Preparation method of nitrogen doped hollow mesoporous carbon sphere

A technology of empty mesopores and nitrogen doping, applied in the field of materials, can solve the problems of low nitrogen doping, high cost of preparation process, cumbersome loading process, etc., achieve uniform pore size distribution, simple preparation process, and high nitrogen doping Effect

Inactive Publication Date: 2016-08-03
NANJING UNIV OF SCI & TECH
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Problems solved by technology

[0004] At present, nitrogen-doped hollow carbon materials have been prepared by different methods: Ferrero et al [G.A.Ferrero, A.B.Fuertes and M.Sevilla. Nitrogen-doped hollow mesoporous carbon spheres were synthesized with solid silica spheres as hard templates and pyrrole monomers as nitrogen-containing carbon precursors. The nitrogen doping of this material is relatively uniform, but the loading process is relatively cumbersome. Not adjustable
[JinH, ZhangHM, ZhongHX, et al., Nitrogen-dopedcarbonxerogel: Anovelcarbon-basedelectrocatalystforoxygenreductionreactioninprotonexchangemembrane (PEM) fuelcells, EnergyEnviron.Sci., 2011, 4(9):3389~3394] etc. used sol-gel polymerization method, Catechol and formaldehyde are used as carbon sources, cobalt nitrate is used as a nitrogen-doped catalyst, ammonia is used as an effective nitrogen source to form a nitrogen-rich atmosphere, and pyridinic nitrogen and graphite nitrogen (quaternary nitrogen) are introduced by in-situ doping In the carbon xerogel, the carbon material prepared by this method changes the electronic structure of the original carbon atom and increases the power supply capacity of the adjacent carbon atom, but the preparation process is expensive and the amount of nitrogen doping is relatively low
[0005] Although some progress has been made in the research of nitrogen-doped hollow mesoporous carbon materials, the existing methods generally need to use more complicated means to introduce nitrogen sources into the carbon sphere matrix or need to add catalysts, etc., and cannot realize the regulation of the size of carbon materials.

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  • Preparation method of nitrogen doped hollow mesoporous carbon sphere
  • Preparation method of nitrogen doped hollow mesoporous carbon sphere
  • Preparation method of nitrogen doped hollow mesoporous carbon sphere

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Experimental program
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Embodiment 1

[0021] Step 1: Accurately measure 100mL deionized water, 40mL ethanol and 0.2mL ammonia water with a mass fraction of 25%, and at the same time accurately weigh 2gCTAC in a beaker, magnetically stir until CTAC is completely dissolved, and then accurately weigh 0.55g isophthalic acid Add the phenol into the beaker, and then stir until it is completely dissolved. Measure 0.74mL of formaldehyde solution with a mass fraction of 37% and 3mLTEOS into the beaker at the same time, continue stirring for 30min, then add 0.3g of melamine in an oil bath at 70°C, and stir until All dissolved, accurately measure 0.55mL formaldehyde solution with a mass fraction of 37%, add it to the beaker, seal it and stir for 24h.

[0022] The second step: after the reaction, the solution is centrifuged with ethanol, separated and washed three times, and then dried in an oven at 100°C. The dried solid powder is heated to 800°C at a heating rate of 3°C / min and calcined in a nitrogen furnace for 3 hours. Co...

Embodiment 2

[0025] Step 1: Accurately measure 100mL deionized water, 40mL ethanol and 0.5mL ammonia water with a mass fraction of 25%, and at the same time accurately weigh 2gCTAC in a beaker, stir magnetically until CTAC is completely dissolved, and then accurately weigh 0.55g isophthalic acid Add the phenol into the beaker, and then stir until it is completely dissolved. Measure 0.74mL of formaldehyde solution with a mass fraction of 37% and 3mLTEOS into the beaker at the same time, continue stirring for 30min, then add 0.3g of melamine in an oil bath at 70°C, and stir until All dissolved, accurately measure 0.55mL formaldehyde solution with a mass fraction of 37%, add it to the beaker, seal it and stir for 24h.

[0026] The second step: after the reaction, the solution is centrifuged with ethanol, separated and washed three times, and then dried in an oven at 100°C. The dried solid powder is heated to 800°C at a heating rate of 3°C / min and calcined in a nitrogen furnace for 3 hours. Co...

Embodiment 3

[0029] Step 1: Accurately measure 100mL deionized water, 40mL ethanol and 0.5mL ammonia water with a mass fraction of 25%, and at the same time accurately weigh 2gCTAC in a beaker, stir magnetically until CTAC is completely dissolved, and then accurately weigh 0.55g isophthalic acid Add the phenol into the beaker, and then stir until it is completely dissolved. Measure 0.74mL of formaldehyde solution with a mass fraction of 37% and 3mLTEOS into the beaker at the same time, continue stirring for 30min, then add 0.3g of melamine in an oil bath at 70°C, and stir until All dissolved, accurately measure 0.55mL formaldehyde solution with a mass fraction of 37%, add it to the beaker, seal it and stir for 24h.

[0030] The second step: after the reaction, the solution is centrifuged with ethanol, separated and washed three times, and then dried in an oven at 100°C. The dried solid powder is heated to 800°C at a heating rate of 3°C / min and calcined in a nitrogen furnace for 3 hours. Co...

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Abstract

The invention discloses a method for preparing nitrogen-doped hollow mesoporous carbon spheres. Resorcinol-formaldehyde resin is used as a carbon precursor, melamine is used as a nitrogen source, and cetyltrimethylammonium chloride is used as a templating agent. Silicate oligomers are used as structural support, ammonia water is used as catalyst, and the size and shape of hollow carbon nanospheres can be effectively controlled by changing the amount of ammonia water. The obtained hollow mesoporous carbon spheres have the characteristics of hollow structure, high porosity and specific surface area, large pore volume, uniform mesoporous size and nitrogen doping.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a preparation method of nitrogen-doped hollow mesoporous carbon spheres. Background technique [0002] Nitrogen-doped hollow carbon spheres are widely used in the fields of environment, energy, catalysis, and biomedicine due to their strong surface polarity, high electrical conductivity, many basic sites on the surface, short diffusion paths, low density, and good surface permeability. Broad application prospects. [0003] In recent years, the preparation, structure and properties of nitrogen-doped hollow mesoporous carbon spheres have attracted much attention from research institutions at home and abroad. At present, there are two main methods for preparing nitrogen-doped hollow carbon spheres: (1) post-treatment method: the target functional group is introduced into the pre-synthesized carbon material by an appropriate chemical method, such as impregnating a surf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01P2004/03C01P2004/04C01P2004/34C01P2004/62
Inventor 李健生胡兴茹刘超王晶罗瑞李骋王连军孙秀云沈锦优韩卫清刘晓东
Owner NANJING UNIV OF SCI & TECH
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