Method for preparing nitrogen-doped carbonaceous material by modifying polymer

A technology of carbonaceous materials and nitrogen-doped carbon, applied in the direction of carbon compounds, chemical instruments and methods, nano-carbon, etc., can solve the problems of low nitrogen doping, reduced electrical conductivity, and damage to the original structure of carbon materials, and achieves applicable Wide range of properties, simple process, and the effect of improving specific capacity

Inactive Publication Date: 2012-12-19
UNIV OF SCI & TECH LIAONING
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Problems solved by technology

[0003] At present, there are mainly the following methods for synthesizing or preparing nitrogen-doped carbonaceous materials: one is to use nitrogen-containing precursors as carbon sources in the process of synthesizing carbon materials to achieve the purpose of nitrogen doping, but due to the thermal During the solution process, a large amount of nitrogen is lost in the form of gas, so it is difficult to obtain high nitrogen doping content, and the process of catalyst removal usually destroys the intrinsic structure of carbonaceous materials (Sen, R. Satishkumar, B. C.; Govindaraj, A.; et al ., Nitrogen-containing carbon nanotubes, J. Mater. Chem., 1997, 7(12): 2335); The other is to carry out nitrogen doping by surface chemical modification of synthesized carbon materials, such as strong acid or NH 3 Such chemical treatment methods can achieve effective nitrogen doping of carbon materials, but this treatment method will also lead to the destruction of the original structure of carbon materials, such as the reduction of electrical conductivity, while introducing nitrogen-containing functions (Arrigo, R , Havecker, M. Schlogl, R. Su, D. S, Dynamic surface rearrangement and thermal stability of nitrogen functional groups on carbon nanotubes Chem. Commun., 2008: 4891); Nitrogen doping of carbon materials with nitrogen-containing organic solvents It is a relatively mild method. Because carbonaceous materials have good compatibility with organic solvents, it is beneficial to uniform nitrogen doping of carbon materials, and will not significantly damage the original structural characteristics of carbon materials, but its nitrogen doping (Li Lixiang, Liu Yongchang, Geng Xin, An Baigang, Preparation and Electrochemical Properties of Nitrogen-doped Carbon Nanotubes, Acta Physicochemical Sinica, 2011, 27: 443)

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  • Method for preparing nitrogen-doped carbonaceous material by modifying polymer
  • Method for preparing nitrogen-doped carbonaceous material by modifying polymer
  • Method for preparing nitrogen-doped carbonaceous material by modifying polymer

Examples

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Embodiment 1

[0019] Example 1, preparation of polymer modified nitrogen-doped carbon material polyaniline modified nitrogen-doped carbon nanotubes

[0020] The multi-walled carbon nanotubes produced by a Japanese company are used, and the average outer diameter is 30-60nm. Weigh 60 mg, add it to a hydrochloric acid solution with a concentration of 0.2 mol / L, then add 0.35 g of aniline, and ultrasonically disperse for 0.5 hours. Stir at room temperature for 0.5 hours, add 0.5 g of ammonium persulfate, continue to stir for 1.5 hours, then cool the solution to 0~5°C in an ice-water mixed bath, then wash with deionized water, filter, and filter the obtained product in the Vacuum drying at 80°C for 10 hours; the dried product was heat-treated at 600°C under the protection of nitrogen, the heating rate was 5°C / min, the constant temperature time was 1 hour, and then naturally cooled to room temperature. The X-ray photoelectron spectrum of the multi-walled carbon nanotube before and after the abo...

Embodiment 2

[0021] Example 2, preparation of polymer modified nitrogen-doped carbon material polypyrrole modified nitrogen-doped activated carbon

[0022] The activated carbon prepared by CVD method has an average diameter of 60nm. No nitrogen element before nitrogen doping. Weigh 1 g of activated carbon, add it to a hydrochloric acid solution containing 0.5 g of pyrrole and a concentration of 1 mol / L, then add 1 g of ammonium persulfate, and continue stirring for 1.5 hours at room temperature. Repeated washing with deionized water and membrane filtration. Dry under vacuum at 40°C for 16 hours. Heat treatment at 850°C under the protection of nitrogen, with a heating rate of 4°C / min, constant temperature for 2 hours, and natural cooling. As determined by X-ray photoelectron spectroscopy, see image 3 , Figure 4 , it can be seen that the nitrogen-doped activated carbon of the product prepared by the method of this embodiment contains 13% atomic percentage of nitrogen. The prepared ni...

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Abstract

The invention discloses a method for preparing a nitrogen-doped carbonaceous material by modifying polymer, which can be used for preparing the nitrogen-doped carbonaceous material with the nitrogen doping amount of 5 to 26 at%. The method disclosed by the invention is characterized by comprising the following steps of: selecting a nitrogen-containing organic compound as a nitrogen precursor and utilizing the nitrogen-containing organic compound to perform polymerization reaction on a carbonaceous material to form a compound of the nitrogen-containing polymer and carbonaceous material; and then carrying out heat treatment on the polymer/carbonaceous material compound in the inert atmosphere to carbonize nitrogen-containing polymer in the compound so as to implement the nitrogen doping on the carbonaceous material and prepare the nitrogen-doped carbonaceous material. According to the invention, when the carbonaceous material is subjected to effective nitrogen doping, the original intrinsic structure of the carbonaceous material can be ensured; moreover, the nitrogen-doped carbonaceous material with the nitrogen content of 5 to 26 at% can be prepared; the specific capacity of using a carbon material as an electrode material of a supercapacitor is obviously improved; and the method has the characteristics of simple technical process and wide applicability.

Description

technical field [0001] The invention relates to the preparation technology of nitrogen-doped carbonaceous materials, in particular to a method for preparing nitrogen-doped carbonaceous materials by polymer modification. Background technique [0002] Due to their unique physical and chemical properties, carbon materials have extensive and important applications in the fields of materials, chemicals, biomedicine, energy, electronics, aerospace, and military industries. In recent years, with the development of new carbon materials (such as carbon nanotubes, graphene, etc.) one. However, due to the hydrophobic nature of carbon and its low surface activity, the wide application of carbon materials, especially some nano-carbon materials or porous carbon materials (carbon fibers, carbon nanotubes, activated carbon, graphene, etc.), is limited. , by modifying the surface of carbon materials to improve their water dispersibility and surface activity, it has become an effective way ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C01B31/04C01B31/08C01B32/00C01B32/156C01B32/168C01B32/194C01B32/354
Inventor 安百钢李莉香陶晶耿新
Owner UNIV OF SCI & TECH LIAONING
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