Preparation method of nitrogen-doped ordered mesoporous carbon material

A technology of doping mesoporous carbon and nitrogen, which is applied in the field of preparation of ordered mesoporous carbon materials, can solve the problems of poor fusion between precursor and template, complex and lengthy precursor process, poor repeatability of material preparation, etc., and achieve simple and easy polymerization process The effect of control safety, good product uniformity and regular structure

Active Publication Date: 2014-12-10
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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Problems solved by technology

However, there are still many deficiencies in the above-mentioned existing technologies, mainly in: 1), the process of synthesizing the precursor is complicated and lengthy, the polymerization reaction is difficult to control, and the repeatability of material preparation is poor; 2), the fusion of the precursor and the template is poor ; 3), the reaction yield is low; etc.

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

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preparation example Construction

[0023] A method for preparing a nitrogen-doped ordered mesoporous carbon material, comprising the steps of:

[0024] Step 1. At room temperature, in a sealed tube reactor or autoclave, dissolve the polyamino compound and the silica gel template in an organic solvent at a mass ratio of 1:0.8 to 1.5, and mix evenly to obtain solution 1, wherein the polyamino compound It is one of benzidine, 4,4'-diaminodiphenylmethane, ethylenediamine or other compounds with two or more primary amino groups; the mass ratio of polyamino compound to organic solvent is 1:5~ 10. Silica gel templates are SBA-15, SBA-3 or MCM-48, etc. Dissolve 2,4,6-trichloro-1,3,5-triazine in an organic solvent in a container, mix well to obtain solution 2, in which 2,4,6-trichloro-1,3,5 - The mass ratio of the triazine to the organic solvent is 1:5-10. The organic solvent in solution 1 and solution 2 is one of N,N-dimethylformamide, dimethylsulfoxide or N,N-dimethylacetamide, preferably N,N-dimethylformamide.

[...

Embodiment 1

[0031] A method for preparing a nitrogen-doped ordered mesoporous carbon material, comprising the following steps:

[0032] (1) At room temperature, dissolve 0.552g benzidine and 0.5g templating agent SBA-15 in 5mL of N,N-dimethylformamide in a sealed tube reactor, and stir to obtain solution 1; at the same time, in the test tube 0.369 g of 2,4,6-trichloro-1,3,5-triazine was dissolved in 2 mL of N,N-dimethylformamide to obtain a clear solution 2;

[0033] (2) Slowly add solution 2 in step (1) to solution 1, stir and mix, add 1mL of N,N-diisopropylethylamine, seal the tube reactor, heat to 130°C and stir for 12h to fully polymerize , stop stirring to obtain oily liquid;

[0034] (3) Pour the oily liquid obtained in step (2) into 200 mL of distilled water to produce a yellow solid, filter it in a Buchner funnel in time and keep the filter cake, wash it with distilled water for 3 times, and dry it in an oven at 80°C for 12 hours to obtain the precursor body, yellow granular solid...

Embodiment 2

[0039] A method for preparing a nitrogen-doped ordered mesoporous carbon material, comprising the following steps:

[0040] (1) At room temperature, dissolve 0.552g benzidine and 0.5g templating agent SBA-15 in 5mL of N,N-dimethylformamide in a sealed tube reactor, and stir to obtain solution 1; at the same time, in the test tube 0.369 g of 2,4,6-trichloro-1,3,5-triazine was dissolved in 2 mL of N,N-dimethylformamide to obtain a clear solution 2;

[0041] (2) Slowly add solution 2 in step (1) to solution 1, stir and mix, add 1mL of N,N-diisopropylethylamine, seal the tube reactor, heat to 130°C and stir for 12h to fully polymerize , stop stirring to obtain oily liquid;

[0042] (3) Pour the oily liquid obtained in step (2) into 200 mL of distilled water to produce a yellow solid, filter it in a Buchner funnel in time and keep the filter cake, wash 3 times with distilled water, and dry in an oven at 80°C for 12 hours to obtain a yellow solid granular solids;

[0043] (4) Gri...

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Abstract

The invention discloses a preparation method of a nitrogen-doped ordered mesoporous carbon material. The preparation method comprises the following steps: performing polymerization reaction on 2,4,6-trichloro-1,3,5-triazine and a polyamine compound in an organic solvent, adding an acid-binding agent to neutralize acid generated during polymerization reaction, so as to promote the polymerization reaction; filtering and drying to obtain a carbon-nitrogen material precursor, and performing high-temperature carbonization under inert atmosphere; cooling to room temperature, removing a template agent by utilizing hydrofluoric acid, to obtain the nitrogen-doped ordered mesoporous carbon material. The polymerization process of the precursor is simple and easily controlled and safe, the nitrogen-doped ordered mesoporous carbon material is good in the integration with a template, the porous structure is controllable, the cost is low, and the equipment is simple and convenient in requirement. The method is high in repeatability, and high in reaction yield; the product is good in uniformity, high in nitrogen content, and regular in structure; the whole process is simple and convenient. The prepared nitrogen-doped ordered mesoporous carbon material has porous ducts with ordered heights, large in specific surface area, the apertures are uniformly distributed, and the nitrogen-doped ordered mesoporous carbon material is high in stability, and has wide application prospects in the field of catalytic and electrode materials, and the like.

Description

technical field [0001] The invention relates to the technical field of preparation of ordered mesoporous carbon materials, in particular to a preparation method of nitrogen-doped ordered mesoporous carbon materials. Background technique [0002] In recent years, there have been more and more reports on carbon-nitrogen materials, not only because the main elements of carbon-nitrogen materials are carbon and nitrogen and a small amount of hydrogen, they are environmentally friendly and meet the requirements of green chemistry; and their thermal stability is good. exhibited excellent catalytic performance. Due to its regular channels, large specific surface area, uniform pore size and high stability, ordered mesoporous carbon materials have important application value in many high-tech fields, such as fuel cells, catalyst supports, sensors, and membrane separation. Among them, nitrogen-doped mesoporous carbon materials mainly refer to a new type of mesoporous carbon materials ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
Inventor 姚小泉田靖吕伟王玲玲孙有文朱荔
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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