Method for one-step synthesis of metal oxide loaded transition metal carbide

A technology of transition metals and oxides, which is applied in the direction of carbide, manganese oxide/manganese hydroxide, cobalt oxide/cobalt hydroxide, etc., and can solve the problems of using hydrofluoric acid, etc.

Inactive Publication Date: 2020-01-14
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims at the technical defects of the prior art, and provides a method for synthesizing metal oxide-supported transition metal carbides in one step, so as to solve the technical problem that hydrofluoric acid needs to be used in conventional synthesis methods in the prior art

Method used

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  • Method for one-step synthesis of metal oxide loaded transition metal carbide
  • Method for one-step synthesis of metal oxide loaded transition metal carbide
  • Method for one-step synthesis of metal oxide loaded transition metal carbide

Examples

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Embodiment 1

[0029] Boil distilled water and cool to 60°C, add sodium hydroxide or potassium hydroxide to make a saturated alkaline solution, then add the raw material MAX (Ti 3 AlC 2 , Ti 2 AlC, etc.), metal oxide precursors (iron acetylacetonate, cobalt acetylacetonate, manganese acetylacetonate, etc.), hydrazine hydrate, in every 100mL of saturated alkaline solution, add 1g MAX phase, 0.5g metal oxide precursor (acetylacetonate Iron acetonate, cobalt acetylacetonate, manganese acetylacetonate, etc.), 1mL hydrazine hydrate (mass fraction: 80%), magnetically stirred for 30min, transferred the solution to a high-temperature reaction kettle, raised the temperature to 280°C, and placed it in a muffle furnace for 8h , the solution was taken out and centrifuged, washed with water until the pH of the solution was about 7, and then dried in vacuum for later use.

Embodiment 2

[0031] Boil distilled water and cool to 60°C, add sodium hydroxide or potassium hydroxide to make a saturated alkaline solution, then add the raw material MAX (Ti 3 AlC 2 , Ti 2 AlC, etc.), metal oxide precursors (iron acetylacetonate, cobalt acetylacetonate, manganese acetylacetonate, etc.), hydrazine hydrate, in every 100mL of saturated alkaline solution, add 1g MAX phase, 1g metal oxide precursor (acetylacetonate Iron, cobalt acetylacetonate, manganese acetylacetonate, etc.), 2mL hydrazine hydrate (mass fraction is 80%), magnetically stirred for 30min, transferred the solution to a high-temperature reaction kettle, raised the temperature to 280°C, and placed it in a muffle furnace for 8h. The solution was taken out and centrifuged, washed with water until the pH of the solution was about 7, dried in vacuum and then used for later use.

Embodiment 3

[0033] Boil distilled water and cool to 60°C, add sodium hydroxide or potassium hydroxide to make a saturated alkaline solution, then add the raw material MAX (Ti 3 AlC 2 , Ti 2 AlC, etc.), metal oxide precursors (iron acetylacetonate, cobalt acetylacetonate, manganese acetylacetonate, etc.), hydrazine hydrate, in every 100mL of saturated alkaline solution, add 1g MAX phase, 1.5g metal oxide precursor (acetylacetonate Iron acetonate, cobalt acetylacetonate, manganese acetylacetonate, etc.), 3mL hydrazine hydrate (mass fraction: 80%), magnetically stirred for 30min, transferred the solution to a high-temperature reaction kettle, raised the temperature to 280°C, and placed it in a muffle furnace for 8h , the solution was taken out and centrifuged, washed with water until the pH of the solution was about 7, and then dried in vacuum for later use.

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Abstract

The invention provides a method for one-step synthesis of a metal oxide loaded transition metal carbide. The method comprises following steps: preparing a saturated strong alkali solution; then addinga raw material MAX phase and a metal precursor; carrying out one-step preparation of the metal oxide loaded transition metal carbide by utilizing the reactivity of the saturated strong alkali solution to the MAX phase and pyrolysis of the metal precursor at high temperature, and on the basis, selectively adding hydrazine hydrate to regulate and control the valence state of the formed transition metal oxide metal; and uniformly stirring an obtained system, heating to 280-350 DEG C, keeping the temperature for 6-10 hours, cooling, centrifugally collecting a black solid; washing, and drying to obtain a finished product. The method is easy to operate, reaction parameters are easy to control, the metal content is controllable, the method can be used for large-scale industrial production, and the obtained metal oxide / MXenes composite material has good hydrophilicity and a large specific surface area, can be subjected to magnetic separation and has outstanding technical advantages.

Description

technical field [0001] The invention relates to the technical field of metal oxide composite materials, in particular to a method for synthesizing metal oxide-supported transition metal carbides in one step. Background technique [0002] Transition metal carbides, nitrides and carbonitrides (MXenes) are members of a new family of two-dimensional materials. And excellent hydrophilic properties, it can be used to support metal oxides as catalysts, so it has good application potential in energy storage and conversion, electromagnetic shielding and other fields. [0003] The common MXenes-based metal oxide composite material is a two-step method. First, the MXenes base material is prepared by hydrofluoric acid, and then the metal hydroxide is deposited by adjusting the pH, and then the metal oxide is loaded by high-temperature dehydration. The hydrofluoric acid used in this method will not only pollute the environment, but also pose a great health threat to the operators. In t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/04C01G51/04C01G45/02C01B32/921
CPCC01G45/02C01G49/04C01G51/04C01P2004/03C01P2004/04C01P2004/80C01B32/921
Inventor 周耐根崔宜张小勇刘美英
Owner NANCHANG UNIV
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