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Method for preparing nitrogen-doped carbon aerogel

A technology of carbon airgel and nitrogen doping, which is applied in the direction of nano-carbon, electrical components, electrochemical generators, etc., can solve the problems of long cycle, complicated preparation process, single structure of carbon airgel, etc., and achieve low price , rich nitrogen content, and good electrochemical stability

Active Publication Date: 2018-04-06
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above-mentioned carbon airgel preparation process is complicated, and there are many instruments used in the operation process, such as the critical carbon dioxide extraction instrument, and the cycle used is also long. Most of the raw materials are toxic and harmful substances such as melamine, resorcinol and formaldehyde. , and the structure of the formed carbon airgel is relatively simple

Method used

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  • Method for preparing nitrogen-doped carbon aerogel
  • Method for preparing nitrogen-doped carbon aerogel
  • Method for preparing nitrogen-doped carbon aerogel

Examples

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Effect test

Embodiment 1

[0024] A method for preparing nitrogen-doped carbon airgel, comprising the following steps:

[0025] Step 1: Add 2 g of bean dregs to 30 mL of concentrated sulfuric acid with a mass concentration of 30% and stir at 600 r / min for 5 h to form a carbon sol precursor.

[0026] Step 2: The carbon sol precursor was diluted 5 times with water, that is, the amount of water added was 4 times the volume of concentrated sulfuric acid, and then microwave hydrothermal treatment was performed at a temperature of 150°C for 90 minutes to obtain a carbon aerogel.

[0027] Step 3: Suction filter the obtained carbon aerogel, dry it in an oven at 60°C and put it into a nitrogen atmosphere furnace, raise the temperature from room temperature to 600°C at a rate of 5°C / min, and the flow rate of nitrogen gas 60mL / min, keep warm for 90min. Nitrogen-doped carbon aerogels can be obtained after cooling.

Embodiment 2

[0029] A method for preparing nitrogen-doped carbon airgel, comprising the following steps:

[0030] Step 1: Add 2 g of bean dregs to 32 mL of concentrated sulfuric acid with a mass concentration of 50% and stir at 500 r / min for 6 h to form a carbon sol precursor.

[0031] Step 2: Dilute the carbon sol precursor 6 times with water, that is, the amount of water added is 5 times the volume of concentrated sulfuric acid, and then perform microwave hydrothermal treatment at a temperature of 160°C for 100 minutes to obtain carbon airgel.

[0032] Step 3: Suction filter the obtained carbon aerogel, dry it in an oven at 70°C and put it in a nitrogen atmosphere furnace, raise the temperature from room temperature to 700°C at a rate of 6°C / min, and the flow rate of nitrogen gas 60mL / min, heat preservation for 100min, and nitrogen-doped carbon airgel can be obtained after cooling.

Embodiment 3

[0034] A method for preparing nitrogen-doped carbon airgel, comprising the following steps:

[0035] Step 1: Add 2 g of bean dregs to 34 mL of concentrated sulfuric acid with a mass concentration of 40% and stir at 400 r / min for 7 h to form a carbon sol precursor.

[0036] Step 2: The carbon sol precursor was diluted 7 times with water, that is, the amount of water added was 6 times the volume of concentrated sulfuric acid, and then microwave hydrothermal treatment was performed at a temperature of 160°C for 100 minutes to obtain a carbon aerogel.

[0037] Step 3: Suction filter the obtained carbon aerogel, dry it in an oven at 70°C, put it into a nitrogen atmosphere furnace, and raise the temperature from room temperature to 800°C at a rate of 7°C / min. 70mL / min, keep warm for 120min. Nitrogen-doped carbon aerogels can be obtained after cooling.

[0038] Depend on figure 1 It can be seen that the carbon airgel prepared by the present invention contains C-N bonds.

[0039] ...

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Abstract

Provided is a method for preparing nitrogen-doped carbon aerogel. Bean dregs are taken as a carbon source, concentrated sulfuric acid is taken as a hydrolyst, and the bean dregs and the concentrated sulfuric acid are evenly stirred after mixing to form a carbon dissolved gel precursor; water is added into the carbon dissolved gel precursor for dilution, through microwave hydrothermal treatment, brown sediment is obtained, the brown sediment is subjected to extraction filtration and drying, and finally, through high-temperature carbonization, the nitrogen-doped carbon aerogel is obtained. According to the method, the bean dregs are taken as the raw material to prepare the nitrogen-doped carbon aerogel, wherein the bean dregs, as food processing waste, are wide in source and low in cost; thepreparation process where catalyzed hydrolysis, microwave hydrothermal treatment and high-temperature carbonization are adopted is simple and suitable for large-scale industrialized production; the product has the advantages of being high in nitrogen content, high in specific surface area and stable in structure, and can be applied to lithium-ion batteries and supercapacitors.

Description

technical field [0001] The invention belongs to the technical field of preparation of nano-carbon materials, and in particular relates to a method for preparing nitrogen-doped carbon airgel. Background technique [0002] Carbon airgel is a lightweight porous carbon material with a three-dimensional nano-network structure. It is the lightest solid condensed material. It can be used in mechanics, heat, optics, and acoustics. It has unique properties and uses. Carbon aerogels have the advantages of high specific surface area, low and controllable density, high porosity, adjustable pore size distribution, and good electrical conductivity. Compared with ordinary carbon aerogels, nitrogen-doped carbon aerogels have more active sites and have better performance. Since the diameters of nitrogen atoms and carbon atoms are similar, when nitrogen atoms replace carbon atoms in carbon materials, the structure of the material will not be greatly distorted. After nitrogen atoms enter the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/15H01G11/32H01M4/583H01M10/0525
CPCC01P2002/80C01P2002/85C01P2004/03C01P2006/12C01P2006/16H01G11/32H01M4/583H01M10/0525Y02E60/10Y02E60/13
Inventor 李翠艳马媛月欧阳海波弓琴琴黄剑锋费杰
Owner SHAANXI UNIV OF SCI & TECH
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