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Nitrogen-doped carbon material and preparation method thereof

A nitrogen-doped carbon and electrode material technology, applied in the field of materials, can solve the problems of low capacitance performance, high equipment requirements, complicated processes, etc., and achieve the effects of low cost, simple preparation method and broad application prospects.

Active Publication Date: 2019-04-19
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, nitrogen-doped carbon materials have a wide range of availability in heteroatom-doped carbon materials, and nitrogen-containing functional groups can mainly be combined with nitrogen-containing reagents (such as NH 3 , nitric acid and amine) reaction or calcined carbonization of nitrogen-rich precursors (such as polyacrylonitrile, melamine), etc. However, it is necessary to introduce a pore-forming agent or undergo etching under harsh conditions to obtain a three-dimensional porous structure. The equipment requirements are high, the process is complicated, and the performance effect of the obtained capacitor is not very high.

Method used

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  • Nitrogen-doped carbon material and preparation method thereof

Examples

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Effect test

Embodiment 1

[0043] (1) Weigh 5.19g of p-phenylenediamine and 9.71g of triethylamine in a 250ml conical flask, then measure 150ml of tetrahydrofuran as a solvent, and stir ultrasonically to completely dissolve p-phenylenediamine; Add 8.85g of cyanuric chloride and 50ml of tetrahydrofuran to the solution; after p-phenylenediamine and cyanuric chloride are completely dissolved, pre-ice bath for 1h for later use.

[0044] (2) Add cyanuric chloride solution while stirring (1000rpm) in the p-phenylenediamine solution in a complete ice bath, and place it in an ice bath environment at 0°C to react for 1 hour; after the ice bath reaction, continue to react at room temperature for 24 hours; Finally, the reaction was condensed and refluxed at 60°C for 24 hours; after the synthesis, the polymer was centrifuged and washed three times with ethanol, ultrapure water and concentrated hydrochloric acid, and dried in a vacuum oven at 60°C for 24 hours.

[0045] (3) After the product is completely dried, mea...

Embodiment 2

[0050] (1) Weigh 5.19g of p-phenylenediamine and 9.71g of triethylamine in a 250ml conical flask, then measure 150ml of tetrahydrofuran as a solvent, and stir ultrasonically to completely dissolve p-phenylenediamine; Add 8.85g of cyanuric chloride and 50ml of tetrahydrofuran to the solution; after p-phenylenediamine and cyanuric chloride are completely dissolved, pre-ice bath for 1h for later use.

[0051](2) Add cyanuric chloride solution while stirring (1000rpm) in the p-phenylenediamine solution in a complete ice bath, and place it in an ice bath environment at 0°C to react for 1 hour; after the ice bath reaction, continue to react at room temperature for 24 hours; Finally, the reaction was condensed and refluxed at 60°C for 24h; after the synthesis, the polymer was centrifuged and washed three times with ethanol and ultrapure water respectively, and dried in a vacuum oven at 60°C for 24h.

[0052] (3) Weigh 0.5g of dried product in a boat-shaped crucible, 2 Calcination an...

Embodiment 3

[0056] Nitrogen-doped carbon materials were prepared at different calcination temperatures. Referring to Example 1, the calcination temperatures in step (4) were replaced with the temperature values ​​in Table 1, and other conditions remained unchanged, and nitrogen-doped carbon materials were obtained. The capacitance results of the obtained materials at a current density of 1A / g are shown in Table 1.

[0057] Table 1 Capacitance of nitrogen-doped carbon materials prepared at different calcination temperatures

[0058] Calcination temperature °C

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Abstract

The invention discloses a nitrogen-doped carbon material and a preparation method thereof, and belongs to the field of materials. According to the invention, cyanuric chloride is used as a raw material, and the three chlorines have different activities, and respectively react with the amino group of p-phenylenediamine under three different temperatures, so a triazine network structure is constructed, and a nitrogen-doped carbon material having three-dimensional porosity is preprared. The preparation method of the nitrogen-doped carbon material of the invention is simple, and the obtained material can directly form a three-dimensional porous carbon material through calcinations; participation of a pore-forming agent is not required; an etching process is not required; and the material and the preparation method are low in cost and suitable for industrial production. The nitrogen-doped carbon material of the invention has quite high electric capacity which can reach 264 F / g, is a favorable electrode material of a supercapacitor, can be used for preparing the supercapacitor, and has a broad application prospect.

Description

technical field [0001] The invention relates to a nitrogen-doped carbon material and a preparation method thereof, belonging to the field of materials. Background technique [0002] Supercapacitors (electrochemical capacitors) have been widely used in alternative batteries and fuel cells for energy storage / conversion applications due to their advantages of high power capacity, long cycle life, fast charge-discharge rate, light weight, and environmental friendliness. [0003] Electrode materials for supercapacitors mainly include carbon materials, metal oxides, and conductive polymers. Carbon materials mainly use the interface electric double layer of active material and electrolyte to store energy. It is a typical EDLC material. The abundant pore volume and high specific surface area are important factors that determine the capacitance. However, if carbon materials only rely on electric double layer capacitance, they have low specific capacitance and poor hydrophilicity, wh...

Claims

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Application Information

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IPC IPC(8): H01G11/24H01G11/30H01G11/34H01G11/44H01G11/38H01G11/86
CPCH01G11/24H01G11/30H01G11/34H01G11/38H01G11/44H01G11/86Y02E60/13
Inventor 王利魁刘云杨井国张佳瑜刘竞姚伯龙
Owner JIANGNAN UNIV
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