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Preparation method of iron-nitrogen co-doped magnetic porous graphitized nano carbon aerogel

A technology of porous graphite and carbon aerogel, applied in nano-carbon, chemical instruments and methods, carbon compounds, etc., can solve the problems of long preparation cycle, high risk, complicated procedures, etc., achieve good electrocatalytic oxygen reduction activity, reduce burden effect

Active Publication Date: 2019-08-13
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above-mentioned method of introducing nitrogen into carbon materials has the following problems: 1) the preparation period is long, the procedure is cumbersome, and it is difficult to realize industrialization; 2) the use of petrochemical preparations as precursors has the risk of environmental pollution; 3) expensive large-scale instruments, high temperatures are required High pressure processing, high risk and high cost

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  • Preparation method of iron-nitrogen co-doped magnetic porous graphitized nano carbon aerogel
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  • Preparation method of iron-nitrogen co-doped magnetic porous graphitized nano carbon aerogel

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Embodiment 1

[0026] A preparation method of iron-nitrogen co-doped magnetic porous graphitized nano-carbon aerogel, comprising the following steps:

[0027] 1) CS-Fe 3+ Preparation of chelate aerogel: Dissolve 3g chitosan (CS, deacetylation degree 88%, molecular weight about 600000) in 110mL 2wt% HAc solution, after complete dissolution, add 10mL dissolved FeCl with a certain mass 3 ·6H 2 O iron salt solution, mix well, continue to stir and react for half an hour, let stand for several hours to remove bubbles, obtain a uniform and stable red-brown viscous transparent solution, pour into a 24-well plate, freeze at -75 ℃ for 12 hours, and then freeze in vacuum Dry to remove moisture to obtain CS-Fe 3+ Chelate aerogel (CS-Fe 3+ aerogel). According to the residual mass of chitosan after calcination at 800 °C is about 36% of the initial mass, the addition of FeCl is calculated based on the ratio of the mass of Fe element added to the residual mass of chitosan. 3 ·6H 2 quality of O.

[00...

Embodiment 2

[0031] A preparation method of iron-nitrogen co-doped magnetic porous graphitized nano-carbon aerogel, comprising the following steps:

[0032] 1) CS-Fe 3+ Preparation of chelate aerogel: Dissolve 3g chitosan (CS, deacetylation degree 88%, molecular weight about 600000) in 3wt% HAc solution with a mass fraction of 3wt%, after complete dissolution, add 10mL to dissolve The iron salt solution with a certain quality of ferric nitrate, mix well, continue to stir and react for half an hour, and let stand for several hours to remove foam to obtain a homogeneous and stable red-brown viscous and transparent solution, pour it into a 24-well plate, and freeze at -75 ℃ for 10 hours Then, vacuum freeze-drying to remove moisture to obtain CS-Fe 3+ Chelate aerogel (CS-Fe 3+ aerogel). According to the residual mass of chitosan after calcination at 750℃ is about 36% of the initial mass, the mass of ferric nitrate added is calculated by the ratio of the mass of Fe element added to the resid...

Embodiment 3

[0036] A preparation method of iron-nitrogen co-doped magnetic porous graphitized nano-carbon aerogel, comprising the following steps:

[0037] 1) CS-Fe 3+ Preparation of chelate aerogel: Dissolve 3g chitosan (CS, deacetylation degree 88%, molecular weight about 600000) in a 4wt% HAc solution with a mass fraction of 4wt%, after complete dissolution, add 10mL to dissolve There is a certain quality of FeCl 3 ·6H 2 O iron salt solution, mix well, continue to stir and react for half an hour, let stand for several hours to remove bubbles, obtain a uniform and stable red-brown viscous transparent solution, pour it into a 24-well plate, freeze at -75 ℃ for 11 hours, and then freeze in vacuum Dry to remove moisture to obtain CS-Fe 3+ Chelate aerogel (CS-Fe 3+ aerogel). According to the residue mass of chitosan after calcination at 700℃ is about 36% of the initial mass, the addition of FeCl is calculated based on the ratio of the mass of Fe element added to the residual mass of ch...

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Abstract

The invention relates to the technical field of carbon aerogel, in particular to a preparation method of iron-nitrogen co-doped magnetic porous graphitized nano carbon aerogel. The preparation methodcomprises the following steps: (1) dissolving chitosan in an acetic acid solution, adding a trivalent iron salt solution, executing stirring until the reaction is completed to obtain a uniform and stable red-brown viscous transparent solution, and executing vacuum freeze drying to obtain chitosan-Fe<3+> chelate aerogel; (2) executing carbonization: obtaining a black aerogel carbonized sample; (3)executing activation: obtaining the iron-nitrogen co-doped magnetic porous graphitized nano carbon aerogel. The chelate formed by the nitrogen-containing high molecular material chitosan and ferric salt is used as a carbon source, a nitrogen source and an iron source to prepare the iron-nitrogen co-doped magnetic porous graphitized nano carbon aerogel, the iron-nitrogen co-doped magnetic porous graphitized nano carbon aerogel has large specific surface area and an ideal pore structure and can present good electrocatalytic oxygen reduction activity, electric double-layer super capacitance performance and organic dye adsorption performance by adjusting the iron content.

Description

technical field [0001] The invention relates to the technical field of carbon aerogels, in particular to a preparation method of iron-nitrogen co-doped magnetic porous graphitized nano-carbon aerogels. Background technique [0002] New nano-carbon materials, such as carbon aerogels, carbon nanotubes, graphene, etc., have the advantages of large specific surface area, good electrical conductivity, chemical stability and mechanical properties, as well as a wide range of sources, rich varieties, and ecological friendliness. , as adsorbents, catalysts, electrode materials, has been widely used in aerospace, communications, nuclear industry, metallurgy, chemical, medical and other fields, known as the "fourth type of industrial materials", carbon material technology is also regarded as a solution to the energy crisis and one of the most effective technologies for environmental pollution from fossil fuels. Doping non-metallic element N atoms in carbon nanomaterials can affect the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/205C01B32/15
CPCC01B32/15C01B32/205
Inventor 曹启花肖玲葛一卓
Owner WUHAN UNIV
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