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Preparation method and application of nitrogen-containing porous carbon material based on polyaspartic acid salt

A polyaspartate and porous carbon material technology, which is applied in the preparation/purification of carbon, hybrid capacitor electrodes, etc., can solve the problems of cumbersome steps, high separation and purification difficulty, uneven distribution, etc., and achieves uniform pore size distribution, The effect of uniform distribution of nitrogen atoms and pore size and loss reduction

Active Publication Date: 2019-12-17
ENERGY RESOURCES INST HEBEI ACADEMY OF SCI
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Problems solved by technology

Currently reported methods for preparing nitrogen-containing porous carbon materials include CN107555412A and the application of the applicant a few days ago. CN107555412A discloses a method for preparing nitrogen-doped porous carbon. A transparent solution is prepared by dissolving the nitrogen source in a solvent, and the An appropriate amount of carbon source is added to the solution to form a fluffy snowflake-like substance, which is obtained by freeze-drying and then heating, separating and purifying. This method has cumbersome steps and is difficult to separate and purify.
The applicant has applied for a few days ago, which discloses a carbon source, nitrogen source and mixed eutectic salt for ball milling, followed by carbonization and pickling to prepare nitrogen-containing porous carbon materials. Although the use of solvents is avoided, it is still It is impossible to completely avoid the phenomenon that the nitrogen source is unevenly distributed in the material due to the addition of an external nitrogen source

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  • Preparation method and application of nitrogen-containing porous carbon material based on polyaspartic acid salt
  • Preparation method and application of nitrogen-containing porous carbon material based on polyaspartic acid salt
  • Preparation method and application of nitrogen-containing porous carbon material based on polyaspartic acid salt

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preparation example Construction

[0042] The present invention is based on the preparation method of the nitrogen-containing porous carbon material of polyaspartic acid salt, and it comprises the following steps:

[0043] Step 1: High temperature carbonization

[0044] Put the polyaspartic acid salt into a carbonization furnace and carbonize it under vacuum conditions. During the carbonization process, the protective gas is continuously introduced at a rate of 15-45mL / min, and the temperature is first raised from room temperature at a rate of 3-8°C / min to After 1.5~2.5 hours of heat preservation at 175℃~225℃, continue to heat up at a rate of 3~8℃ / min to 900±10℃ for 0.5~1.5 hours, and then slowly lower to room temperature to obtain a black nitrogen-containing carbon material;

[0045] Step 2: pickling

[0046] Soak in hydrochloric acid solution and ultrasonically clean for three times for half an hour each time to obtain a nitrogen-containing porous carbon material.

[0047] In the present invention, also inc...

Embodiment 1

[0070] Step 1: High temperature carbonization

[0071] Put potassium polyaspartate into a carbonization furnace to carbonize under vacuum conditions, and continuously feed N at a rate of 30mL / min during the carbonization process. 2 / Ar, first increase the temperature from room temperature to 200±5°C for 2 hours at a rate of 5°C / min, then continue to heat at a rate of 5°C / min to 900±5°C for 1 hour, and then slowly lower to room temperature, that is, the black Nitrogen-containing carbon materials;

[0072] Step 2: pickling

[0073] Soak in 0.1 mol / L hydrochloric acid solution and ultrasonically clean for three times for half an hour each time to obtain a nitrogen-containing porous carbon material.

[0074] The parameters of the prepared nitrogen-containing porous carbon material are as follows: the specific surface area is 1550 m 2 / g, pore volume 1.2 cm 3 / g, the yield is 15%. When the current density is 1A / g, the specific capacitance value is 161F / g, and after 1000 cycles...

Embodiment 2

[0076] Step 1: High temperature carbonization

[0077] Put sodium polyaspartate into a carbonization furnace and carbonize under vacuum conditions, and continuously feed N at a rate of 30mL / min during the carbonization process. 2 / Ar, first increase the temperature from room temperature to 200±5°C for 2 hours at a rate of 5°C / min, then continue to heat at a rate of 5°C / min to 900±5°C for 1 hour, and then slowly lower to room temperature, that is, the black Nitrogen-containing carbon materials;

[0078] Step 2: pickling

[0079] Soak in 0.1 mol / L hydrochloric acid solution and ultrasonically clean for three times for half an hour each time to obtain a nitrogen-containing porous carbon material.

[0080] The parameters of the prepared nitrogen-containing porous carbon material are as follows: the specific surface area is 1152 m 2 / g, pore volume 0.8 cm 3 / g, the yield is 13%. When the current density is 1A / g, the specific capacitance value is 155F / g, and after 1000 cycles, ...

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Abstract

The invention relates to a preparation method and application of a nitrogen-containing porous carbon material based on polyaspartic acid salt, belonging to the field of carbon materials. The polyaspartic acid salt is firstly put into a carbonization furnace to be carbonized under a vacuumizing condition to prepare a black nitrogen-containing carbon material, and the nitrogen-containing porous carbon material is obtained by pickling. The nitrogen-containing porous carbon material obtained by the method has large specific surface area, more uniform distribution of nitrogen atoms and pore diameters, and better electrical properties.

Description

technical field [0001] The invention belongs to the field of carbon materials, and in particular relates to a preparation method and application of a nitrogen-containing porous carbon material based on polyaspartate. Background technique [0002] At present, carbon materials are widely used in the fields of adsorbents, catalysts, fuel cells, electrode materials for secondary batteries, supercapacitors, composite materials, gas sensors, solar cells, and various electronic devices due to their excellent porous properties. Compared with ordinary carbon materials, nitrogen-containing carbon materials have more active sites, and their performance is more excellent. 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 nanostructure of carbon materials, they can effectively modulate their morphology, structure and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/05H01G11/24H01G11/32H01G11/34H01G11/44
CPCC01B32/05H01G11/24H01G11/32H01G11/34H01G11/44Y02E60/13
Inventor 王莎莎刘振法张利辉许跃龙
Owner ENERGY RESOURCES INST HEBEI ACADEMY OF SCI
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