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Preparation method of hollow copper pipe rich in three-dimensional micropores

A technology of hollow copper tubes and micropores, applied in chemical instruments and methods, electrodes, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of incomplete removal of impurities, achieve excellent product selectivity, and be easily Effects with simple storage and steps

Active Publication Date: 2019-07-12
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

On this basis, the three-dimensional microporous hollow copper tubes rich in three-dimensional micropores can be directly prepared by simple subsequent heat treatment in a reducing atmosphere, which can solve the shortcomings of the traditional preparation methods that cannot completely remove impurities and direct large-scale synthesis at low cost.

Method used

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  • Preparation method of hollow copper pipe rich in three-dimensional micropores
  • Preparation method of hollow copper pipe rich in three-dimensional micropores
  • Preparation method of hollow copper pipe rich in three-dimensional micropores

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preparation example Construction

[0031] In the specific implementation process, the present invention provides a preparation method rich in three-dimensional microporous hollow copper tubes, using commercial copper tubes as the starting material, soaking them in an acidic solution of a certain concentration for a short time, and then using deionized water Wash and dry, place on a burning boat, put into a muffle furnace for heat treatment in an oxygen-containing atmosphere, and obtain the intermediate product CuO x , and then placed in a tube furnace for heat treatment in a reducing atmosphere to obtain a hollow copper tube rich in three-dimensional micropores. By changing the reaction temperature in the heat treatment process, the pore size of the hollow copper tube rich in three-dimensional micropores is regulated through the heat treatment process at different temperatures. The specific features are:

[0032] 1. The starting materials used are one or more of various shapes of commercial metal copper, copper...

Embodiment 1

[0040] In this embodiment, the commercial copper tube is cut into a cylinder with a diameter of 1cm × 2cm (in this embodiment, the wall thickness of the commercial copper tube is 0.15mm), and it is placed in a 15mL container containing 0.65M (molar concentration) h + (In this example, H + Soak it in an aqueous solution of HCl for 5-10 seconds, wash it with deionized water and dry it under a nitrogen atmosphere, and then put it into a muffle furnace and process it in an air atmosphere at 900°C for 0.5 hours to obtain an intermediate product CuO with a rough surface. x (0≤x<2), mainly composed of CuO, accounting for about 100wt%. The intermediate product was put into a tube furnace and treated in an ammonia atmosphere at 900°C for 1 hour to obtain a hollow copper tube rich in three-dimensional microporous structure.

[0041] Such as figure 1 Shown, the XRD diffraction peak of used starting material commercial copper tube; figure 2 As shown, the surface of the commercial cop...

Embodiment 2

[0043] In this embodiment, the commercial copper tube is cut into a cylinder with a diameter of 1cm × 2cm (in this embodiment, the wall thickness of the commercial copper tube is 0.15mm), and it is placed in a 15mL container containing 0.65M (molar concentration) h + (In this example, H + Soak it in an aqueous solution of HCl for 5-10 seconds, wash it with deionized water and dry it under a nitrogen atmosphere, and then put it into a muffle furnace and process it in an air atmosphere at 900°C for 0.5 hours to obtain an intermediate product CuO with a rough surface. x (0≤x<2), mainly composed of CuO, accounting for about 100wt%. The intermediate product was put into a tube furnace and treated in an ammonia atmosphere at 400°C for 1 hour to obtain a hollow copper tube rich in three-dimensional microporous structure.

[0044] Such as Figure 9 As shown, in the hollow copper tube rich in three-dimensional micropore structure, the diameter of the three-dimensional micropores is ...

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Abstract

The invention relates to the field of metal porous framework structural materials, in particular to a preparation method of a hollow copper pipe rich in three-dimensional micropores. According to themethod, a commercial copper pipe is taken as a starting material, the copper pipe is cleaned by deionized water, dried and placed in a combustion boat after being soaked in an acid solution with certain concentration for a short time, the combustion boat is put in a muffle furnace and subjected to heat treatment in the oxygen atmosphere, the copper pipe is transformed into CuOx, CuOx is placed ina tube furnace and subjected to heat treatment in the reducing atmosphere, the hollow copper pipe rich in the three-dimensional micropores is obtained, and the pore size of the micropore structure canbe regulated by changing reaction temperature in a heat treatment process. The hollow copper pipe rich in the three-dimensional micropores is directly prepared from the commercial copper pipe as thestarting material, a large quantity of pores are formed in the surface and bulk phase of the hollow copper pipe, the pore size of the micropore structure can be changed by regulating temperature variables, so that effective regulation for the preparation process of the hollow copper pipe rich in the three-dimensional micropores can be realized effectively, and the defects that impurities are introduced and direct large-scale synthesis cannot be realized in a traditional preparation method can be overcome.

Description

technical field [0001] The invention relates to the field of metal porous skeleton structure materials, in particular to a method for preparing hollow copper tubes rich in three-dimensional micropores. Background technique [0002] Metallic copper electrocatalytic materials have many advantages such as high efficiency, low cost, high thermodynamic stability, and environmental friendliness. They are one of the most competitive materials among many electrocatalytic materials and can be widely used in electrocatalytic HER, OER, and carbon dioxide reduction. The matrix material, etc., has very good commercial value. Especially, hollow copper tubes rich in three-dimensional micropores can increase the number of active sites in catalytic reactions due to their advantages of good permeability, high specific surface area, high porosity, and stable shape. However, the traditional methods for preparing metal copper with three-dimensional microporous structure are very limited, mainly...

Claims

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Application Information

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IPC IPC(8): C25B11/06C22C1/08C22C9/00B01J23/72
CPCC25B11/04C22C1/08C22C9/00B01J23/72B01J35/33
Inventor 刘岗秦浩杨志卿叶恒强成会明
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI