In-situ nitrogen-doped ultra large aperture mesoporous carbon material and preparation method thereof

A nitrogen-doped, mesoporous carbon technology, applied in the field of materials, can solve problems such as restricting application promotion and restricting applications, and achieves the effects of broad application prospects, elimination of possibilities, and easy availability of raw materials

Active Publication Date: 2017-05-31
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Chinese Patent Publication No. CN101153051A published on April 2, 2008 an invention titled "an ordered mesoporous material with super large pore size and its preparation method", which utilizes amphiphilic PEO- The b-PS triblock copolymer is used as a structure-directing agent, and the phenolic resin is used as a carbon precursor to induce self-assembly through solvent volatilization to prepare mesoporous carbon materials with a pore size between 10-100nm. The disadvantage is that PEO-b- PS tri-block copolymers need to be synthesized through multi-step organic reactions in the laboratory, which greatly limits the application and promotion of this method, and the hydrophilicity of the prepared carbon materials needs to be improved through post-processing
(TakahitoMitome, Porous structure and pore size control of

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0020] Example 1

[0021] A method for preparing an in-situ nitrogen-doped mesoporous carbon material with a large aperture includes the following steps:

[0022] (1) Disperse 1g of chitosan powder (biochemical reagent, deacetylation degree between 80-95%, viscosity between 50-800mPa.s) in 29ml deionized water, then add 2ml 2MHCL solution and stir for 15min Get chitosan acidic solution A; Dissolve 1g of F127 in 4ml of ethanol, add 1ml of 0.2MHCL, stir for 5min, drop 3.7ml of ethyl orthosilicate, and react for 10min to obtain solution B; add A dropwise to B In, stirring at 40°C for 2 hours to obtain a mixture (all stirring power in this step is between 100-350W, and stirring speed is 200rpm);

[0023] (2) Move the obtained mixture into a petri dish, age at 25°C for 48h to obtain a mature gel, then put it into an oven to cure at 80°C for 12h, then place it in a tube furnace in an inert atmosphere (N 2 ) Under protection, heat up to 900°C at a rate of 2°C / min and keep it for 2 hours to...

Example Embodiment

[0025] Example 2

[0026] A method for preparing an in-situ nitrogen-doped mesoporous carbon material with a large aperture includes the following steps:

[0027] (1) Disperse 1g of chitosan powder (biochemical reagent, deacetylation degree between 80-95%, viscosity between 50-800mPa.s) in 29ml deionized water, then add 2ml 2M HCL solution and stir for 15min Then obtain chitosan acidic solution A; Dissolve 1.5g F127 in 6ml ethanol, add 1ml 0.2M HCL, stir for 5min, drop 3.7ml ethyl orthosilicate, and react for 10min to obtain B solution; Add dropwise to B and stir at 40°C for 3 hours to obtain a mixture (all the stirring power in this step is between 100-350W, and the stirring speed is 250rpm);

[0028] (2) Transfer the resulting mixture into a petri dish, age at 25°C for 48h to obtain a mature gel, then put it in an oven at 100°C for 8h curing, then place it in a tube furnace in an inert atmosphere (N 2 ) Under protection, the temperature is raised to 900°C at a rate of 3°C / min and ...

Example Embodiment

[0030] Example 3

[0031] A method for preparing an in-situ nitrogen-doped mesoporous carbon material with a large aperture includes the following steps:

[0032] (1) Disperse 1g of chitosan powder (biochemical reagent, deacetylation degree between 80-95%, viscosity between 50-800mPa.s) in 29ml deionized water, then add 2ml 2M HCL solution and stir for 15min Then get chitosan acidic solution A; Dissolve 0.75g F127 in 3ml ethanol, add 1ml 0.2MHCL, stir for 5min, add 3.7ml ethyl orthosilicate dropwise, react for 10min to get B solution; drop A dropwise Add B and stir for 1.5h at 40°C to obtain a mixture (all the stirring power in this step is between 100-350W, and the stirring speed is 100rpm);

[0033] (2) Transfer the resulting mixture into a petri dish, age at 15°C for 72h to obtain a mature gel, then put it in an oven at 80°C for 12h, then place it in a tube furnace in an inert atmosphere (N 2 ) Under protection, the temperature is raised to 900°C at a rate of 3°C / min and kept for...

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Abstract

The invention discloses an in-situ nitrogen-doped ultra large aperture mesoporous carbon material and a preparation method thereof. The aperture is concentrated between 17.4 and 26.8nm, the BET specific surface area is 428-984 m<2>/g, the pore volume is 0.72-2.38 cm<3>/g, the nitrogen element content is 4.17-4.63wt%, and the doping form of nitrogen atoms is pyridine nitrogen, pyrrole nitrogen or quaternary ammonium nitrogen. According to the preparation method, nitrogen-containing biopolymer chitosan is used as a carbon source, tetraethoxysilane (TEOS) is used as a silicon source, commercial surfactant F127 is used as a structure-directing agent, deionized water is used as a main solvent, the chitosan is combined with the hydrolyzed tetraethoxysilane into a high-polymerization hybrid material by using a sol-gel method, the hybrid material is assembled with the structure-directing agent F127 into a mesoporous structure via hydrogen bonding, and the mesoporous carbon material is obtained after template removal. The method is simple, the raw materials are readily available, and the aperture size can be adjusted.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to an in-situ nitrogen-doped ultra-large-aperture mesoporous carbon material, and also relates to a preparation method of the in-situ nitrogen-doped ultra-large-aperture mesoporous carbon material. Background technique [0002] Ultra-large pore diameter mesoporous (10-50nm) carbon materials are a hot spot in the scientific research of nanomaterials in recent years. They have extensive applications in biosensors, adsorption and separation of macromolecules, especially protein molecules, and targeted delivery of macromolecular drug carriers Application prospect. Due to the high requirements for the biocompatibility of carbon materials in these application fields, the required ultra-large pore mesoporous carbon materials should not only have large pore diameter, pore volume and specific surface area, but also be non-toxic, harmless, high Biocompatible materials should ha...

Claims

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Application Information

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IPC IPC(8): C01B32/05A61K47/04
CPCA61K47/02C01P2006/12C01P2006/16
Inventor 林倩潘红艳杨春亮曹建新王贤书
Owner GUIZHOU UNIV
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