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Preparation method and application of heteroatom-doped metal carbon-containing material

A heteroatom and metal technology, applied in the field of preparation of metal carbonaceous materials, can solve the problems of limited degree of graphitization, limited catalytic ability, large specific surface area of ​​materials, etc., and achieves the effect of strong stability and improved electrochemical performance.

Inactive Publication Date: 2017-09-26
北京至心安科技股份有限公司
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Problems solved by technology

[0003] Patent "CN 106311152 A" (a mesoporous zeolite-like imidazolate framework material and its preparation method and application) describes a method for preparing zeolite-like imidazole by solvothermal method. The material has a large specific surface area but has no high-efficiency Catalytically active sites and therefore unsuitable for electrode materials
[0004] Patent "CN 104817577 A" (an efficient and simple preparation method and catalytic application of zeolite-like imidazole framework ZIF-8 crystals with different shapes) describes a method for preparing zeolite-like imidazole framework ZIF-8 crystals in methanol solution, This method prepares ZIF-8 with different morphologies and applies it to catalysis, but the zeolite-like imidazole material itself only contains N as a heteroatom and has no other heteroatoms, so its catalytic ability is limited.
[0005] Patent "CN 103213968 B" (a heteroatom-doped carbon material and its preparation method and application) describes a heteroatom-doped Although heterogeneous carbon materials have more heteroatoms, their degree of graphitization is limited, and the electrochemical performance of composite materials of heteroatoms and carbon is often not as good as that of metal-containing materials.

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  • Preparation method and application of heteroatom-doped metal carbon-containing material
  • Preparation method and application of heteroatom-doped metal carbon-containing material
  • Preparation method and application of heteroatom-doped metal carbon-containing material

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[0055] Part of the specific embodiments of the present invention provides a method for preparing a heteroatom-doped metal carbonaceous material, the preparation method comprising the following steps:

[0056] (1) Dissolving metal ions, imidazole ligand compounds and water-soluble polymers in solvent A;

[0057] (2) adding the graphene oxide solution to the solution in step (1) after a period of time;

[0058] (3) mixing and stirring the solutions of steps (1) and (2), separating the solid and liquid, and calcining the obtained precipitate under the protection of an inert gas to obtain a nitrogen-doped metal carbonaceous material;

[0059] (4) Put the nitrogen-doped metal carbonaceous material obtained in step (3) into the high-temperature zone of the double-temperature-controlled vacuum tube furnace, and place the material containing heteroatoms in the low-temperature zone, and heat it under high temperature with inert protective gas and low pressure. calcining to obtain a he...

Embodiment 1

[0061] A method for preparing a three-dimensional cobalt-carbon material doped with boron and nitrogen atoms, the preparation method comprising the following steps:

[0062] (1) Dissolve 0.5 M cobalt sulfate, 0.5 M 2-methylimidazole and 0.5 g polyacrylamide in 50 mL acetonitrile solvent, and stir at 200 rpm;

[0063] (2) After 30 s, add 0.1 g / L, 1 mL graphene oxide solution to the solution in step (1);

[0064] (3) Mix the solutions obtained in steps (1) and (2) and stir at a speed of 200 rpm for 1 h, then centrifuge at a speed of 10,000 rpm for 1 min to separate the solid from the liquid. Drying at 80 ℃ for 12 h, followed by calcination under nitrogen protection for 2 h, the calcination temperature was 750 ℃, and the calcination heating rate was 5 ℃ / min to obtain the nitrogen-doped cobalt carbon material N-Co / C-1;

[0065] (4) Put 1 g of the N-Co / C-1 material obtained in step (3) into the high-temperature zone of a double-temperature-controlled vacuum tube furnace for 10 min...

Embodiment 2

[0068] A method for preparing a three-dimensional cobalt-carbon material doped with fluorine, boron and nitrogen atoms, the preparation method comprising the following steps:

[0069] (1) Dissolve 0.5 M cobalt oxide, 1 M 4-nitroimidazole and 4 g polyvinylpyrrolidone in 50 mL N,N-dimethylacetamide solvent;

[0070] (2) After 60 s, add 1 g / L, 4 mL graphene oxide solution to the solution in step (1);

[0071] (3) Mix the solutions of steps (1) and (2) and stir at 200 rpm for 1.5 h, then centrifuge at 11,000 rpm for 2 min to separate the solid from the liquid. Drying at ℃ for 14 h, calcining for 3 h under the protection of nitrogen, the calcination temperature is 700 ℃, and the calcination heating rate is 6 ℃ / min, and the nitrogen-doped three-dimensional cobalt carbon material N-Co / C-2 is obtained;

[0072] (4) Put the N-Fe / C-4 material obtained in step (3) into the high-temperature zone of a double-temperature-controlled vacuum tube furnace for 20 min. The temperature in the hig...

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Abstract

The invention relates to a preparation method and application of a heteroatom-doped metal carbon-containing material. The preparation method comprises the following steps: dissolving metal ions, an imidazole ligand compound and a water-soluble high molecular polymer into a solvent A respectively; adding a graphene oxide solution after a period of time; mixing and stirring; carrying out solid-liquid separation and calcining obtained sediment under the protection of inert gas to obtain a nitrogen-doped metal carbon-containing material; doping the nitrogen-doped metal carbon-containing material with other heteroatoms under a chemical vapor deposition condition; carrying out high-temperature calcining under inert protection gas and low pressure so as to obtain the heteroatom-doped metal carbon-containing material. The material provided by the invention can be used as an electrode material and is used for heavy metal detection, organic matter detection, active carbon detection or oxygen reduction reaction and the like.

Description

technical field [0001] The invention relates to the field of material preparation, in particular to a preparation method and application of a heteroatom-doped metal carbonaceous material. Background technique [0002] Recently, as a new type of material, zeolitic imidazolate frameworks (ZIFs) cracked at high temperature have been widely used in various electrochemical reactions, because compared with commercial Pt / C, IrO2 and other materials, its It has more stable performance. ZIFs are a series of porous crystals with a three-dimensional topology, which are formed through the coordination between transition metals and imidazole ligands, and belong to Metal-Organic Frameworks (MOFs). The "M-Im-M" bond is formed between the metal and the ligand in ZIFs, and the included angle is consistent with that of zeolite SiO2, so it is named as the zeolite-like imidazole structure. Due to the existence of these rings, the formed molecular sieves form standard channels or cages. [00...

Claims

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Application Information

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IPC IPC(8): C01G9/00C01G49/00C01G51/00C25B1/02C25B11/04H01G11/24H01G11/30
CPCY02E60/13C01G51/00C01G9/00C01G49/00C01P2004/03C01P2004/04C01P2004/80C25B1/02C25B11/04H01G11/24H01G11/30
Inventor 李泽晖曹友錋罗扬王温博孙绍铭
Owner 北京至心安科技股份有限公司
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