N-rich mesoporous carbon material and template-free preparation method thereof as well as method for manufacturing working electrode and application of working electrode

A technology of nitrogen-rich mesoporous and working electrodes, which is applied in the preparation/purification of carbon, etc., can solve the problem that the structure and composition of nitrogen-rich mesoporous carbon materials lack effective control of the arrangement and orientation of mesoporous surface atoms, and achieve low cost, The effect of large pore volume and simple operation

Inactive Publication Date: 2012-10-03
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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Problems solved by technology

It has been reported that the nitrogen-rich mesoporous carbon materials prepared by this method are still limited to aromatic cyano and cyanamide compounds, and the structure and composition of the nitrogen-rich mesoporous carbon materials prepared are still lacking in effective control ( Microscopic mesoporous ...

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  • N-rich mesoporous carbon material and template-free preparation method thereof as well as method for manufacturing working electrode and application of working electrode
  • N-rich mesoporous carbon material and template-free preparation method thereof as well as method for manufacturing working electrode and application of working electrode
  • N-rich mesoporous carbon material and template-free preparation method thereof as well as method for manufacturing working electrode and application of working electrode

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preparation example Construction

[0030] Preparation of nitrogen-rich mesoporous carbon

[0031] The structural formula of the building block used in the implementation case:

[0032]

Embodiment 1

[0034] 307mg of melamine and 500mg of terephthalaldehyde (molar ratio 1:1.5) were placed in a three-necked flask, and 16mL of dimethyl sulfoxide solution was added to fully dissolve them. Heat to reflux at 180 °C for 72 hours under an inert atmosphere. After cooling to room temperature, the precipitate was filtered and separated by Buchner funnel and THF was extracted by Soxhlet to obtain a three-dimensional mesoporous polyimide white powder prepared by Schiff base chemical adjustment, with a yield of 61% and a pore volume of 1.01cm 3 g -1 , pore size 3.3nm, specific surface area 1377m 2 g -1 , where the nitrogen adsorption-desorption isotherm belongs to Type IV (such as figure 1 Shown in a), elemental analysis proves that the molar ratio of carbon to nitrogen in nitrogen-rich mesoporous carbon is 1:1.

[0035] Low-temperature calcination under argon or nitrogen to obtain a polyimide precursor with a high degree of polymerization, wherein the low-temperature calcination te...

Embodiment 2

[0037] 231 mg of melamine and 500 mg of p-naphthalene dicarbaldehyde ((molar ratio 1:1.5)) were placed in a three-necked flask, and 11 mL of dimethyl sulfoxide solution was added to fully dissolve them. Heat to reflux at 180 °C for 72 hours under an inert atmosphere. After cooling to room temperature, the precipitate was filtered and separated by Buchner funnel and THF was extracted by Soxhlet to obtain a light yellow powder of three-dimensional mesoporous polyimide prepared by Schiff base chemical adjustment, with a yield of 66% and a pore volume of 0.73 cm 3 g -1 , pore size 3.8nm, specific surface area 1032m 2 g -1 , where the nitrogen adsorption-desorption isotherm belongs to Type IV (such as figure 1 Shown in b), elemental analysis proves that the molar ratio of carbon to nitrogen in nitrogen-rich mesoporous carbon is 1:1.

[0038] Low-temperature calcination under argon or nitrogen to obtain a polyimide precursor with a high degree of polymerization, wherein the low-...

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Abstract

The invention discloses an N-rich mesoporous carbon material and a template-free preparation method thereof as well as a method for manufacturing a working electrode and an application of the working electrode, and belongs to the technical field of mesoporous carbon material preparation. In organic solvent, substituted dialdehyde and a melamine derivative are taken as building units; through heating reflux under the inert atmosphere, the building units are subject to the Schiff base reaction to obtain a mesoporous polyamid precursor, and are subject to the low-tempreature roasting under the inert atmosphere to be further carbonized to obtain N-rich mesoporous carbon; or the polyamid precursor is subject to one-step high-temperature carbonization to obtain N-rich mesoporous carbon. Through the adjusting of the structures of the substituted dialdehyde and the melamine derivative and the pyrolysis conditions of the polyamid precursor, the controllable synthesis of N-rich mesoporous carbon is achieved. The invention can achieve the template-free synthesis of the N-rich mesoporous carbon, and has the advantages of simplicity in operation, low cost and large-scale production. The optimized N-rich mesoporous carbon materials are made into an electrode which has a favorable capacitance performance, rapid current response and a stable cycle life under acidic and alkaline conditions.

Description

technical field [0001] The invention belongs to the technical field of mesoporous carbon material preparation, and specifically relates to a novel nitrogen-rich mesoporous carbon material, a preparation method and its application as an electrode material in an electrochemical capacitor. Background technique [0002] Mesoporous carbon materials have: (1) regular pore structure, uniform pore size / arrangement; (2) narrow pore size distribution, pore size can be continuously adjusted in a wide range; (3) large specific surface area and pore volume; (4) After optimized synthesis conditions or pretreatment, it can have good thermal and chemical stability; (5) The particles have a regular shape and maintain a high degree of pore order, so in recent years it has become One of the hot materials of international interdisciplinary research. The mesoporous carbon materials obtained by further functionalization will surely show more excellent performance and expand its practical applica...

Claims

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Application Information

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IPC IPC(8): C01B31/02C01B32/05
Inventor 梁彦瑜来庆学
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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