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Nitrogen-doped porous carbon and preparation method thereof

A technology of porous carbon and nitrogen doping, which is applied in the preparation/purification of carbon, etc., which can solve the problems of low utilization rate of nitrogen source, complex preparation process, and low nitrogen content of materials, and achieve a wide range of raw material selection, easy operation, and high efficiency The effect of using

Active Publication Date: 2013-08-28
DALIAN UNIV OF TECH
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Problems solved by technology

[0005] In the process of preparing nitrogen-doped porous carbon from heavy organic matter, there are many problems such as easy decomposition of nitrogen source, low utilization rate of nitrogen source, complicated preparation process, and low nitrogen content in the obtained material.

Method used

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  • Nitrogen-doped porous carbon and preparation method thereof
  • Nitrogen-doped porous carbon and preparation method thereof
  • Nitrogen-doped porous carbon and preparation method thereof

Examples

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Effect test

Embodiment 1

[0031] Mix melamine and formaldehyde at a molar ratio of 1:6, adjust the pH to 8 with sodium hydroxide, and bathe in water at 60°C for 30 minutes to obtain a clear solution A; The ratio of coal tar pitch to tetrahydrofuran is 1g:25mL. Dissolve coal tar pitch in tetrahydrofuran, and add magnesium citrate according to the mass ratio of coal tar pitch to magnesium citrate as 1:3, and mix well to obtain mixed solution B; The mixture B is mixed, and the reaction time is 5h at 80°C to make it fully cross-linked and blended. The residual solvent in the resulting blend is evaporated to dryness and cured at 150°C for 12h; in a carbonization furnace, under a helium atmosphere of 50mL / min , heated up to 700°C at a heating rate of 1°C / min, carbonized for 5 hours, washed with acid and water, and dried to obtain nitrogen-doped porous carbon. The main properties of the porous carbon are shown in Table 1.

Embodiment 2

[0033]Mix melamine and formaldehyde at a molar ratio of 1:1, adjust the pH to 7 with sodium hydroxide, and bathe in water at 90°C for 10 minutes to obtain a clear solution A; weigh it according to the mass ratio of coal liquefaction by-product asphaltenes to melamine at 1:5 Coal liquefaction by-product asphaltene, according to the ratio of coal liquefaction by-product asphaltene and tetrahydrofuran is 1g:15mL Dissolve coal liquefaction by-product asphaltene in tetrahydrofuran, and according to the mass of coal liquefaction by-product asphaltene and polyvinyl butyral Add polyvinyl butyral at a ratio of 1:5, mix thoroughly and evenly to obtain mixed solution B; mix solution A with mixed solution B, and react for 24 hours at 20°C to fully cross-link and blend, and blend the obtained solution The residual solvent in the product was evaporated to dryness, and solidified at 200°C for 1h; in a carbonization furnace, under a nitrogen atmosphere of 150mL / min, the temperature was raised ...

Embodiment 3

[0035] Mix urea and formaldehyde at a molar ratio of 1:3, adjust the pH to 9 with sodium hydroxide, and bathe in water at 40°C for 60 minutes to obtain a clear solution A; weigh it according to the mass ratio of coal liquefaction by-product asphaltenes to urea at 1:3 Coal liquefaction by-product asphaltene, according to the ratio of coal liquefaction by-product asphaltene and tetrahydrofuran is 1g:20mL Dissolve coal liquefaction by-product asphaltene in tetrahydrofuran, and the mass ratio of coal liquefaction by-product asphaltene to magnesium citrate is 1 : 0.5 Add magnesium citrate, mix well and get mixed solution B; mix solution A with mixed solution B, react at 90°C for 1 hour, make it fully cross-linked and blend, evaporate the residual solvent in the resulting blend to dryness , cured at 100°C for 24h; in a carbonization furnace, under a nitrogen atmosphere of 300mL / min, the temperature was raised to 1000°C at a rate of 10°C / min, carbonized for 0.5h, washed with acid and ...

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Abstract

The invention relates to a preparation method of nitrogen-doped porous carbon, and in particular relates to a method for preparing doped porous carbon by taking a heavy organism as a carbon source, belonging to the technical field of carbon material preparation. The method comprises the following steps of: firstly, conducting a reaction between a nitrogen source and formaldehyde to generate a prepolymer; then, mixing the prepolymer with a template and the carbon source, and reacting at certain temperature; and finally, curing and carbonizing a crosslinking product to obtain nitrogen-doped porous carbon. The method provided by the invention can obtain nitrogen-doped porous carbon with different pore structures and nitrogen contents through multiple ways such as control on the nitrogen source type, temperature control, control on the mass ratio of a carbon source to a nitrogen source, control on the dosage of a template agent and the like. By adopting a chemical polymerization blending carbonization method, the method effectively controls the loss of nitrogen in a thermal treatment process and improves the utilization rate of the nitrogen source; the selection range of the raw material is wide; and the method is easy to operate and easily realizes large-scale preparation while providing a new way for efficiently utilizing heavy organic matters.

Description

technical field [0001] The invention relates to a method for preparing nitrogen-doped porous carbon, in particular to a method for preparing doped porous carbon using heavy organic matter as a carbon source, and belongs to the technical field of carbon material preparation. Background technique [0002] Heavy organic matter is mainly fossil resources composed of macromolecules with a molecular weight greater than 500, including coal and its heavy derivatives (such as coal liquefaction heavy oil, coal direct liquefaction residue, coal tar and asphalt, etc.), heavy petroleum, vacuum slag Oil, catalytic cracking oil slurry, petroleum asphalt, etc. are the main organic resources in the world, especially in my country. As far as my country's energy composition is rich in coal, less oil and less gas, the efficient utilization of heavy organic matter is of great significance for the establishment of a resource-saving and environment-friendly society and even for the development of m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C01B32/05
Inventor 周颖刘哲邱介山肖南王春雷孙利赵强王道龙
Owner DALIAN UNIV OF TECH
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