Preparation method of monodisperse cobalt-nitrogen co-doped hollow carbon nano-particles

A carbon nanoparticle and co-doping technology, applied in nanocarbon and other directions, can solve the problems of small specific surface area of ​​carbon materials and achieve the effect of an environmentally friendly preparation process

Active Publication Date: 2017-04-19
JIANGSU UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the document "Well-definedcarbonpolyhedrons prepared from nano metal-organic frameworks for oxygenreduction.J.Mater.Chem.A, 2(2014) 11606–11613", Ruqiang Zou et al. reported cobalt-nitrogen co-doped porous with controllable particle size Carbon nanoparticles, its disadvantage is that the specific surface area of ​​the carbon material (100-400m 2 g -1 )Relatively small

Method used

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  • Preparation method of monodisperse cobalt-nitrogen co-doped hollow carbon nano-particles
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  • Preparation method of monodisperse cobalt-nitrogen co-doped hollow carbon nano-particles

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Experimental program
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Embodiment 1

[0037] (1) Add 40 mL of 0.1 mol / L zinc acetate aqueous solution and 200 mL of 0.1 mol / L triethanolamine aqueous solution into an Erlenmeyer flask, stir at room temperature for 30 min, and then irradiate it ultrasonically in a water bath at 30°C for 20 min After that, let it stand for 10h. After centrifugation, washing and drying, ZnO nanospheres are obtained.

[0038] (2) Add 80.0 mg of ZnO nanospheres and 20.0 mg of cobalt nitrate obtained in step 1 to an Erlenmeyer flask containing a mixed solvent of DMF and water (64 mL, volume ratio 3:1), and ultrasonically 20 min at room temperature to fully diffuse , then add 0.660g of 2-methylimidazole, after ultrasonication for 5min, transfer it to a hot water kettle, place it in a 50°C oven for 5h, after the reaction, centrifuge, wash and dry to obtain ZnO@Zn / Co-ZIF precursor.

[0039](3) The ZnO@Zn / Co-ZIF precursor obtained in step 2) was placed in a high-temperature furnace, and the temperature was raised to 800 °C at a rate of 5...

Embodiment 2

[0043] (1) Add 40 mL of 0.1 mol / L zinc acetate aqueous solution and 200 mL of 0.1 mol / L triethanolamine aqueous solution into an Erlenmeyer flask, stir at room temperature for 30 min, and then irradiate it ultrasonically in a water bath at 30°C for 20 min After that, let it stand for 10h. After centrifugation, washing and drying, ZnO nanospheres are obtained.

[0044] (2) Add 80.0 mg of ZnO nanospheres and 12.0 mg of cobalt nitrate obtained in step 1 to an Erlenmeyer flask containing a mixed solvent of DMF and water (64 mL, volume ratio 2:1), and ultrasonicate for 20 min at room temperature to fully diffuse , then add 0.660g of 2-methylimidazole, after ultrasonication for 5min, transfer it to a hot water kettle, put it in a 60°C oven for 4h, after the reaction, centrifuge, wash and dry to get ZnO@Zn / Co-ZIF precursor.

[0045] (3) The ZnO@Zn / Co-ZIF precursor obtained in step 2) was placed in a high-temperature furnace, and the temperature was raised to 900 °C at a rate of 5 ...

Embodiment 3

[0047] (1) Add 40 mL of 0.1 mol / L zinc acetate aqueous solution and 200 mL of 0.1 mol / L triethanolamine aqueous solution into an Erlenmeyer flask, stir at room temperature for 30 min, and then irradiate it ultrasonically in a water bath at 30°C for 20 min After that, let it stand for 10h. After centrifugation, washing and drying, ZnO nanospheres are obtained.

[0048] (2) Add 80.0 mg of ZnO nanospheres and 8.0 mg of cobalt nitrate obtained in step 1 to an Erlenmeyer flask filled with DMF and water mixed solvent (64 mL, volume ratio 1:1), and ultrasonically 20 min at room temperature to make it fully diffuse , followed by adding 1.32g of 2-methylimidazole, after ultrasonication for 5 minutes, pour the solution in the conical flask into a hydrothermal kettle, place it in a 70°C oven for 3 hours, after the reaction, centrifuge, wash and dry to obtain ZnO@Zn / Co-ZIF precursor.

[0049] (3) The ZnO@Zn / Co-ZIF precursor obtained in step 2) was placed in a high-temperature furnace, a...

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Abstract

The invention relates to a preparation method of monodisperse cobalt-nitrogen co-doped hollow carbon nano-particles. The method comprises the following steps: adding cobalt ions in ZnO nanosphere template and Zn source to form a double-metal hybrid zeolite imidazate skeleton compound shell, namely the ZnO@Zn / Co-ZIF precursor; and then performing high-temperature carbonization on the ZnO@Zn / Co-ZIF precursor to directly obtain the cobalt-nitrogen co-doped hollow carbon nano-particles with the specific surface area as 400-600m<2>g-1. By use of the preparation method disclosed by the invention, the synthesis method is simple, the operation of removing a nuclear layer template by use of acid-pickling is unnecessary, and the environment-friendly preparation process can be realized.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, in particular to a preparation method of monodisperse cobalt nitrogen co-doped hollow carbon nanoparticles. Background technique [0002] In recent years, porous carbon nanomaterials doped with heteroatoms (such as nitrogen, boron, phosphorus, sulfur, cobalt, etc.), especially hollow-structured carbon nanomaterials with special pore structures, have been , low density, and good physical and chemical stability, it has a wide range of applications in the fields of catalysis, adsorbents, electrode materials, and batteries. On the one hand, after heteroatoms are introduced into the carbon structure, due to the difference in bond length, valence electrons, and atomic size with carbon atoms, defects appear in sites near adjacent carbon atoms, the charge distribution is uneven, and the electrical neutrality of carbon materials is destroyed. It is more conducive to constructing the catalytic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/15
CPCC01P2002/72C01P2004/04C01P2004/30C01P2004/62C01P2006/12
Inventor 宋肖锴郭琳丽刘坚周雅静王志贤
Owner JIANGSU UNIV OF TECH
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