A large-scale production method of nitrogen-rich and phosphorus-doped amorphous carbon/graphite carbon nanocomposite powder

A nanocomposite, amorphous carbon technology, applied in the direction of carbon compounds, multi-walled carbon nanotubes, nanocarbons, etc., can solve the problem of amorphous carbon's low content of heteroatom doping, low preparation purity, and difficulty in large-scale preparation and other problems, to avoid environmental conversion problems, high purity, and achieve high-efficiency production.

Active Publication Date: 2022-04-12
DALIAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The technical problems to be solved by the present invention are low doping content of heteroatoms in amorphous carbon, difficulties in large-scale preparation and low preparation purity under the premise of ensuring high doping content of nitrogen elements.

Method used

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  • A large-scale production method of nitrogen-rich and phosphorus-doped amorphous carbon/graphite carbon nanocomposite powder
  • A large-scale production method of nitrogen-rich and phosphorus-doped amorphous carbon/graphite carbon nanocomposite powder
  • A large-scale production method of nitrogen-rich and phosphorus-doped amorphous carbon/graphite carbon nanocomposite powder

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Experimental program
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Effect test

Embodiment 1

[0049] 1. Distill the aniline monomer (purity ≥ 99%, water content < 0.1%) under reduced pressure, during which nitrogen gas is continuously introduced to protect against the oxidation of aniline, and an oil bath (glycerol, glycerol) is used after decompression , heated to 100°C, treated for 0.5 hours, sealed and protected from light after distillation, and stored in the refrigerator for cooling;

[0050] 2. Multi-walled carbon nanotubes (2g, purity ≥ 95%) are put into a mixed solution containing concentrated sulfuric acid and concentrated nitric acid (the volume ratio of concentrated sulfuric acid and concentrated nitric acid is 4:1 (40ml, the mass fraction of concentrated sulfuric acid ≥ 70%; the mass fraction of concentrated nitric acid is about 68%), heated to 130°C, and the heating rate was 0.5°C / min for oil bath heating for 2.5 hours. Stirring speed is 500 rev / min);

[0051] 3. Add 40 mg of acidified CNTs / graphene oxide (purity ≥ 95%) to 200 ml of deionized water, ultra...

Embodiment 2

[0058] 1. Distill the aniline monomer (purity ≥ 99%, water content < 0.1%) under reduced pressure, during which nitrogen gas is continuously introduced to protect against the oxidation of aniline, and an oil bath (glycerol, glycerol) is used after decompression , heated to 130°C, treated for 0.2 hours, sealed and protected from light after distillation, and stored in the refrigerator for cooling;

[0059] 2. Multi-walled carbon nanotubes (2g, purity ≥ 95%) are put into a mixed solution containing concentrated sulfuric acid and concentrated nitric acid (the volume ratio of concentrated sulfuric acid and concentrated nitric acid is 4:1 (40ml, the mass fraction of concentrated sulfuric acid ≥ 70%; concentrated nitric acid mass fraction is about 68%), be heated to 160 ℃, and heating rate is 1 ℃ / min to carry out oil bath heating 1.5 hours, in this process, this high-temperature solution is condensed and refluxed and constantly stirred (continuous stirring Stirring speed is 500 rev / ...

Embodiment 3

[0067] 1. Distill the aniline monomer (purity ≥ 99%, water content < 0.1%) under reduced pressure, during which nitrogen gas is continuously introduced to protect against the oxidation of aniline, and an oil bath (glycerol, glycerol) is used after decompression , heated to 110°C, treated for 0.3 hours, sealed and protected from light after distillation, and stored in the refrigerator for cooling;

[0068] 2. Multi-walled carbon nanotubes (2g, purity ≥ 95%) are put into a mixed solution containing concentrated sulfuric acid and concentrated nitric acid (the volume ratio of concentrated sulfuric acid and concentrated nitric acid is 4:1 (40ml, the mass fraction of concentrated sulfuric acid ≥ 70%; concentrated nitric acid mass fraction is about 68%), be heated to 140 ℃, and heating rate is 0.8 ℃ / min and carries out oil bath heating 2 hours, in this process, this high-temperature solution is condensed and refluxed and constantly stirred (continuous stirring Stirring speed is 500 r...

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Abstract

The invention relates to a large-scale production method of nitrogen-rich and phosphorus-doped amorphous carbon / graphite-carbon nanocomposite powder, which belongs to the technical field of nanometer powder production. In order to realize the large-scale production of this method, the raw materials such as aniline, ammonium persulfate, phytic acid and graphitic carbon widely used in industry are combined with a simple wet chemical in-situ polymerization method and a common heat treatment method to adjust each of them. parameters, polymerize and carbonize the conductive polymer material polyaniline to increase the doping amount of nitrogen and phosphorus in the amorphous carbon / graphitic carbon composite nanopowder, and form different nanostructures by controlling the ratio of aniline monomer to graphite carbon Nitrogen-rich, phosphorus-doped amorphous carbon / graphitic carbon composite nanopowder. The beneficial effects of the invention are: the production efficiency is greatly improved, the cost is reduced, it is suitable for large-scale production, the doping content of heterogeneous atoms is high, and the prepared powder has high purity.

Description

technical field [0001] The invention relates to the technical field of nano powder production, in particular to a large-scale production method of nitrogen-rich and phosphorus-doped amorphous carbon / graphite carbon nanocomposites. Background technique [0002] Wet chemical and heat treatment processes are two of the most common processes in industrial production. Among them, the wet chemical method is a method of preparing materials through chemical reactions with the participation of a liquid phase. Although the heat treatment method only processes materials by heating and heating, the parameter settings and procedures are extremely important. It can be used for the preparation of amorphous carbon materials through the combination of wet chemical method and subsequent heat treatment process. For the preparation of amorphous carbon materials doped with heterogeneous elements (such as nitrogen, phosphorus, N, P), in order to meet its practical application, it is necessary to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/168C01B32/198C01B32/15B82Y30/00
CPCC01B32/168C01B32/198C01B32/15B82Y30/00C01B2202/06
Inventor 黄昊齐民董旭峰朱盛铭
Owner DALIAN UNIV OF TECH
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