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Nitrogen and phosphor co-doped hollow carbon sphere material with shell layer having grading macropore-mesoporous structure as well as preparation method and application thereof

A technology of mesoporous structure and co-doping is applied in the field of preparation and application of porous materials to achieve the effects of high yield, easy large-scale industrial production and reduced energy consumption

Active Publication Date: 2017-08-11
SHANDONG UNIV OF SCI & TECH
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Problems solved by technology

However, there are no reports of nitrogen and phosphorus co-doped hollow carbon microspheres with hierarchical macroporous-mesoporous shells and their preparation methods so far.

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  • Nitrogen and phosphor co-doped hollow carbon sphere material with shell layer having grading macropore-mesoporous structure as well as preparation method and application thereof
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  • Nitrogen and phosphor co-doped hollow carbon sphere material with shell layer having grading macropore-mesoporous structure as well as preparation method and application thereof

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[0034] In view of this, in a specific embodiment of the present invention, there is provided a method for preparing hollow carbon microspheres co-doped with nitrogen and phosphorus and the shell layer has a hierarchical macropore-mesoporous structure, including:

[0035] (1) Dispersing the silica nanospheres in distilled water and ultrasonically treating them to obtain a silica template dispersion;

[0036] (2) adding the silica template dispersion liquid obtained in step (1) into the melamine resin prepolymer system, and purifying by solvothermal method under the action of a catalyst to obtain a precursor-template complex, namely composite resin microspheres;

[0037] (3) The precursor-template composite obtained in step (2) is subjected to high-temperature carbonization and template removal to obtain hollow carbon microspheres co-doped with nitrogen and phosphorus, and the shell layer has a hierarchical macropore-mesoporous structure.

[0038] In yet another specific embodim...

Embodiment 1

[0050] 1) Disperse 0.7g of silicon dioxide in 30mL of water, and sonicate to obtain a silicon dioxide template dispersion;

[0051] 2) In another system, add 30mL of water, 10mL of formaldehyde, 0.024g of hexamethylenetetramine, dissolve and add 6.3g of melamine, after a period of prepolymerization, heat up to 65°C and stir until the solution is clear; Pour silicon dioxide into the system, add 0.175 mmol of hydroxyethylidene diphosphonic acid, stir at 65°C for 4 hours, filter with suction, and dry;

[0052] 3) After carbonization at 700°C for 2 hours, and then removing silicon dioxide with HF, carbon microspheres with a nitrogen-phosphorus co-doped shell layer and a hierarchical pore structure can be obtained, with a particle size of 15±0.7 μm and a nitrogen content of 15.35% , the phosphorus content is 0.2%. Nitrogen adsorption and desorption analysis showed that the most probable pore diameter was 3.8nm. The electrochemical test results show that when the current density i...

Embodiment 2

[0054] 1) Disperse 0.7g of silicon dioxide in 30mL of water, and sonicate to obtain a silicon dioxide template dispersion;

[0055] 2) In another system, add 30mL of water, 10mL of formaldehyde, 0.024g of hexamethylenetetramine, dissolve and add 6.3g of melamine, after a period of prepolymerization, heat up to 65°C and stir until the solution is clear; Pour silicon dioxide into the system, add 0.175 mmol of hydroxyethylidene diphosphonic acid, stir at 65°C for 4 hours, filter with suction, and dry;

[0056] 3) High temperature carbonization at 800°C for 2 hours, and then removing silicon dioxide with HF, then you can get hollow carbon microspheres with nitrogen-phosphorus co-doped shell layer and hierarchical pore structure, with a particle size of 12±1 μm and a nitrogen content of 8.03% , the phosphorus content is 0.24%. The hollow structure can be observed by transmission electron microscope.

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Abstract

The invention discloses a nitrogen and phosphor co-doped hollow carbon sphere material with a shell layer having a grading macropore-mesoporous structure as well as a preparation method and application thereof. An in situ doping method is adopted, a silicon dioxide nano-ball is taken as a hard template, a melamino-formaldehyde resin is taken as a carbon precursor and a nitrogen source, an etidronic acid is taken as a catalyst and a phosphorus source and the nitrogen, and lastly, the phosphor co-doped hollow carbon sphere material with the shell layer having the grading macropore-mesoporous structure is compounded. The prepared hollow carbon sphere material has the advantages of high nitrogen and phosphor atom doping content, controllable shape, excellent electrochemical property, and the like, and meanwhile, the preparation raw material is low in cost, the cost is low, the preparation method is simple and the nitrogen and phosphor co-doped hollow carbon sphere material is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of preparation and application of porous materials. In particular, a preparation method of a hollow carbon sphere material co-doped with nitrogen and phosphorus and the shell layer has a hierarchical macropore-mesoporous structure and its application in supercapacitors. Background technique [0002] Due to the characteristics of surface chemical inertness, high mechanical stability, good electrical conductivity, large specific surface area and pore volume, porous hollow carbon sphere materials are widely used in the fields of adsorption, catalysis, hydrogen storage, electrochemical double layer capacitors and fuel cells. Show great application potential. Template synthesis of hollow carbon materials has made great progress (J.P.Han, G.Y.Xu, B.Ding, J.Pan, H.Dou, J.Mater.Chem.A, 2(2014) 5352; S.-E. Bae, K.J. Kim, I.H. Choi, S. Huh, Carbon, 99(2016) 8; Y.L. Liu, C.X.Shi, X.Y.Xu, P.C. Sun, T.H. Chen, J. Power Sources, ...

Claims

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Application Information

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IPC IPC(8): C01B32/05H01G11/24H01G11/30H01G11/32
CPCY02E60/13H01G11/30C01P2002/85C01P2004/03C01P2004/62C01P2004/80H01G11/24H01G11/32
Inventor 刘蕾张宁刘枫许世达于青
Owner SHANDONG UNIV OF SCI & TECH
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