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Free radical induced graphite type nitrogen-doped graphene catalytic material and preparation method thereof

A catalytic material, graphite-type nitrogen technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problem of difficulty in adjusting the doping ratio of various forms of N, and achieve good electrocatalytic activity , expand the practical application prospects, and prepare the effect of cheap and easy-to-obtain raw materials

Pending Publication Date: 2022-07-05
HUAQIAO UNIVERSITY
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  • Description
  • Claims
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Problems solved by technology

However, in the case of traditional doping, various forms of N doping coexist in the graphene network, and the doping ratio of various forms of N is difficult to control.

Method used

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  • Free radical induced graphite type nitrogen-doped graphene catalytic material and preparation method thereof
  • Free radical induced graphite type nitrogen-doped graphene catalytic material and preparation method thereof
  • Free radical induced graphite type nitrogen-doped graphene catalytic material and preparation method thereof

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preparation example Construction

[0037] A preparation method of a free radical-induced graphite-type nitrogen-doped graphene catalytic material, which specifically comprises the following steps:

[0038] (1) Weigh each raw material according to the proportion of raw material components: graphite powder 40~60wt%, sodium nitrate 0.50~0.80wt%, potassium permanganate 1.50~2.60wt%, concentrated sulfuric acid 4.00~6.00wt%, nitrite 5.00 ~10.00wt%, hydrogen peroxide 10.00~15.00wt%, the balance is water;

[0039] (2) After fully mixing and dissolving concentrated sulfuric acid, graphite powder, sodium nitrate and water in an ice bath at 0 to 5 °C, slowly adding potassium permanganate, and reacting at a constant temperature for 0.5 to 2 hours to obtain a mixed solution;

[0040] (3) placing the mixed solution obtained in step (2) in an oil bath at 90 to 100 ° C, and after constant temperature reaction for 0.5 to 1 h, hydrogen peroxide is added to remove the residual oxidant potassium permanganate;

[0041] (4) stirrin...

Embodiment 1

[0043] A free radical-induced graphite-type nitrogen-doped graphene catalytic material, the specific preparation method comprising the following steps:

[0044] (1) Weigh each raw material according to the proportion of raw material components: graphite powder 50wt%, sodium nitrate 0.65wt%, potassium permanganate 2.0wt%, concentrated sulfuric acid 5.0wt%, nitrite 8.0wt%, hydrogen peroxide 13.0wt%, The balance is water;

[0045] (2) After fully mixing and dissolving concentrated sulfuric acid, graphite powder, sodium nitrate and water in an ice bath at 0°C, slowly adding potassium permanganate and reacting at a constant temperature for 1.5 hours to obtain a mixed solution;

[0046] (3) The above mixed solution was placed in an oil bath at 100°C, and after constant temperature reaction for 0.5h, hydrogen peroxide was added to remove the oxidant residue;

[0047] (4) stirring the material obtained in step (3) at room temperature, slowly adding nitrite and hydrogen peroxide, fully ...

Embodiment 2

[0050] The electrocatalytic activity test was carried out on the free radical-induced graphite-type nitrogen-doped graphene catalytic material prepared in Example 1, and the electrocatalytic degradation of paracetamol was carried out using a constant potential galvanometer.

[0051] Add 200mL of 10mg L to a 250mL beaker -1 The prepared paracetamol solution and 0.2g NaCl were used as electrolytes; the prepared heteroatom doped graphene material was fixed on 2.5cm with conductive glue 2 on the carbon cloth, used as the anode after drying; the cathode is 2.0cm 2 copper sheet. Turn on the current meter switch and set the initial current. The electrocatalytic process was continuously stirred with a magnetic stirrer, and 1 mL of water samples were collected at specified time intervals, placed in a 2 mL centrifuge tube, and 1 mL of methanol was added to quench free radicals. Use 0.22μm organic filter membrane to filter the water sample, then use 2998PDA (246nm) high performance li...

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Abstract

The invention discloses a free radical induced graphite type nitrogen-doped graphene catalytic material and a preparation method thereof, and the nitrogen-doped graphene catalytic material is prepared from the following raw material components in percentage by mass through a hydrothermal synthesis method: 40 to 60 weight percent of graphite powder, 0.50 to 0.80 weight percent of sodium nitrate, 1.50 to 2.60 weight percent of potassium permanganate, 4.00 to 6.00 weight percent of concentrated sulfuric acid, 5.00 to 10.00 weight percent of nitrite, 10.00 to 15.00 weight percent of hydrogen peroxide and the balance of water, wherein the graphite-type nitrogen is doped in the total nitrogen-doped structure by more than 75%. According to the preparation method, the loading capacity and the loading form of nitrogen atoms are regulated and controlled under proper reaction conditions, and the high-conductivity graphite type nitrogen doping proportion is increased, so that the hybridized graphene material has more excellent conductivity and catalytic activity; the practical application prospect of the material in the catalysis industry can be expanded, the research on the catalysis theory of the hybrid graphene material can be deepened, and the development of the material has important significance in the aspects of scientific research and practical application.

Description

technical field [0001] The invention belongs to the technical field of graphene catalysts, and in particular relates to a free radical-induced graphite-type nitrogen-doped graphene catalyst material and a preparation method thereof. Background technique [0002] Since the successful preparation of graphene materials in 2004, graphene materials have become a research hotspot in the fields of physics, chemistry, biomedicine and materials science due to their non-toxicity, easy availability, and strong chemical stability. Among them, graphene oxide has sufficient oxygen functional groups, small particle size, and a large number of exposed edge sites, which provide a good substrate for surface modification. However, the practical application of graphene is still limited by the following material defects: (i) the zero-bandgap electronic structure of graphene material greatly limits its application in the field of electrochemistry; (ii) graphene has The higher surface energy make...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/00C02F1/461C02F101/30C02F101/34C02F101/38
CPCB01J27/24C02F1/46109C02F2001/46142C02F2101/308C02F2101/34C02F2101/38B01J35/33
Inventor 张倩洪俊明周玉莲于永波王冰鑫
Owner HUAQIAO UNIVERSITY
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