Metal monatomic/N co-doped 3D (Three Dimensional) structure nano porous carbon and preparation method thereof

A nanoporous carbon, co-doping technology, applied in nanocarbon, nanotechnology for materials and surface science, nanotechnology, etc., to achieve the effects of high nitrogen content, short reaction time, and simple preparation method

Active Publication Date: 2019-03-26
ANHUI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there is no literature report on the preparation of bottlebrush-like cellulose-polyacrylonitrile block polymers by atom transfer radical polymerization starting from biomass cellulose, which is used as a precursor, adsorbed by metal ions, carbonized, and directly prepared A report on single-atom metal / N co-doped 3D structured nanoporous carbon

Method used

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  • Metal monatomic/N co-doped 3D (Three Dimensional) structure nano porous carbon and preparation method thereof
  • Metal monatomic/N co-doped 3D (Three Dimensional) structure nano porous carbon and preparation method thereof
  • Metal monatomic/N co-doped 3D (Three Dimensional) structure nano porous carbon and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Example 1: Monoatomic iron / N co-doped 3D structure nanoporous carbon, the schematic diagram of its preparation process is shown in the figure:

[0049] First, dissolve 0.5 g of cellulose in 10.0 g of 1-allyl-3-methylimidazole to form a uniform solution; then add a certain amount of 2-bromoisobutyryl bromide and then proceed to the heating reaction, wherein the halogenation reagent 2 - The molar ratio of bromoisobutyryl bromide to the hydroxyl group in cellulose is 0.5, and the reaction solution is repeatedly precipitated and purified to obtain brominated cellulose polymer;

[0050] Dissolve 10mg of brominated cellulose polymer in N,N-dimethylformamide, then add 20ml of acrylonitrile, 10mg of copper bromide and 10mg of 2,2'-bipyridine, deoxygenate with nitrogen, and freeze with liquid nitrogen , add 30 mg of cuprous bromide, heat up to 60°C and polymerize for 5-12 hours, add styrene monomer, continue the polymerization for 8-24 hours, measure the monomer conversion rate ...

Embodiment 2

[0057] Example 2: Monoatomic Fe / N co-doped 3D structured nanoporous carbon

[0058] First dissolve 0.5g of cellulose in 10.0g of 1-ethyl-3-methylimidazolium bromide to form a uniform solution; add a certain amount of 2-bromo-2-methylpropionyl chloride and then carry out the temperature rise reaction, wherein The molar ratio of the halogenation reagent 2-bromo-2-methylpropionyl chloride to the hydroxyl group in the cellulose is 1, and the reaction solution is repeatedly precipitated and purified to obtain a brominated cellulose polymer;

[0059] Dissolve 200 mg of brominated cellulose polymer in dimethyl sulfoxide, then add 20 ml of acrylonitrile, 3 mg of copper chloride and 200 mg of 4,4'-dinonyl-2,2'-bipyridine, and remove the After oxygen and liquid nitrogen freezing, add 30 mg of cuprous chloride, heat up to 60 ℃, polymerize for 5-12 hours, add styrene monomer, continue polymerization for 8-24 hours, and measure the monomer by nuclear magnetic resonance (NMR) After the con...

Embodiment 3

[0063] Example 3: Single atom cobalt / N co-doped 3D structured nanoporous carbon

[0064] First, dissolve 0.5g of cellulose in 10.0g of 1-ethyl-3-methylimidazolium bromide to form a uniform solution; add a certain amount of 4-chlorobutyryl chloride and then proceed to the heating reaction, in which the halogenation reagent 4-chlorobutyryl The molar ratio of butyryl chloride to the hydroxyl group in the cellulose is 2, and the reaction solution is repeatedly precipitated and purified to obtain a chlorinated cellulose polymer;

[0065] Dissolve 200 mg of chlorinated cellulose polymer in dimethyl sulfoxide, then add 20 ml of acrylonitrile, 3 mg of copper chloride and 200 mg of 4,4'-dinonyl-2,2'-bipyridine, and remove the After oxygen and liquid nitrogen freezing, add 27 mg of cuprous chloride, heat up to 60 ℃, polymerize for 5-12 hours, add styrene monomer, continue polymerization for 8-24 hours, and measure the monomer by nuclear magnetic resonance (NMR) After the conversion rat...

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Abstract

The invention discloses a preparation method of metal monatomic/N co-doped 3D (Three Dimensional) structure nano porous carbon. The metal monatomic/N co-doped 3D structure nano porous carbon is prepared by taking a bottle-brush-shaped cellulose polyacrylonitrile block polymer as a template and adsorbing metal ions; the preparation method comprises the following steps: dissolving cellulose in ionicliquid to form a uniform solution; then adding a halogenation reagent and carrying out temperature-rising reaction; dissolving a halogenated cellulose polymer into a polar organic solvent; carrying out grafted polymerization of an acrylonitrile monomer and a second monomer in sequence by adopting an atom transfer radical polymerization method; adding a metal ion solution into a solution of the bottle-brush-shaped cellulose polyacrylonitrile block polymer; after sufficiently adsorbing, carbonizing to obtain the metal monatomic/N co-doped 3D structure nano porous carbon. The 3D structure nano porous carbon prepared by the preparation method has the advantages of high nitrogen content, controllable doping amount of monatomic metal and large specific surface area and has a wide application prospect.

Description

technical field [0001] The invention relates to the technical field of nanomaterials, in particular to a metal single atom / N co-doped 3D nanoporous carbon and a preparation method thereof. Background technique [0002] Nanoporous carbon materials have large specific surface area, unique pore structure, good heat and corrosion resistance, excellent biocompatibility, and excellent mechanical and electrochemical properties. Controlled release, supercapacitor and other fields have broad application prospects. Due to the depletion of fossil energy and the deterioration of the natural environment, people have begun to vigorously develop sustainable energy storage and conversion systems. However, the kinetics of the cathode reaction of these energy conversion and storage devices are slow, and catalysts are often required to enhance the activity of the reaction. The study found that platinum-based electrocatalysts are currently the catalysts with better performance for oxygen redu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/15B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B32/15
Inventor 张建安王苗苗吴庆云吴明元杨建军刘久逸
Owner ANHUI UNIVERSITY
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