Preparation method of cobalt-nitrogen co-doped carbon nanocage

A carbon nanocage and co-doping technology, which is applied in the direction of nano-carbon, medical preparations of non-active ingredients, pharmaceutical formulas, etc., can solve problems such as unstable performance, variable size, and unclear polyhedral structure, and achieve uniform particle size. Good reproducibility and good shape results

Active Publication Date: 2021-04-20
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006]However, the existing methods for preparing cobalt-nitrogen co-doped carbon nanocages are usually obtained by pyrolysis and nitriding of ZIF-8@ZIF-67, There is no specific research on the ZIF-8@ZIF-67 precursor synthesis method involved in the synthesis process and the subsequent high-temperature process, so that the final polyhedron has shortcomings such as unclear structure, variable size, and unstable performance.
Therefore, there are certain shortcomings and many challenges in the synthesis of Co / NCNC at present.

Method used

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  • Preparation method of cobalt-nitrogen co-doped carbon nanocage
  • Preparation method of cobalt-nitrogen co-doped carbon nanocage
  • Preparation method of cobalt-nitrogen co-doped carbon nanocage

Examples

Experimental program
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Embodiment 1

[0032] 2.38g (0.008mol) Zn(NO 3 ) 2 ·6H 2 O and 2.627g (0.032mol) 2-methylimidazole were respectively dispersed in 100mL of anhydrous methanol solution, Zn(NO 3 ) 2 ·6H 2 O methanol solution is placed on a magnetic stirrer and stirred at a stirring rate of 300r / min for 10min, and the methanol solution of 2-methylimidazole is poured into Zn(NO 3 ) 2 ·6H 2 O methanol solution, maintain a stirring rate of 300r / min and place it at 10°C for 30min. After the product is cross-centrifuged and washed with absolute ethanol and deionized water three times, the obtained precipitate is dispersed in anhydrous methanol with ultrasonic assistance to obtain 200mL The methanol solution of ZIF-8 was taken out, and 50 mL was taken out for use. 582mg (0.002mol) Co(NO 3 ) 2 ·6H 2 O and 656.8mg (0.008mol) 2-methylimidazole were respectively dispersed in 50mL of anhydrous methanol, and Co(NO 3 ) 2 ·6H 2 The methanol solution of O and the methanol solution of 2-methylimidazole were poured...

Embodiment 2

[0034] 2.38g (0.008mol) Zn(NO 3 ) 2 ·6H 2 O and 2.627g (0.032mol) 2-methylimidazole were respectively dispersed in 100mL of anhydrous methanol solution, Zn(NO 3 ) 2 ·6H 2 O methanol solution is placed on a magnetic stirrer and stirred at a stirring rate of 300r / min for 10min, and the methanol solution of 2-methylimidazole is poured into Zn(NO 3 ) 2 ·6H 2 O methanol solution, maintain a stirring rate of 300r / min and place it at 25°C for 30min to react for 30min. After the product is cross-centrifuged and washed with absolute ethanol and deionized water three times, the obtained precipitate is dispersed in anhydrous methanol with ultrasonic assistance to obtain 200mL The methanol solution of ZIF-8 was taken out, and 50 mL was taken out for use. 582mg (0.002mol) Co(NO 3 ) 2 ·6H 2 O and 656.8mg (0.008mol) 2-methylimidazole were respectively dispersed in 50mL of anhydrous methanol, and Co(NO 3 ) 2 ·6H 2 The methanol solution of O and the methanol solution of 2-methylim...

Embodiment 3

[0036] 2.38g (0.008mol) Zn(NO 3 ) 2 ·6H 2 O and 2.627g (0.032mol) 2-methylimidazole were respectively dispersed in 100mL of anhydrous methanol solution, Zn(NO 3 ) 2 ·6H 2 O methanol solution is placed on a magnetic stirrer and stirred at a stirring rate of 300r / min for 10min, and the methanol solution of 2-methylimidazole is poured into Zn(NO 3 ) 2 ·6H 2 O methanol solution, maintain a stirring rate of 300r / min and place it at 25°C for 1h. After the product is cross-centrifuged and washed with absolute ethanol and deionized water three times, the obtained precipitate is dispersed in anhydrous methanol with ultrasonic assistance to obtain 200mL The methanol solution of ZIF-8 was taken out, and 50 mL was taken out for use. 582mg (0.002mol) Co(NO 3 ) 2 ·6H 2 O and 656.8mg (0.008mol) 2-methylimidazole were respectively dispersed in 50mL of anhydrous methanol, and Co(NO 3 ) 2 ·6H 2 The methanol solution of O and the methanol solution of 2-methylimidazole were poured in...

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Abstract

The invention designs a preparation method of a cobalt-nitrogen co-doped carbon nanocage, which specifically comprises the following steps: by using a ZIF-8 structure as an inner core, coating a ZIF-67 shell on the outer layer of the ZIF-8 structure by a seed-mediated growth method; in the process, after Co < 2 + > and 2-methylimidazole are added, taking ZIF-8 spontaneously as an inner core to wrap ZIF-67 to obtain a ZIF-8@ZIF-67 bimetallic core-shell structure; further, in a flowing nitrogen atmosphere at 800 DEG C, carbonizing the organic ligand to form a porous N-doped material, and preliminarily obtaining a cobalt-nitrogen co-doped carbon nanocage material; and performing HCl etching to finally obtain the cobalt-nitrogen co-doped carbon nanocage material. The cobalt-nitrogen co-doped carbon nanocage nanoparticles prepared by the method are good in morphology, uniform in particle, simple in synthesis method step and high in repeatability, have higher activity through morphology and size adjustment, and have a wide application prospect in the fields of electrochemistry, catalysis, biomedicine, virus resistance and the like.

Description

Technical field: [0001] The present invention designs a method for preparing cobalt-nitrogen co-doped carbon nanocages (Co / NCNC for short), specifically using the ZIF-8 structure as the core, and wrapping the ZIF-67 shell on its outer layer by a seed-mediated growth method . During this process, when ZIF-8 is dispersed in methanol solution, its core is gradually hydrolyzed. Since ZIF-67 and ZIF-8 are MOF materials with similar structures, the addition of Co 2+ And 2-methylimidazole will spontaneously wrap ZIF-67 on the outside with ZIF-8 as the inner core, resulting in a bimetallic core-shell structure of ZIF-8@ZIF-67. Further, in a flowing nitrogen atmosphere at 800 °C, Zn 2+ 、Co 2+ The derivatized carbon is reduced to Zn and Co atoms, carbon nanotubes are gradually produced at high temperature, organic ligands are carbonized to form porous N-doped materials, and cobalt-nitrogen co-doped carbon nanocage materials are initially obtained; after HCl etching for 12-24 hours, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/15A61P35/00A61P31/14A61P31/12A61P31/10A61P31/04A61K47/69A61K33/24
Inventor 刘惠玉潘雪婷刘笑妤
Owner BEIJING UNIV OF CHEM TECH
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