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A kind of preparation method of hollow copper oxide catalyst used for synthesizing methyl chlorosilane

A technology of methylchlorosilane and copper oxide, which is applied in the field of preparation of hollow copper oxide catalysts, can solve problems such as low reproducibility, difficulty in large-scale synthesis, and difficult repeatability of product morphology, and achieve simple and controllable process and product shape. Good appearance reproducibility, control conditions and means are easy to implement

Inactive Publication Date: 2015-09-23
HEBEI UNIV OF ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally, expensive organic templates are added during the reaction to assist in the synthesis, or the reaction parameters are precisely regulated. The product morphology is not easy to repeat, the reproducibility is low, and it is not easy to synthesize on a large scale.

Method used

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  • A kind of preparation method of hollow copper oxide catalyst used for synthesizing methyl chlorosilane
  • A kind of preparation method of hollow copper oxide catalyst used for synthesizing methyl chlorosilane
  • A kind of preparation method of hollow copper oxide catalyst used for synthesizing methyl chlorosilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 0.40g of copper oxide and dissolve it in 5ml of ammonia water containing ammonium carbonate (33.3wt%), then add 45ml of N,N-dimethylformamide (DMF, the volume ratio of the mixed solution to DMF is 0.1, and the concentration of copper ions is 0.1mol / l), mix evenly, transfer the mixed solution to a 100ml stainless steel hydrothermal kettle, heat to 130°C and keep it warm for 15h. After the reaction, the product is separated, washed, dried, and then roasted at 500°C for 2h to obtain a black powder product.

[0028] The black powder product prepared above was subjected to an XRD test on a D / max-rB multifunctional X-ray diffractometer produced by Shimadzu Corporation of Japan. figure 1 It is the XRD spectrum of the black powder product obtained in Example 1. The diffraction peaks in the spectrum are typical copper oxide characteristic diffraction peaks. According to the standard powder diffraction card (JCPDSNo.48-1548), its crystal structure is monoclinic . The XRD ...

Embodiment 2

[0031] Weigh 2.0g of copper oxide and dissolve it in 11.5ml of ammonia water containing ammonium carbonate (33.3wt%), then add 38.5ml of N,N-dimethylformamide (DMF, the volume ratio of the mixed solution to DMF is 0.3, and the concentration of copper ions is 0.5 mol / l), mix evenly and transfer the mixed solution to a 100ml stainless steel hydrothermal kettle, heat it to 120°C and keep it for 20h. After the reaction, the product is separated, washed, dried, and then roasted at 300°C for 4h to obtain a black powder product.

[0032] XRD spectrum analysis product is monoclinic copper oxide. SEM photos show that the product is hollow-shaped, and its size is about 7.2 μm. TEM photos further confirmed that the product has a hollow structure with a size of 7.1 μm. Electron diffraction pictures confirmed that the product was composed of single crystal nanoparticles. The specific surface analyzer test shows that the hollow copper oxide has a mesoporous structure, and the BET specific...

Embodiment 3

[0034] Weigh 0.2g of copper oxide and dissolve it in 16.7ml of ammonia water containing ammonium carbonate (33.3wt%), then add 33.3ml of N,N-dimethylformamide (DMF, the volume ratio of the mixed solution to DMF is 0.5, and the concentration of copper ions is 0.05 mol / l), mix evenly and transfer the mixed solution to a 100ml stainless steel hydrothermal kettle, heat it to 180°C and keep it for 10h. After the reaction, the product is separated, washed, dried, and then roasted at 250°C for 10h to obtain a black powder product.

[0035] XRD spectrum analysis product is monoclinic copper oxide. SEM photos show that the product is hollow-shaped, and its size is about 6.5 μm. TEM photos further confirmed that the product has a hollow structure with a size of 6.3 μm. Electron diffraction pictures confirmed that the product was composed of single crystal nanoparticles. The specific surface analyzer test shows that the hollow copper oxide has a mesoporous structure, and the BET specif...

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Abstract

The invention provides a preparation method of a hollow copper oxide catalyst for synthesizing methyl chlorosilane, belonging to the field of an organosilicone monomer catalyst. The preparation method of the hollow copper oxide catalyst for synthesizing methyl chlorosilane comprises the steps of dissolving copper oxide into mixed solution of ammonium hydroxide and ammonium salt, then mixing the solution and an organic solvent to carry out solvent thermal reaction, and separating, washing, drying and roasting the product to obtain hollow copper oxide. According to the method provided by the invention, the preparation process is simple and efficient, reaction parameters are controllable, large-scale synthesis is easy, prepared hollow copper oxide serving as the catalyst is used for synthesizing methyl chlorosilane monomer which has relatively high reactivity and selectivity. Through the preparation method, industrial solid copper oxide powder with irregular appearance and low reactivity is converted into the hollow copper oxide catalyst with high reactivity, and scientific significance and application values are important.

Description

technical field [0001] The invention relates to the technical field of organosilicon monomer catalyst preparation, in particular to a method for preparing a hollow copper oxide catalyst used for synthesizing methylchlorosilane. Background technique [0002] As a type of p-type semiconductor transition metal oxide, copper oxide is widely used in important fields such as catalysts, lithium-ion battery materials, and supercapacitor materials. Especially in the field of organosilicon monomer synthesis, copper oxide, as an efficient copper catalyst, can improve the selectivity of dimethyldichlorosilane in methylchlorosilane products. It is well known that the morphology, size and structure of materials are the key factors affecting their physical and chemical properties. Therefore, copper oxide materials with different morphologies and structures have aroused great interest. At present, copper oxide materials with various shapes such as nanowires, nanorods, nanotubes, nanocubes...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/72C07F7/16
Inventor 刘爱凤车红卫
Owner HEBEI UNIV OF ENG