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A preparation method of iron-nitrogen co-doped magnetic porous graphitized nano-carbon airgel

A technology of porous graphite and carbon aerogel, applied in nano-carbon, chemical instruments and methods, carbon compounds, etc., can solve the problems of high risk, long preparation period, environmental pollution, etc., to reduce burden and achieve good electrocatalytic oxygen reduction. active effect

Active Publication Date: 2020-10-13
WUHAN UNIV
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  • Description
  • Claims
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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

Method used

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  • A preparation method of iron-nitrogen co-doped magnetic porous graphitized nano-carbon airgel
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  • A preparation method of iron-nitrogen co-doped magnetic porous graphitized nano-carbon airgel

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Embodiment 1

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

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

[0028] 2) carbonization: put the ...

Embodiment 2

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

[0032] 1) CS-Fe 3+ Preparation of chelate airgel: 3g chitosan (CS, degree of deacetylation 88%, molecular weight about 600000) was dissolved in 3wt% HAc solution with a mass fraction of 3wt%, after being completely dissolved, 10mL was added to dissolve Iron salt solution with a certain quality of ferric nitrate, mix well, continue to stir for half an hour, let it stand for several hours to remove bubbles, and obtain a uniform and stable red-brown viscous transparent solution, pour it into a 24-well plate, and freeze it at -75°C for 10h Afterwards, vacuum freeze-drying to remove moisture, to obtain CS-Fe 3+ Chelate airgel (CS-Fe 3+ aerogel). According to chitosan after roasting at 750 ℃, the mass of the residue is about 36% of the initial mass, so the mass of iron nitrate added is calculated based on the ratio of the mass of added Fe element...

Embodiment 3

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

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

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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 method for preparing 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, and are widely sourced, rich in variety, and eco-friendly , as an adsorbent, catalyst, electrode material, has been widely used in aerospace, communications, nuclear industry, metallurgy, chemical industry, medical treatment and other fields, and is called "the fourth type of industrial material". 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-metal element N atoms in nanocarbon materials can affect the sp...

Claims

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Application Information

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Patent Type & Authority Patents(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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