Method for controllably preparing nitrogen-doped porous carbon material, and application

A nitrogen-doped porous carbon and carbonization technology, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of low specific surface area, small specific capacitance, and inability to control nitrogen doping of carbon materials, and achieve a wide range of effects.

Inactive Publication Date: 2019-07-16
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] (2) Cellulose carboxylic acid derivatives are only used as carriers for metal materials
The prepared carbon materials have low specific surface area and small specific capacitance, and the nitrogen doping cannot be fundamentally controlled

Method used

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  • Method for controllably preparing nitrogen-doped porous carbon material, and application
  • Method for controllably preparing nitrogen-doped porous carbon material, and application
  • Method for controllably preparing nitrogen-doped porous carbon material, and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] We prepared nitrogen-doped porous carbon materials with different structures by using different activation temperatures.

[0075] Take 1 part of cellulose carboxylic acid derivative (CMC) and slowly add it to 80ml of pure water and stir for 2 hours to fully dissolve it to obtain product A; (2) Add 1 part of 1-methylimidazole organic base to product A and stir 12h, freeze-dried to obtain product B; (3) pulverized product B with a pulverizer, and then washed three times with ethyl acetate solvent to obtain product C; (4) vacuum-dried product C at 60°C for 12 hours to obtain proton-type polyionic liquid Precursor product D; (5) Pre-carbonize product D at 500°C for 2 hours in an argon atmosphere tube furnace at a heating rate of 5°C / min and argon flow of 200ml / min to obtain product E; (6) Pre-carbonize product E at 500°C for 2 hours Mix the product with KOH (C / KOH=1:4), place it in an argon atmosphere tube furnace, and activate it at different temperatures (700°C, 800°C, 90...

Embodiment 2

[0079] We prepared nitrogen-doped porous carbon materials with different structures by using polyionic liquid precursors of different cellulose carboxylic acid derivative protonic acids.

[0080] Take 1 part of cellulose carboxylic acid derivatives (carboxymethylcellulose CMC, cellulose-succinic anhydride, cellulose-maleic anhydride, cellulose-phthalic anhydride) and slowly add it to 80ml of pure water and stir for 2h, Make it fully dissolved to obtain product A; (2) add 1 part of 1-methylimidazole to product A and stir for 12 hours, freeze-dry to obtain product B; (3) grind product B with a pulverizer, and then use ethyl acetate The solvent was washed three times to obtain product C; (4) product C was vacuum-dried at 60°C for 12 hours to obtain product D of the proton-type polyionic liquid precursor; (5) product D was placed in an argon atmosphere tube furnace with a heating rate of 5 ℃ / min, the argon gas flow rate is 200ml / min, pre-carbonize at 500℃ for 2h to obtain product ...

Embodiment 3

[0082] We prepared nitrogen-doped porous carbon materials with different structures by using different organic bases.

[0083] Take 1 part of cellulose carboxylic acid derivative and slowly add it into 80ml of pure water and stir for 2 hours to fully dissolve it to obtain product A; (2) add 1 part of organic base (1,8-diazabicyclo [5.4.0] Undec-7-ene, 1-methylimidazole, triethylamine, 1,1,3,3-tetramethylguanidine) and stirred for 12h, freeze-dried to obtain product B; (3) Product B was pulverized with a pulverizer, and then washed three times with ethyl acetate solvent to obtain product C; (4) product C was vacuum-dried at 60°C for 12 hours to obtain product D, a proton-type polyionic liquid precursor; (5) product D was In an argon atmosphere tube furnace, the temperature rise rate is 5°C / min, the flow rate of argon gas is 200ml / min, pre-carbonize at 500°C for 2 hours to obtain product E; (6) fully mix product E with KOH (C / KOH=1: 4), placed in an argon atmosphere tube furnac...

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Abstract

The invention discloses a method for controllably preparing a nitrogen-doped porous carbon material, and an application. The method comprises the steps of 1) mixing cellulose carboxylic acid derivatives and organic base in water, carrying out oil bath at 20-45 DEG C, reacting for 1-24 hours to synthesize a cellulose carboxylic acid derivative proton type ionic liquid solution, and carrying out drying to obtain a product A; 2) crushing the product A by a crusher, washing the product A with an ethyl acetate solvent, and carrying out vacuum drying at 20-65 DEG C for 10-15 hours to obtain a cellulose carboxylic acid derivative proton type polyionic liquid product B; 3) carbonizing the product B through a direct carbonization method or a two-step method to obtain an initial product C of the nitrogen-doped carbon material; and 4) washing the product C with hydrochloric acid and pure water, and carrying out vacuum drying at 80-120 DEG C for 10-15 hours to obtain the nitrogen-doped porous carbon material. The nitrogen-doped porous carbon material is used as an electrode in the field of energy storage, and has the characteristics that the raw materials are environment-friendly and wide in source, the preparation process is simple, the power density is high in application to the field of batteries, the charging time is short, and the cycle life is long.

Description

technical field [0001] The invention relates to a method and application for controllable preparation of nitrogen-doped porous carbon materials, in particular to a method and application for preparing nitrogen-doped porous carbon materials by using cellulose carboxylic acid derivative proton type polyionic liquid as a precursor. Background technique [0002] Carbon anode materials are currently used in supercapacitor electrode materials, and their materials are basically carbon materials, such as artificial graphite, natural graphite, mesocarbon microspheres, petroleum coke, carbon fiber, pyrolytic resin carbon, etc. However, due to the low theoretical specific capacitance of this carbon material, it is far from meeting the actual needs, and the miscibility of this graphite material with organic solvents is poor, and the high-current charge and discharge performance is not good. Therefore, in order to change this situation, researchers introduced heterogens such as N, O, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01G11/34H01M4/583
CPCH01G11/34H01M4/583Y02E60/10
Inventor 徐芹芹李在权谢海波
Owner GUIZHOU UNIV
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