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Preparation method of high nitrogen content-doped porous carbon with high specific surface area

A technology with high specific surface area and high nitrogen content, applied in the field of nanomaterials, can solve the problems of unsuitable industrial application, cumbersome and complex process, unfriendly environment, etc. Effect

Active Publication Date: 2014-07-16
TONGJI UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

Although porous carbon with high nitrogen content and high specific surface area can be obtained by in-situ nitrogen doping, there are many problems, such as: the preparation process requires the use of many organic chemical reagents, which are relatively expensive; the template removal process requires the use of hydrogen fluorine acid and other strong corrosive agents, the process is cumbersome and unfriendly to the environment, so this method is not suitable for industrial applications

Method used

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  • Preparation method of high nitrogen content-doped porous carbon with high specific surface area
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  • Preparation method of high nitrogen content-doped porous carbon with high specific surface area

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Embodiment 1

[0031] Such as figure 1 as shown, figure 1 It is a flow chart of the preparation method of high specific surface area and high nitrogen content doped porous carbon shown in the embodiment. A method for preparing porous carbon doped with high specific surface area and high nitrogen content, comprising the following steps:

[0032] Put the biomass raw material corncob in a blast drying oven, dry at a temperature of 100°C for at least 24 hours, crush and sieve, control the particle size to 200um, put the particles into the material boat, and place the material boat in the atmosphere furnace In the process, vacuumize the furnace cavity, and then replace it twice with nitrogen gas, and obtain carbides after high-temperature carbonization treatment in a nitrogen atmosphere. The nitrogen flow rate is 0.5L / min, and the temperature is programmed from room temperature to 400°C. For 3 hours, the heating rate is 5°C / min; then the carbide is dispersed in a saturated solution of potassium...

Embodiment 2

[0036] A method for preparing porous carbon doped with high specific surface area and high nitrogen content, comprising the following steps:

[0037] Put the biomass raw material coconut shell in a blast drying oven, dry at a temperature of 150°C for at least 24 hours, crush and sieve, control the particle size to 500um, put the particles into the material boat, and place the material boat in the atmosphere furnace In the process, vacuumize the furnace cavity, and then replace it twice with nitrogen gas, and obtain carbides after high-temperature carbonization treatment in a nitrogen atmosphere. The nitrogen flow rate is 2L / min, and the temperature is programmed from room temperature to 300°C. 5 hours, the heating rate is 3°C / min; then the carbide is dispersed in a saturated solution of potassium hydroxide, the mixing ratio of potassium hydroxide solution and carbide is 2:1, the stirring time is 0.5 hour, and the alkali carbon is obtained after drying Mixture: put the alkali-c...

Embodiment 3

[0039] A method for preparing porous carbon doped with high specific surface area and high nitrogen content, comprising the following steps:

[0040] Put the biomass raw bamboo leaves in a blast drying oven and dry them at a temperature of 125°C for at least 24 hours. After crushing and sieving, the particle size is controlled to 25um. Put the particles into the material boat, and place the material boat in the atmosphere furnace In the process, vacuumize the furnace cavity, and then replace it with nitrogen twice. Carbide is obtained after high-temperature carbonization treatment under nitrogen atmosphere. The nitrogen flow rate is 1.25L / min, and the temperature is programmed from room temperature to 500°C. The treatment time is For 2 hours, the heating rate is 4°C / min; then the carbide is dispersed in a saturated solution of potassium hydroxide, the mixing ratio of potassium hydroxide solution and carbide is 3:1, the stirring time is 0.75 hours, and the alkali is obtained aft...

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Abstract

The invention discloses a preparation method of high nitrogen content-doped porous carbon with a high specific surface area. The preparation method comprises the following steps: drying and smashing a biomass raw material to obtain particles and carbonizing the particles in a nitrogen atmosphere at a high temperature to obtain carbide; then, dispersing the carbide in a potassium hydroxide solution, and stirring and drying to obtain an alkali and carbon mixture; activating the alkali and carbon mixture at the high temperature in the nitrogen atmosphere, and washing, filtering and drying to obtain the porous carbon material; uniformly dispersing the porous carbon material in a strong acid solution for oxidation treatment, and filtering, washing and drying to obtain an oxidized porous carbon material; and finally, ammonifying the oxidized porous carbon material at the high temperature in an ammonia atmosphere to obtain the high nitrogen content-doped porous carbon with the high specific surface area. The specific surface area of the doped porous carbon is 2500-3500<m2> / g, the pore diameter of the material is 0.5-6nm and the nitrogen content is 4-12%. The method disclosed by the invention is simple and effective, easy to operate, convenient for batch production on a large scale and suitable for application in industrial production.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, in particular to a method for preparing porous carbon doped with high specific surface area and high nitrogen content. Background technique [0002] Due to the characteristics of surface chemical inertness, high mechanical stability, good electrical conductivity, and large specific surface area and pore volume, porous carbon materials have shown great applications in the fields of carbon dioxide adsorption, catalysis, hydrogen storage, supercapacitors and lithium batteries. potential. [0003] Since Ryoo et al. (J.Phys.Chem.B, 1999, 103, 7743) used MCM-48 mesoporous silica as a hard template and sucrose as a carbon precursor to synthesize highly ordered carbon molecular sieves for the first time, in the porous carbon materials Great progress has been made in the synthesis and application. However, the surface properties of pure carbon materials are limited, which limits their practi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C01B32/05
Inventor 张存满耿振王达斌周向阳
Owner TONGJI UNIV
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