Preparation method of nitrogen-doped porous carbon material based on organic covalent framework

A nitrogen-doped porous carbon and covalent technology, which is applied in the field of supercapacitor electrode materials and composite materials, can solve the problem of low specific capacity and achieve the effects of low density, good cycle stability, and good electrical storage performance

Inactive Publication Date: 2018-05-15
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the specific capacity of these carbon supercapacitors is very low, generally in the range of 100-200F / g

Method used

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  • Preparation method of nitrogen-doped porous carbon material based on organic covalent framework
  • Preparation method of nitrogen-doped porous carbon material based on organic covalent framework
  • Preparation method of nitrogen-doped porous carbon material based on organic covalent framework

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Dissolve 0.9733g of p-phenylenediamine and 1.107g of cyanuric chloride (the molar ratio of substances is 3:2) in 35ml and 10ml of dioxane-mesitylene-acetic acid mixed solvents respectively (the volume ratio of the three solvents is 5 :5:1), then transfer the mixed solution to a stainless steel autoclave, and keep it at 120°C for 70 hours; the product is washed repeatedly with tetrahydrofuran and methanol, after washing, it is vacuum dried at 120°C for 24 hours, and the obtained Earthy yellow powder precursor. Burn the precursor at 700°C for 3 hours in a nitrogen atmosphere to obtain a black carbon material product with a specific surface area of ​​about 398m 2 g -1 , with a pore size of about 1 nm.

[0036] The calomel electrode was used as the reference electrode, the platinum sheet electrode was used as the auxiliary electrode, the active material was coated on the nickel foam as the working electrode, and 6 M KOH was used as the electrolyte to conduct the electroch...

Embodiment 2

[0038] Dissolve 0.9733g of p-phenylenediamine and 1.107g of cyanuric chloride (the molar ratio of substances is 3:2) in 35 ml and 10ml of dioxane-mesitylene-acetic acid mixed solvents respectively (the volume ratio of the three solvents is 5:5:1), then transfer the mixed solution to a stainless steel autoclave, and keep it at 120°C for 70 hours; the product is washed repeatedly with tetrahydrofuran and methanol, after washing, it is vacuum-dried at 120°C for 24 hours, and ground to obtain The khaki powder precursor. The precursor was burned at 500 °C for 3 hours in a nitrogen atmosphere to obtain a black carbon material product with a specific surface area of ​​about 60 m 2 g -1, the pore size is about 1.4nm. When the current density is 0.5 A g -1 , the specific capacitance is 1155 F·g -1 .

Embodiment example 3

[0040] Dissolve 0.9733g of p-phenylenediamine and 1.107g of cyanuric chloride (the molar ratio of substances is 3:2) in 35 ml and 10ml of dioxane-mesitylene-acetic acid mixed solvents respectively (the volume ratio of the three solvents is 5:5:1), then transfer the mixed solution to a stainless steel autoclave, and keep it at 120°C for 70 hours; the product is washed repeatedly with tetrahydrofuran and methanol, after washing, it is vacuum-dried at 120°C for 24 hours, and ground to obtain The khaki powder precursor. Burn the precursor at 700 °C for 1.5 hours in a nitrogen atmosphere to obtain a black carbon material product with a specific surface area of ​​about 100 m 2 g -1 , with a pore size of about 1.2 nm. When the current density is 0.5 A g -1 , the specific capacitance is 1095 F·g -1 .

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Abstract

The invention provides a preparation method of a nitrogen-doped porous carbon material based on an organic covalent framework. The preparation method comprises the following steps: carrying out a solvothermal reaction on phenylenediamine and cyanuric chloride in a 1,4-dioxane-mesitylene-acetic acid mixed solvent, repeatedly washing the product with tetrahydrofuran and methanol, drying and grindingto obtain a precursor; and calcining the precursor in a nitrogen atmosphere, thereby obtaining the nitrogen-doped porous carbon material. The carbon material has large specific surface area, low density and high nitrogen content, is applied to a super-capacitor negative electrode material and has excellent electrical storage property and cycling stability. The nitrogen-doped porous carbon material has excellent performance.

Description

technical field [0001] The present invention relates to a method for synthesizing nitrogen-doped porous carbon materials, in particular to a method for preparing nitrogen-doped porous carbon materials based on organic covalent frameworks, which are mainly used as electrode materials for supercapacitors and belong to the field of composite materials and supercapacitors. The technical field of capacitor electrode materials. Background technique [0002] Covalent organic frameworks (COFs) are a new class of porous organic materials, which have the advantages of large specific surface area, rich pore structure, light weight, orderly structure, and adjustable structure and pore size. In 2005, the Yaghi team at the University of Michigan in the United States successfully prepared the first covalent organic framework polymer COF-1 by dehydration condensation of 1,4-p-diphenylboronic acid itself. Actively engage in research in this field. In terms of the synthesis and application ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/05
Inventor 郭昊薛瑞王婷黄冬冬杨武
Owner NORTHWEST NORMAL UNIVERSITY
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