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Preparation method of nitrogen-doped carbon material

A nitrogen-doped carbon and nitrogen technology, applied in the preparation/purification of carbon, can solve the problems of affecting performance and low nitrogen doping amount, and achieve mild reaction conditions, easily controllable nitrogen doping amount, and high nitrogen content. Effect

Inactive Publication Date: 2012-08-08
LANZHOU UNIVERSITY OF TECHNOLOGY
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Problems solved by technology

Nitrogen-containing carbohydrates such as pyridine, imidazole, ethylenediamine, and phthalocyanine have been used as precursors to prepare nitrogen-doped carbon materials by high-temperature pyrolysis, but due to the restriction of the nitrogen content in the precursors, the prepared nitrogen-doped carbon materials nitrogen The amount of doping is not high, which affects its final performance

Method used

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  • Preparation method of nitrogen-doped carbon material
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  • Preparation method of nitrogen-doped carbon material

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preparation example Construction

[0016] The invention is a method for preparing a nitrogen-doped carbon material, the steps of which are:

[0017] (1) Take 2-5g of sucrose, add 40-80mL of ammonia water with a concentration higher than 12% to dissolve, and place it in a hydrothermal reaction kettle with a polytetrafluoroethylene lining;

[0018] (2) heating the reaction kettle in the above (1) at a temperature of 160-200° C. for 8-24 hours, filtering after cooling, and drying in vacuum to obtain the precursor;

[0019] (3) heating the precursor in (2) above to 600-900°C at a rate of 5-10°C / min, and keeping it warm for 1-4 hours;

[0020] (4) Naturally cool the product in (3) above to room temperature, and grind to obtain a nitrogen-doped carbon material;

[0021] (5) The processes described in (3) and (4) above are carried out under the protection of an inert atmosphere, and the gas flow rate is 50-100 mL / min.

[0022] The inert atmosphere mentioned above is nitrogen.

[0023] The nitrogen content of the ni...

Embodiment 2

[0027] Take 4g of sucrose, dissolve it in 60mL of 30% ammonia water, place the solution in a polytetrafluoroethylene-lined hydrothermal reaction kettle, react at 200°C for 16 hours, filter and wash to obtain a precursor with a nitrogen content of 19.6% . The precursor was heated to 800°C at a rate of 10°C / min in a nitrogen flow of 100mL / min, kept for 1 hour, cooled to room temperature under the protection of a nitrogen atmosphere, and ground to obtain a nitrogen-doped carbon material with a nitrogen content of 12.7%.

Embodiment 3

[0029] Take 3g of sucrose, dissolve it in 60mL of 24% ammonia water, put the solution in a hydrothermal reaction kettle with polytetrafluoroethylene lining, react at 200°C for 8 hours, filter and wash to obtain the precursor with a nitrogen content of 17.0% . The precursor was heated to 700°C at a rate of 5°C / min in a nitrogen flow of 60mL / min, held for 3 hours, cooled to room temperature under the protection of a nitrogen atmosphere, and ground to obtain a nitrogen-doped carbon material with a nitrogen content of 14.2%.

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Abstract

Disclosed is a preparation method of a nitrogen-doped carbon material. The nitrogen-doped carbon material prepared in the invention has latent applications in the aspects of hydrogen storage, fuel cells, biosensors, supercapacitors and the like. According to the method, cane sugar is used as a carbon source, ammoniacal liquor is used as a nitrogen source, and the nitrogen-doped carbon material isprepared by simple steps of hydro-thermal carbonization, calcination in inert atmosphere and the like, wherein the hydro-thermal temperature is 160-200 DEG C, the concentration of the ammoniacal liquor is higher than 12%, and the carbonization temperature is 600-900 DEG C. Nitrogen doping amount can be controlled within the range of 17.8%-3.6% by adjusting hydro-thermal carbonization condition and calcination temperature. The prepared nitrogen-doped carbon material has a lamella shape with the lamellar thickness being about 200nm. Nitrogen atoms are mixed in graphitic carbon molecular networkmainly in graphite-like and pyridine-like structures.

Description

technical field [0001] The invention relates to a preparation method of nitrogen-doped carbon material. Background technique [0002] High-temperature pyrolysis of nitrogen-containing precursors is one of the most convenient methods to obtain nitrogen-doped carbon materials. At the same time, studies have shown that the amount of nitrogen doping has a direct relationship with the properties of nitrogen-doped carbon materials. Nitrogen-containing carbohydrates such as pyridine, imidazole, ethylenediamine, and phthalocyanine have been used as precursors to prepare nitrogen-doped carbon materials by high-temperature pyrolysis, but due to the restriction of the nitrogen content in the precursors, the prepared nitrogen-doped carbon materials nitrogen The doping amount is not high, thus affecting its final performance. Contents of the invention [0003] The purpose of the present invention is to provide a method for preparing nitrogen-doped carbon material. [0004] The inven...

Claims

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Application Information

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IPC IPC(8): C01B31/02C01B32/05
Inventor 张德懿马颖冯辉霞郝远
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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