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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

AI Technical Summary

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 mesoporous carbons using a combination of a soft-templating method and a solvent evaporation technique, Colloids and Surfaces A: Physicochem.Eng.Aspects 494(2016)180–185), although they successfully prepared ultra-large pore size Mesoporous carbon material, but the selected carbon source is still phenolic resin as announced in the above patent, so the whole reaction process is also carried out in an organic solvent, which cannot fundamentally meet the requirements of environmental friendliness in the preparation process and biomedical materials. Requirements for harmful residues, and the problem of hydrophilicity needs to be solved through post-treatment processes, which greatly limits its application in biosensors, adsorption and separation of bioactive molecules, and targeted delivery of macromolecular drug carriers.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A method for preparing an in-situ nitrogen-doped super-large-aperture mesoporous carbon material, comprising the steps of:

[0022] (1) Evenly disperse 1g chitosan powder (biochemical reagent, deacetylation degree between 80-95%, viscosity between 50-800mPa.s) in 29ml deionized water, then add 2ml2MHCL solution, stir for 15min To obtain chitosan acidic solution A; dissolve 1gF127 in 4ml ethanol, then add 1ml0.2M HCL, stir for 5min, then add 3.7ml tetraethyl orthosilicate dropwise, and react for 10min to obtain solution B; add A dropwise to B , stirred at 40°C for 2 hours to obtain the mixture (all the stirring power in this step was between 100-350W, and the stirring speed was 200rpm);

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

Embodiment 2

[0026] A method for preparing an in-situ nitrogen-doped super-large-aperture mesoporous carbon material, comprising the steps of:

[0027] (1) Evenly disperse 1g of chitosan powder (biochemical reagent, deacetylation degree between 80-95%, viscosity between 50-800mPa.s) in 29ml of deionized water, then add 2ml of 2M HCL solution, and stir for 15min Finally, chitosan acidic solution A was obtained; 1.5g F127 was dissolved in 6ml ethanol, then 1ml0.2M HCL was added, after stirring for 5min, 3.7ml tetraethyl orthosilicate was added dropwise, and solution B was obtained after 10min of reaction; Add dropwise to B, stir at 40°C for 3 hours to obtain a mixture (all stirring power in this step is between 100-350W, stirring speed is 250rpm);

[0028] (2) Transfer the obtained mixture into a petri dish, age at 25°C for 48h to obtain a mature gel, put it into an oven for curing at 100°C for 8h, and then place it in a tube furnace under an inert atmosphere (N 2 ) under protection, the temp...

Embodiment 3

[0031] A method for preparing an in-situ nitrogen-doped super-large-aperture mesoporous carbon material, comprising the steps of:

[0032] (1) Evenly disperse 1g of chitosan powder (biochemical reagent, deacetylation degree between 80-95%, viscosity between 50-800mPa.s) in 29ml of deionized water, then add 2ml of 2M HCL solution, and stir for 15min Finally, chitosan acidic solution A was obtained; 0.75g F127 was dissolved in 3ml ethanol, then 1ml0.2M HCL was added, after stirring for 5min, 3.7ml tetraethyl orthosilicate was added dropwise, and solution B was obtained after 10min of reaction; Add to B, stir at 40°C for 1.5h to obtain a mixture (all stirring power in this step is between 100-350W, stirring speed is 100rpm);

[0033] (2) Transfer the obtained mixture into a petri dish, age at 15°C for 72h to obtain a mature gel, put it into an oven at 80°C for 12h, and then place it in a tube furnace under an inert atmosphere (N 2 ) under protection, the temperature was raised t...

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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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