Preparation method of metal-nitrogen-doped porous carbon microspheres

A nitrogen-doped porous carbon and nitrogen-doped carbon technology is applied in the preparation/purification of carbon, which can solve the problems of easy falling off, easy decomposition, poor stability, etc., and achieves large specific surface area, simple steps, and wide selectivity. Effect

Active Publication Date: 2017-05-31
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chemical nitrogen doping refers to the existence of nitrogen atoms on the surface of carbon materials in the form of surface functional groups, providing B-base sites for materials, such as amino groups and other surface nitrogen-containing functional groups. Such nitrogen-containing functional groups are highly alkaline and prone to chemical reactions. However, its stability is poor, and it is easy to decompose and fall off at high temperature.

Method used

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  • Preparation method of metal-nitrogen-doped porous carbon microspheres
  • Preparation method of metal-nitrogen-doped porous carbon microspheres
  • Preparation method of metal-nitrogen-doped porous carbon microspheres

Examples

Experimental program
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Embodiment 1

[0033] (1) Preparation of 4VP / absolute ethanol solution: at room temperature, take 1.07ml of 4VP monomer and add it to 250ml of absolute ethanol, and magnetically stir to dissolve 4VP to obtain a 4VP / absolute ethanol solution with a concentration of 0.04mol / L for later use .

[0034] (2) Preparation of FeCl 3 / absolute ethanol solution: take 1.62g FeCl 3 Dissolve in 250ml absolute ethanol, magnetically stir to make FeCl 3 Dissolve FeCl with a concentration of 0.04mol / L 3 / absolute ethanol solution for use.

[0035] (3) Fe 3+ - Preparation of organic microspheres: under magnetic stirring conditions at room temperature, take 25ml FeCl 3 / absolute ethanol solution was added to 100ml 4VP / absolute ethanol solution, molar ratio Fe 3+ : 4VP=0.25; react for 12 hours, form a stable complex precipitation, then centrifuge, dry at 60°C for 12 hours to get Fe 3+ -Organic microspheres (Fe 3+ -4VP-0.25°C).

[0036] (4) Carbonization: the Fe 3+ -4VP-0.25 is placed in a quartz bo...

Embodiment 2

[0042] (1) Preparation of 4VP / absolute ethanol solution: at room temperature, take 1.07ml of 4VP monomer and add it to 250ml of absolute ethanol, and magnetically stir to dissolve 4VP to obtain a 4VP / absolute ethanol solution with a concentration of 0.04mol / L for later use .

[0043] (2) Preparation of CuCl 2 / absolute ethanol solution: take 1.34g CuCl 2 Dissolve in 250ml absolute ethanol, magnetically stir to make CuCl 2 Dissolve CuCl with a concentration of 0.04mol / L 2 / absolute ethanol solution for use.

[0044] (3)Cu 2+ - Preparation of organic microspheres: under magnetic stirring conditions at room temperature, take 25ml CuCl 2 / absolute ethanol solution was added to 100ml 4VP / absolute ethanol solution, molar ratio Cu 2+ : 4VP=0.25; after 6 hours of reaction, a stable complex precipitate is formed, and then centrifuged, and vacuum dried at 60°C for 12 hours to obtain Cu 2+ -Organic microspheres (Cu 2+ -4VP-0.25).

[0045] (4) Carbonization: Cu 2+ -4VP-0.25 ...

Embodiment 3

[0049] (1) Preparation of 4VP / absolute ethanol solution: at room temperature, take 1.07ml of 4VP monomer and add it to 250ml of absolute ethanol, and magnetically stir to dissolve 4VP to obtain a 4VP / absolute ethanol solution with a concentration of 0.04mol / L for later use .

[0050] (2) Preparation of MgCl 2 / absolute ethanol solution: take 0.95g MgCl 2 Dissolve in 250ml of absolute ethanol, stir magnetically to make MgCl 2 Dissolved to obtain MgCl with a concentration of 0.04mol / L 2 / absolute ethanol solution for use.

[0051] (3)Mg 2+ - Preparation of organic microspheres: under the condition of magnetic stirring at room temperature, take 50ml MpCl 2 / dehydrated ethanol solution is added to 100ml 4VP / dehydrated ethanol solution, molar ratio Mg 2+ : 4VP=0.5; react for 24 hours, form a stable complex precipitation, and then centrifuge, vacuum dry at 60°C for 12 hours to get Mg 2+ -Organic microspheres (Mg 2+ -4VP-0.5).

[0052] (4) Carbonization: the Mg 2+ -4VP-0....

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Abstract

The invention discloses a preparation method of metal-nitrogen-doped porous carbon microspheres. According to the preparation method, a 4VP (4-vinyl pyridine) monomer is taken as a carbon and nitrogen source, different metal salts are taken as an initiator, a coordination agent, a catalyst and a template agent, firstly, the 4VP monomer is polymerized at the normal temperature by utilizing the metal salts as the initiating agent, a metal-coordination structure is formed by metal ions and nitrogen atoms in 4VP molecules, and metal-organic matter microspheres are formed; then metal in the microspheres has functions of the catalyst and the template agent at the high temperature, so that organic matter is converted into carbon, a spherical structure is reserved, and the metal-nitrogen-doped porous carbon microspheres are obtained after acid pickling. Selectivity of metal sources is high, steps are simple, and the prepared nitrogen-doped porous carbon material is large in specific surface area and high in nitrogen content. By means of large specific surface area and high nitrogen content, the material has huge application prospect in the fields of energy storage and conversion, catalysis and environment protection.

Description

technical field [0001] The invention belongs to the technical field of functional materials, and in particular relates to a preparation method of metal-nitrogen doped porous carbon microspheres. Background technique [0002] Porous carbon has the characteristics of wide source of raw materials, good physical and chemical stability, large specific surface area, large pore volume, good electrical conductivity, high temperature resistance, acid and alkali resistance, etc. It is widely used in electrode materials, catalysis and catalyst carriers, gas adsorption separation and water Purification and many other fields. Studies have shown that the main factors affecting the performance of porous carbon are pore structure and surface chemical properties. In recent years, the research on the surface chemical properties of porous carbon has become a hot spot, mainly by introducing heteroatoms into the carbon skeleton, such as N, O, B, S, P, etc. The introduction of heteroatoms into ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/05
CPCC01P2002/85C01P2002/90C01P2004/03C01P2004/80C01P2006/12C01P2006/14
Inventor 韩生付宁韦焕明陈海军蔺华林冯晨萁江新泽兰国贤刘金宝喻宁波余伟萍何抗抗马文飞钱炜刘玉萍任济夫
Owner SHANGHAI INST OF TECH
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