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Nitrogen-doped porous carbon material and preparation method thereof

A nitrogen-doped porous carbon and Lewis acid technology, which is applied in the preparation/purification of carbon, chemical instruments and methods, electrolytic capacitors, etc., can solve the problems of expensive equipment, small sample volume, high production cost, etc., and achieve abundant raw material resources , Strong reproductive ability, easy to operate

Inactive Publication Date: 2012-07-18
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The on-site doping method refers to the use of nitrogen-containing organic small molecules for vapor deposition and growth to obtain nitrogen-doped carbon materials. This preparation method requires expensive instruments and equipment, and the amount of prepared samples is small, which can only meet scientific The needs of research cannot meet the industrial production of large-scale membranes
The post-activation method refers to the post-functionalization of the prepared carbon material in the activation gas containing nitrogen. However, this activation process usually needs to be completed at a higher temperature, so production energy consumption and safety factors are constraints. Two important issues for development
The direct carbonization method refers to the direct carbonization of nitrogen-containing organic small molecules or polymers under the action of templates. This method usually requires the use of pure chemical reagents, so the production cost is high and has a serious impact on the environment.
In addition, the preparation and removal of templates described in the direct carbonization method further complicates the carbonization process.

Method used

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  • Nitrogen-doped porous carbon material and preparation method thereof
  • Nitrogen-doped porous carbon material and preparation method thereof
  • Nitrogen-doped porous carbon material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 2mg of Bacillus subtilis and inoculate it into 50mL of culture medium, cultivate it with shaking at 36°C until the cell growth enters the logarithmic phase, collect the bacteria by centrifugation, and freeze-dry them for later use; the formula of the culture medium is: 1L distilled water, 20g glucose, 15g Peptone, 5g sodium chloride and 0.5g beef extract.

[0029] After mixing the lyophilized Bacillus subtilis cells and zinc chloride at a mass ratio of 1:4, transfer them to a high-temperature furnace, and treat them at 800°C for 4 hours under the protection of nitrogen, and wash them with 0.1M dilute hydrochloric acid solution to pH after cooling. The value is 6-7, and it can be obtained after drying.

[0030] The physical and chemical properties of the obtained nitrogen-doped porous carbon material were characterized by scanning electron microscopy, elemental analyzer, etc. See figure 1 and figure 2 , the oxygen reduction electrocatalysis test and supercapacit...

Embodiment 2

[0033] Weigh 2mg of Bacillus subtilis and inoculate it into 50mL of culture medium, cultivate it with shaking at 36°C until the cell growth enters the logarithmic phase, collect the bacteria by centrifugation, and freeze-dry them for later use; the formula of the culture medium is: 1L distilled water, 20g glucose, 15g Peptone, 5g sodium chloride and 0.5g beef extract.

[0034]After mixing the lyophilized Bacillus subtilis and zinc chloride at a mass ratio of 2:1, transfer it to a high-temperature furnace, and treat it at 500°C for 4 hours under the protection of nitrogen, and wash it with 0.1M dilute hydrochloric acid solution to pH after cooling. The value is 6-7, and it can be obtained after drying.

[0035] The specific surface area of ​​nitrogen-doped porous carbon material obtained by nitrogen adsorption and desorption analysis and elemental analyzer is 687m 2 g -1 , the pore size is mainly micropores less than 2nm; elemental analysis mass percent is carbon 78.1%, oxyge...

Embodiment 3

[0037] Weigh 2mg of Bacillus subtilis and inoculate it into 50mL of culture medium, cultivate it with shaking at 36°C until the cell growth enters the logarithmic phase, collect the bacteria by centrifugation, and freeze-dry them for later use; the formula of the culture medium is: 1L distilled water, 20g glucose, 15g Peptone, 5g sodium chloride and 0.5g beef extract.

[0038] After mixing the freeze-dried Bacillus subtilis and zinc chloride at a mass ratio of 1:1, transfer it to a high-temperature furnace, treat it at 800°C for 20 hours under nitrogen protection, and wash it with 0.1M dilute nitric acid solution to pH after cooling. The value is 6-7, and it can be obtained after drying.

[0039] The specific surface area of ​​nitrogen-doped porous carbon material obtained by nitrogen adsorption and desorption analysis and elemental analyzer is 756m 2 g -1 , the pore size is mainly micropores; elemental analysis mass percent is carbon 90.3%, oxygen 4.7%, nitrogen 4.0%. The ...

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Abstract

The invention belongs to the field of organic nanometer materials and the electrochemistry and discloses a nitrogen-doped porous carbon material and a preparation method thereof. The preparation method of the nitrogen-doped porous carbon material comprises the following steps of: taking a microorganism as a carbon precursor and mixing with Lewis acid to obtain the porous carbon material with rich nitrogen element and large specific surface area after ion thermal reaction. Compared with the prior art, the preparation method has the advantages that raw material resources are rich and are simply and easily obtained, the use of strong acid, strong alkali and other high-pollution chemical reagents is simultaneously avoided, the greenness and the environment friendliness are ensured, the operation is convenient, the energy consumption is low, and the preparation method is suitable for large-scale industrialized production. The nitrogen-doped porous carbon material prepared by adopting the preparation method has a rich pore structure, is larger in specific surface area and rich in nitrogen heteroatom, simultaneously has good electrocatalytic oxygen reduction capability and excellent charge storage capacity and can be used for the preparation of an electrocatalytic oxygen reduction electrode and a supercapacitor.

Description

technical field [0001] The invention belongs to the field of inorganic nanometer materials and electrochemistry, and in particular relates to a nitrogen-doped porous carbon material and a preparation method thereof. Background technique [0002] Due to their rich pore structure, large specific surface area, good chemical stability and excellent mechanical properties, porous carbon materials have attracted close attention and have been widely used in gas separation, water purification treatment, catalytic chromatography, energy storage And complex shapes, difficult to process engineering ceramics and other fields. Porous carbon materials mainly include activated carbon (AC), activated carbon fiber (ACF), carbon molecular sieve (CMS), and carbon nanotubes (CNTs), which were newly developed in the 1990s. In addition to the properties of ordinary porous carbon, functionalized porous carbon materials also have other more specific and special uses. Element doping is one of the c...

Claims

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Application Information

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IPC IPC(8): C01B31/02H01G9/042B01J21/18C01B32/05
CPCY02E60/13
Inventor 杨秀荣朱慧王小磊杨帆刘雪霞
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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