏发兵赵丽润车红卫王莹利高俊杰翟世辉朱德洪
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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