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A kind of copper-zinc composite oxide, its preparation method and application

A composite oxide and copper-zinc technology, which is applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, chemical/physical processes, etc. Uniformity and other issues, to achieve the effect of environmental friendliness, high M2 selectivity, and good dispersion

Active Publication Date: 2018-03-30
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the disadvantages of cumbersome process flow, low product yield and poor quality in the existing CuO / ZnO composite oxide industrial production technology, and the dense structure of the main catalyst CuO in the Rochow reaction, which is mixed with the additive Zn or ZnO components Inhomogeneous shortcomings, the object of the present invention is to provide a copper-zinc composite oxide, its preparation method and use, the copper-zinc composite oxide has a uniform appearance and particle size, CuO and ZnO have good dispersion, and have a synergistic effect. It is used as a catalyst in the "direct method" synthesis of M2 monomer reaction, with excellent M2 selectivity and silicon powder raw material conversion rate, M2 selectivity ≥ 89.0%, silicon powder raw material conversion rate ≥ 30.0%

Method used

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  • A kind of copper-zinc composite oxide, its preparation method and application
  • A kind of copper-zinc composite oxide, its preparation method and application
  • A kind of copper-zinc composite oxide, its preparation method and application

Examples

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Embodiment 1

[0066] A preparation method of copper-zinc composite oxide, comprising the steps of:

[0067] (1) At 20°C, configure a solution containing copper ions and zinc ions (n Cu2+ 4mmol and n Cu2+ :n Zn2+ =10:1) 50mL, the solvent is a pure aqueous solution, the copper ions are derived from copper nitrate, and the zinc ions are derived from zinc nitrate;

[0068] (2) prepare sodium carbonate solution (C Na2CO3 0.8mol / L) 50mL, it was added to the solution containing copper ions and zinc ions described in (1), stirred for 0.5h to obtain a suspension;

[0069] (3) Transfer the suspension to a 100mL polytetrafluoroethylene-lined autoclave, perform a hydrothermal reaction at 130°C for 18 hours, then cool naturally to 20°C to obtain a hydrothermal product;

[0070] (4) Filtrate the hydrothermal product, wash the obtained solid several times with deionized water and absolute ethanol, and then dry it at 60° C. for 12 hours;

[0071] (5) Calcining the dried product at 400° C. for 12 hours...

Embodiment 2

[0076] A preparation method of copper-zinc composite oxide, comprising the steps of:

[0077] (1) At 25°C, configure a solution containing copper ions and zinc ions (n Cu2+ is 10mmol and n Cu2+ :n Zn2+ =5:1) 300mL, the solvent is a pure aqueous solution, the copper ions are derived from copper acetate, and the zinc ions are derived from zinc acetate;

[0078] (2) preparation potassium carbonate solution (C K2CO3 2mol / L) 50mL, it was added to the solution containing copper ions and zinc ions described in (1), stirred for 1.5h to obtain a suspension;

[0079](3) Transfer the suspension to a 600mL polytetrafluoroethylene-lined autoclave, perform a hydrothermal reaction at 100°C for 24 hours, then cool naturally to 20°C to obtain a hydrothermal product;

[0080] (4) Centrifuge the hydrothermal product, wash the obtained solid several times with deionized water and absolute ethanol, and then dry it at 80° C. for 10 h;

[0081] (5) Calcining the dried product at 500° C. for 10 ...

Embodiment 3

[0085] A preparation method of copper-zinc composite oxide, comprising the steps of:

[0086] (1) At 30°C, configure a solution containing copper ions and zinc ions (n Cu2+ is 50mmol and n Cu2+ :n Zn2+ =6:1) 200mL, solvent is aqueous ethanol (alcohol-water ratio is 0.4:1), copper ion is derived from copper chloride, and zinc ion is derived from zinc chloride;

[0087] (2) prepare sodium bicarbonate solution (C NaHCO3 1mol / L) 100mL, which was added to the solution containing copper ions and zinc ions described in (1), stirred for 2.5h to obtain a suspension;

[0088] (3) Transfer the suspension to a 500mL polytetrafluoroethylene-lined autoclave, perform a hydrothermal reaction at 150°C for 18 hours, then cool naturally to 20°C to obtain a hydrothermal product;

[0089] (4) Filtrate the hydrothermal product, wash the obtained solid several times with deionized water and absolute ethanol, and then dry it at 100°C for 8 hours;

[0090] (5) Calcining the dried product at 600° ...

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Abstract

The invention provides a copper-zinc composite oxide, its preparation method and use. The morphology of the copper-zinc composite oxide is microspheres assembled from nanosheets. The components of the nanosheets include ZnO and CuO, and ZnO is in CuO. Evenly dispersed in the medium, the mass percentage of ZnO is 1% to 20%, and the mass percentage of CuO is 80% to 99%. The copper-zinc composite oxide provided by the invention is directly synthesized in one step and is simple to operate. It avoids the shortcomings of the template method of needing to synthesize microsphere templates first and does not require any organic surfactant or auxiliary energy, thus reducing reaction costs and energy consumption. It is environmentally friendly, has easy-to-control reaction conditions, good reproducibility, and is suitable for industrial-scale production; the copper-zinc composite oxide is used as a catalyst in the "direct method" synthesis of M2 monomer reaction, and can achieve M2 selectivity ≥ 89.0% , Silicon powder raw material conversion rate ≥ 30.0%.

Description

technical field [0001] The invention belongs to the technical field of inorganic materials, and relates to a copper-zinc composite oxide, its preparation method and application, in particular to a copper-zinc composite oxide microsphere catalyst with a special porous structure, its preparation method and its use in the synthesis of Catalyst for Methyldichlorosilane. Background technique [0002] Composite metal oxides, as a new multifunctional inorganic fine material, have broad application prospects. Among them, the combination of CuO, which is a p-type semiconductor metal oxide with a narrow band gap, and ZnO, an n-type semiconductor metal oxide with a wide band gap, can effectively improve the electronic band structure of the sample, thereby improving the physical and chemical properties of the sample, making it It has potential application value in catalysis, photocatalysis and photoelectric devices. [0003] At present, the main production methods of CuO / ZnO composite...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/80B01J35/10B01J35/08C07F7/16
CPCC07F7/16B01J23/80B01J35/40B01J35/51B01J35/60
Inventor 苏发兵张煜纪永军李晶刘合之王光娜朱永霞谭强强
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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