Preparation method of porous graphitized hollow carbon microsphere

A technology of porous graphite and hollow carbon, applied in chemical instruments and methods, carbon compounds, inorganic chemistry, etc., can solve the problem of difficult uniform mixing of carbon precursors, poor electrical conductivity, uneven distribution of carbon material pore structure and graphitized structure, etc. problem, to achieve the effect of low cost, good conductivity, and good conductivity

Active Publication Date: 2020-04-10
TAIYUAN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the method of increasing the specific surface area of ​​carbon materials mostly uses highly corrosive activators KOH, ZnCl 2 etc. Most of the prepared carbon materials are mainly amorphous structure, and the electrical conductivity is poor.
Patent CN107265436 A discloses a kind of potassium ferrate as carbon material and graphitization catalyst, although the specific surface and graphitization degree of carbon material are improved at the same time, but potassium ferrate cannot exist stably in aqueous solution, making it react with carbon precursor Difficult to mix uniformly, resulting in uneven distribution of carbon material pore structure and graphitized structure

Method used

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  • Preparation method of porous graphitized hollow carbon microsphere
  • Preparation method of porous graphitized hollow carbon microsphere
  • Preparation method of porous graphitized hollow carbon microsphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Weigh 1 g of tannic acid and dissolve it in 10 mL of distilled water, add 0.05 g of melamine sponge into the tannic acid solution, stir to make it fully impregnated, and then add 10 mL of 0.05 g / mL ferric oxalate under stirring Potassium solution was added dropwise to the above mixed solution, after continuous stirring for 1 hour, thermal polymerization at 40°C for 4 hours, and the self-assembled iron-tannic acid polymer was obtained through the chelation and coordination of metal and tannic acid , and then dried in an oven at 80°C.

[0027] (2) Carbonize the dried solid in a nitrogen atmosphere, raise the temperature to 700°C at a rate of 5°C / min, keep it warm for 1 hour, cool naturally, and wash repeatedly with acid and distilled water to remove metal elements in the product and drying at 80°C to obtain the porous graphitized hollow carbon microspheres.

[0028] The prepared carbon microspheres were measured by D / max-2500 X-ray diffractometer, and the correspondi...

Embodiment 2

[0031] (1) Weigh 1 g of phytic acid and dissolve it in 10 mL of distilled water, add 0.1 g of melamine sponge into the phytic acid solution, stir to make it fully impregnated, and then add 10 mL of 0.1 g / mL potassium ferricyanide under stirring The solution was added dropwise to the above mixed solution, and after continuous stirring for 1 hour, thermal polymerization was carried out at 60°C for 6 hours at a low temperature to obtain a self-assembled iron-phytic acid polymer through the chelation and coordination of metal and phytic acid, and then placed Dry in an oven at 80°C.

[0032] (2) Carbonize the dried solid in a nitrogen atmosphere, raise the temperature to 800°C at a rate of 20°C / min, keep it warm for 2 hours after carbonization, cool naturally, and wash repeatedly with acid and distilled water to remove metal elements in the product and drying at 80°C to obtain the porous graphitized hollow carbon microspheres.

[0033] The method of testing its degree of graphitiz...

Embodiment 3

[0036] (1) Weigh 2 g of tannic acid and dissolve it in 20 mL of distilled water, add 0.2 g of melamine sponge into the tannic acid solution, stir to make it fully impregnated, and then add 20 mL of 0.25 g / mL oxalic acid under stirring Add the iron potassium solution dropwise to the above mixed solution, continue to stir for 1 hour, then thermally polymerize at 40°C for 8 hours, and obtain self-assembled iron-tannic acid polymerization through the chelation and coordination of metal and tannic acid were then dried in an oven at 80°C.

[0037](2) Carbonize the dried solid in a nitrogen atmosphere, raise the temperature to 750°C at a rate of 5°C / min, keep it warm for 2 hours, cool naturally, and wash repeatedly with acid and distilled water to remove metal elements in the product and drying at 80°C to obtain the porous graphitized hollow carbon microspheres.

[0038] The method of testing its degree of graphitization and specific surface area is the same as in Example 1.

[003...

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Abstract

The invention provides a preparation method of a porous graphitized hollow carbon microsphere, belonging to the field of preparation of porous carbon materials. According to the method, a soluble organic matter is used as a carbon precursor, potassium-iron double salt is used as a catalyst, and a hollow microsphere structure is formed through self-assembly by utilizing a chelating effect between hydroxyl oxygen and metal ions in an organic matter; in the carbonization process, based on the confinement and shape selection effects of uniformly-dispersed iron particles and the activation effect of potassium, graphitization and activation are realized at the same time; and finally, the porous graphitized hollow carbon microsphere with uniformly distributed graphitized structures is obtained. Compared with a technology for preparing the hollow carbon microsphere by adopting a template method, the method of self-assembling of an organic compound and metal ions in the invention has the advantages that the method is simple, cost is relatively low, and the obtained hollow carbon microsphere has high specific surface area and relatively high graphitization degree, and has huge application prospects in the fields of energy storage, catalysis, adsorption and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation of porous carbon materials, in particular to a preparation method of porous graphitized hollow carbon microspheres. [0002] technical background [0003] Hollow carbon microspheres have high specific surface area, abundant active sites, good electrical conductivity, and short ion diffusion path, so they have received extensive attention in the fields of energy storage, catalysis, and adsorption. The traditional preparation of hollow carbon microspheres mostly adopts the hard template method. For example, Liu Lei (CN 107032321 A) used silica nanospheres as the hard template, melamine formaldehyde resin as the carbon precursor, and hydroxyethylidene diphosphonic acid as the catalyst. Hollow carbon microspheres with macroporous-mesoporous structure were prepared after carbonization and template removal. The introduction of templates makes the preparation process cumbersome and increases the cost...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/205
CPCC01B32/205C01P2006/12C01P2004/03C01P2002/80C01P2002/72C01P2006/17
Inventor 张晓华闫晓燕刘宝胜张跃忠赵新新
Owner TAIYUAN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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