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Preparation method of nitrogenous porous carbon

A technology of porous carbon and pre-oxidation, applied in the field of porous materials, can solve the problems of poor economy, low surface area, complicated operation, etc., and achieve the effects of low production cost, abundant sources and simple process.

Inactive Publication Date: 2014-03-12
NANJING INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Melamine and dicyandiamide are preparation C 3 N 4 An ideal precursor, the raw materials are easily available, safe and non-toxic, and economical, and can be prepared on a large scale 3 N 4 ; It has been reported in the literature that melamine was used as a raw material to prepare graphite-like g-C in a semi-closed crucible. 3 N 4 , photodegradable organic dyes have good performance after loading Ag (Langmuir 2009, 25, 10397.), but this g-C 3 N 4 No porosity, very low surface area, limited performance
From the literature, the preparation of porous C 3 N 4 Both use hard template method (such as SBA-15, spherical nano-SiO 2 etc.), the types of nitrogen-containing compound precursors used are more, due to the use of templates to form pores and adjust the pore size, the resulting porous C 3 N 4 Also need strong alkali or hydrofluoric acid to remove the template agent, this method is cumbersome to operate, the cycle is long, and the economy is poor

Method used

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  • Preparation method of nitrogenous porous carbon
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  • Preparation method of nitrogenous porous carbon

Examples

Experimental program
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Embodiment 1

[0023] Mix 5g of mesoporous carbon with 1 times the volume of hydrogen peroxide solution with a concentration of 0.1M, let stand for 24h, filter, wash and dry to obtain pre-oxidized mesoporous carbon; weigh 50g of melamine and 5g of pre-oxidized mesoporous carbon, and mix the two Place them at both ends of the reaction container, and separate them with a spacer in the middle; cover and seal the container, place it in a heating furnace, heat it to 350°C in a nitrogen atmosphere, keep it warm for 4 hours, then raise the temperature to 525°C, keep it warm for 4 hours, and naturally After cooling, nitrogen-containing porous carbon is obtained, with a surface area of ​​1150m 2 / g, total pore volume 1.50cm 3 / g, the average pore diameter is 4.1nm, the mesoporosity is 100%, and the nitrogen content is 17at% (atomic %).

Embodiment 2

[0025] Mix 5g ordered mesoporous carbon (CMK-3) with 10 times the volume of 5M nitric acid solution, let it stand for 1h, filter, wash and dry to obtain preoxidized CMK-3; weigh 5g melamine, 5g preoxidized CMK-3, place the two at both ends of the reaction vessel, and separate them with a ceramic spacer in the middle; cover and seal the vessel, place it in a heating furnace, heat it to 500°C in a nitrogen atmosphere, keep it warm for 0.1h, and then raise the temperature To 725 ℃, keep warm for 0.1h, after natural cooling, nitrogen-containing porous carbon is obtained, and its surface area is 1100m 2 / g, total pore volume 1.10cm 3 / g, the average pore diameter is 3.8nm, the mesoporosity is 99%, and the nitrogen content is 10at% (atomic %).

Embodiment 3

[0027] Mix 10g of bamboo activated carbon with 5 times the volume of potassium permanganate solution with a concentration of 2M, filter, wash and dry to obtain pre-oxidized bamboo activated carbon after standing for 2 hours; weigh 1g of melamine, 10g of pre-oxidized bamboo activated carbon, Put melamine and porous carbon at both ends of the reaction vessel, and separate them with a ceramic spacer in the middle; cover and seal the vessel, place it in a heating furnace, heat it to 400°C in a carbon dioxide atmosphere, keep it warm for 4 hours, and then raise the temperature to 600°C , heat preservation for 2h, after natural cooling, nitrogen-containing porous carbon is obtained, and its surface area is 610m 2 / g, total pore volume 0.403cm 3 / g, the average pore diameter is 1.1nm, the microporosity is 78%, and the nitrogen content is 7at% (atomic %).

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Abstract

The invention relates to a preparation method of nitrogenous porous carbon, which comprises the following steps: preoxidizing porous carbon with an oxidizer; and in a closed environment, depositing a nitrogenous substance in the preoxidized porous carbon pore canals by a chemical vapor deposition process by using melamine / dicyandiamide as a nitrogenous precursor, thereby obtaining the nitrogenous porous carbon. The method overcomes the defects of low nitrogen content in the product, high time consumption and the like in the existing nitrogenous porous carbon preparation method, obviously enhances the nitrogen content in the nitrogenous porous carbon (the maximum nitrogen content is up to 17%at), has the advantages of simple technique, abundant raw material sources and low production cost, and can easily implement industrialization; and the obtained nitrogenous porous carbon product has excellent properties, and has favorable application prospects in the fields of adsorptive separation, catalysis, electrode materials and the like.

Description

technical field [0001] The present invention relates to a preparation method of nitrogen-containing porous carbon, and more particularly relates to a kind of pre-oxidized porous carbon as a matrix, melamine / dicyandiamide as raw material, using chemical vapor deposition reaction, nitrogen-containing species in a closed environment The nitrogen-containing porous carbon material is prepared by depositing on the inner wall of the porous carbon channel, and belongs to the field of porous materials. Background technique [0002] Porous materials such as porous carbon, with high surface area and developed pores, are widely used as adsorbents, catalyst supports, battery and supercapacitor electrode materials, etc., but conventional porous carbon materials are difficult to meet the increasing performance needs, such as activated carbon, although compared with The surface area is high, but its pore size is small (<2nm), which is not conducive to the penetration and free entry and e...

Claims

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Application Information

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IPC IPC(8): C01B31/02B01J20/20B01J20/30B01D53/02B01J27/24H01G11/38C01B32/05C01B32/354
Inventor 黄玉安王翼飞赖文秋怀旭张可强谭学锋
Owner NANJING INST OF TECH
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