Preparation method of metal-loaded nitrogen-doped bulk porous carbon material

A porous carbon material and block technology, which is applied in the field of preparation of metal-loaded nitrogen-doped block porous carbon materials, can solve problems such as difficult circulation and separation, and achieve high specific surface area, high porosity, and wide application prospects Effect

Inactive Publication Date: 2018-11-30
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, the size of conventional carbon materials is mostly low-dimensional st

Method used

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  • Preparation method of metal-loaded nitrogen-doped bulk porous carbon material
  • Preparation method of metal-loaded nitrogen-doped bulk porous carbon material
  • Preparation method of metal-loaded nitrogen-doped bulk porous carbon material

Examples

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Embodiment 1

[0028] A method for preparing a metal-loaded nitrogen-doped bulk porous carbon material:

[0029] (1) Take 10.0 g of cellulose nanowire suspension with a solid content of 3.0 wt.%, add 3.0 wt.% chitosan acetic acid solution (10.0 g), cobalt acetate tetrahydrate (46.7 mg), and stir magnetically at 60° C. for 4 h;

[0030] (2) Place the suspension prepared in (1) into liquid nitrogen for quick freezing, the cooling time is 10 minutes, and then freeze-dry in a freeze dryer for 30 hours to obtain a cobalt-loaded natural polymer-based porous material;

[0031] (3) Put the porous material prepared in (2) in an atmosphere furnace, under the condition of nitrogen protection, the heating rate is 5°C / min to 800°C, and keep it for 3h, to obtain cobalt-supported nitrogen-doped massive porous carbon Co-N / C 0-800(M-N / Cx y-z: M is the loaded metal element, x is the natural polysaccharide polymer, where x is the default raw material is cellulose nanowire, y is the mass percentage of ammonium...

Embodiment 2

[0039] A method for preparing a metal-loaded nitrogen-doped bulk porous carbon material:

[0040] (1) Get 10.0g solid content 3.0wt.% cellulose nanowire suspension, add 3.0wt.% chitosan acetic acid solution (10.0g), cobalt acetate tetrahydrate (46.7mg), ammonium chloride (0.3g) , 60 ℃ magnetic stirring for 4h;

[0041] (2) Place the suspension prepared in (1) into liquid nitrogen for quick freezing, the cooling time is 10 minutes, and then freeze-dry in a freeze dryer for 30 hours to obtain a cobalt-loaded natural polymer-based porous material;

[0042] (3) Put the porous material prepared in (2) in an atmosphere furnace, under the condition of nitrogen protection, the heating rate is 5°C / min to 800°C, and keep it for 3h, to obtain cobalt-supported nitrogen-doped massive porous carbon Co-N / C 50-800.

[0043] Depend on image 3 It shows that the prepared Co-N / C 5-800 cobalt nanoparticles are embedded in the porous carbon surface, and there are a lot of holes on the surface ...

Embodiment 3

[0050] A method for preparing a metal-loaded nitrogen-doped bulk porous carbon material:

[0051] (1) Take 10.0g solid content 3.0wt.% cellulose nanowire suspension, add 3.0wt.% chitosan acetic acid solution (10.0g), nickel chloride hexahydrate (217.0mg), ammonium chloride (0.3g ), stirred at room temperature for 12h;

[0052] (2) Place the suspension prepared in (1) into liquid nitrogen for quick freezing, the cooling time is 10 minutes, and then freeze-dry in a freeze dryer for 30 hours to obtain a nickel-loaded natural polymer-based porous material;

[0053] (3) Put the porous material prepared in (2) in an atmosphere furnace, under the condition of nitrogen protection, the heating rate is 5°C / min to 800°C, and keep it warm for 3h to obtain nickel-supported nitrogen-doped bulk porous carbon Ni-N / C 50-800.

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Abstract

The invention discloses a preparation method of a metal-loaded nitrogen-doped bulk porous carbon material. The preparation method comprises: mixing a natural polysaccharide polymer solution or suspension, an inorganic ammonium salt and a metal salt and carrying out freeze-drying to obtain a natural polysaccharide polymer porous material and carrying out high temperature carbonization on the natural polysaccharide polymer porous material to obtain the metal-loaded nitrogen-doped bulk porous carbon material. The inorganic ammonium salt is used as a pore-foaming agent and a nitrogen source and isheated to decompose and form pores on the surface of a base and the ammonia gas generated by the decomposition reacts with a carbon matrix at a high temperature so that the metal-loaded nitrogen-doped bulk porous carbon material is formed. The metal-loaded nitrogen-doped bulk porous carbon material has the advantages of high specific surface area, high porosity and low density, and has wide application prospects in the fields of energy, catalytic synthesis, gas adsorption, oil-water separation and the like.

Description

technical field [0001] The invention relates to a method for preparing a metal-loaded nitrogen-doped bulk porous carbon material, which belongs to the technical field of metal-loaded materials. Background technique [0002] Porous carbon materials are an important class of raw materials, which have a wide range of applications in the fields of gas adsorption, oil-water separation, energy, and catalyst supports. Metal-loaded nitrogen-doped carbon-based materials, because the introduction of nitrogen atoms can effectively adjust the acidity and alkalinity, charge distribution, and charge transfer ability of the matrix material, thereby improving the application performance of metal-loaded carbon materials. The preparation of conventional metal-supported nitrogen-doped carbon materials mainly includes two methods: 1. Using nitrogen-containing microorganisms, polymers, and organic molecules as ligands to stabilize metal ions (such as polyacrylonitrile, urea, melamine, thiourea, ...

Claims

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Application Information

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IPC IPC(8): C01B32/05C01B32/342
CPCC01B32/05C01B32/342
Inventor 隋晓锋张聪聪王碧佳毛志平徐红张琳萍钟毅
Owner DONGHUA UNIV
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