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A preparation method of monodisperse cobalt nitrogen co-doped hollow carbon nanoparticles

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: 2019-07-23
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-definedcarbonpolyhedronspreparedfromnanometal-organicframeworksforoxygenreduction.J.Mater.Chem.A,2(2014)11606-11613", RuqiangZou et al. reported cobalt-nitrogen co-doped porous carbon nanoparticles with controllable particle size. The specific surface area (100-400m2g-1) of the obtained carbon material is relatively small

Method used

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  • A preparation method of monodisperse cobalt nitrogen co-doped hollow carbon nanoparticles
  • A preparation method of monodisperse cobalt nitrogen co-doped hollow carbon nanoparticles
  • A preparation method of monodisperse cobalt nitrogen co-doped hollow carbon nanoparticles

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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 filled with DMF and water mixed solvent (64 mL, volume ratio 3:1), and ultrasonically 20 min at room temperature to make it fully diffused. Then add 0.660g of 2-methylimidazole, after ultrasonication for 5 minutes, transfer it to a hot water kettle, place it in a 50°C oven for 5 hours, 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...

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 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 60°C oven for 4h, after the reaction, centrifuge, wash and dry to obtain 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 diffused. Then add 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, and the te...

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Abstract

The invention relates to a preparation method of monodisperse cobalt-nitrogen co-doped hollow carbon nanoparticles, using ZnO nanosphere template and Zn source, adding cobalt ions to form a double metal hybrid zeolite-like imidazolate skeleton compound shell, that is, ZnO@ Zn / Co‑ZIF precursor; followed by high temperature carbonization of ZnO@Zn / Co‑ZIF precursor to directly obtain a specific surface area of ​​400‑600m 2 g ‑1 cobalt-nitrogen co-doped hollow carbon nanoparticles. The synthesis method of the invention is simple, does not need to use pickling to remove the core layer template, and can realize an environment-friendly preparation process.

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 Patents(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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