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Application and preparation method of biomass-based nitrogen-doped porous carbon

A nitrogen-doped porous carbon and biomass technology, applied in the direction of carbon preparation/purification, chemical instruments and methods, alkali metal compounds, etc., can solve problems that are not suitable for large-scale production and industrial applications, complex preparation processes, and expensive precursors and other problems, to achieve high adsorption capacity, simple process, and reduce costs

Inactive Publication Date: 2017-05-10
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0040] In summary, in the prior art reported in the literature, some preparation processes are complicated, for example, hydrofluoric acid is required to remove the silica template; the carbon and nitrogen sources (ethylenediamine) used in some methods are toxic; some methods The precursors used are relatively expensive; some methods have complex preparation processes, such as ammonification treatment in the later stage, which consumes time, energy, and high cost, and is not suitable for large-scale production and industrial applications.

Method used

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  • Application and preparation method of biomass-based nitrogen-doped porous carbon
  • Application and preparation method of biomass-based nitrogen-doped porous carbon
  • Application and preparation method of biomass-based nitrogen-doped porous carbon

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Embodiment 1

[0066] a. Dissolve 5g of sodium hydroxide in 50ml of water and stir to dissolve, add 15g of urea and stir to dissolve, at a temperature of 10°C, add 5g of cellulose carbamate, and mechanically stir vigorously for 12min to obtain a uniform cellulose carbamate / Urea / sodium hydroxide sol solution, and then put the sol solution in an evaporating dish, spread it flat, and dry it at a temperature of 80°C for 5 hours to obtain a sol;

[0067]b. Under the protection of nitrogen, put the dried sol in step a into a tube furnace for calcination, raise the temperature to 550°C at a rate of 5°C / min, keep it for 1h, then raise the temperature to 700°C, and keep it for 1h. A black solid was obtained, and then the black solid was washed with water and 10 wt % hydrochloric acid until neutral, and dried at 120° C. for 4 hours to obtain biomass-based nitrogen-doped porous carbon.

Embodiment 2

[0069] a. Dissolve 5g of sodium hydroxide in 50ml of water and stir to dissolve, add 15g of urea and stir to dissolve, at a temperature of 8°C, add 5g of cellulose carbamate, and mechanically stir vigorously for 10min to obtain a uniform cellulose carbamate / Urea / sodium hydroxide sol solution, and then put the sol solution in an evaporating dish, spread it flat, and dry it at a temperature of 60°C for 6 hours to obtain a sol;

[0070] b. Under the protection of nitrogen, place the dried sol in step a for calcination in a tube furnace, raise the temperature to 550°C at a rate of 5°C / min, keep it for 1h, then raise the temperature to 800°C, and keep it for 1h. A black solid was obtained, and then the black solid was washed with water and 10 wt % hydrochloric acid until neutral, and dried at 120° C. for 4 hours to obtain biomass-based nitrogen-doped porous carbon.

Embodiment 3

[0072] a. Dissolve 5g of sodium hydroxide in 50ml of water and stir to dissolve, add 15g of urea and stir to dissolve, at a temperature of 15°C, add 5g of cellulose carbamate, and mechanically stir vigorously for 15min to obtain a uniform cellulose carbamate / Urea / sodium hydroxide sol solution, and then put the sol solution in a 50ml beaker, spread it flat, and dry it at a temperature of 70°C for 9 hours to obtain a sol;

[0073] b. Under the protection of nitrogen, place the dried sol in step a for calcination in a tube furnace, raise the temperature to 550°C at a rate of 5°C / min, keep it for 1h, then raise the temperature to 900°C, and keep it for 1h. A black solid was obtained, and then the black solid was washed with water and 10 wt % hydrochloric acid until neutral, and dried at 120° C. for 4 hours to obtain biomass-based nitrogen-doped porous carbon.

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Abstract

The invention discloses application and a preparation method of biomass-based nitrogen-doped porous carbon. The method includes: taking cheap cellulose carbamate as a raw material and urea as a nitrogen source, well mixing with sodium hydroxide solution, drying to form sol, and performing high-temperature calcination to obtain the porous-structure biomass-based nitrogen-doped porous carbon high in specific surface area and pore volume. According to electron microscopy images, the prepared material is in a three-dimensional inner-crosslinked porous structure; according to XPS and elemental analysis, nitrogen is successfully doped into a carbon substrate, the nitrogen content is 7.7-15.5%, and the specific surface area is 700-3700m<2> / g; according to supercapacitor experiments, the biomass-based nitrogen-doped porous carbon is great in electrochemical performance; according to pollutant adsorption experimental data, the material is high in adsorption rate and adsorption capacity in adsorption of dye pollutant methylene blue, and the adsorption capacity reaches 1520mg / g. The method is simple in preparation, the raw materials are renewable, and low cost is realized. In addition, sodium carbonate which is a by-product is obtained by washing of calcined samples, so that cost can be effectively reduced, and economic benefits are increased.

Description

technical field [0001] The invention relates to a preparation method of biomass-based nitrogen-doped porous carbon, which belongs to the field of nanometer materials, and relates to the preparation of a biomass-based nitrogen-doped porous carbon material and its application for electrochemical materials and dye adsorption. Background technique [0002] Porous carbon materials have the characteristics of high specific surface area, porosity, adjustable pore size, and excellent chemical stability, so they are widely used in the fields of adsorption, catalysis, separation, and energy storage. Nitrogen-doped porous carbon increases the electron density at the Fermi level due to the doping of nitrogen atoms, and at the same time reduces the position of the valence band, improving the oxidation stability and conductivity of the material. The surface structure of the material is changed, the basic sites on the surface of the material are increased, and its hydrophilicity is enhance...

Claims

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Application Information

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IPC IPC(8): C01B32/05C01D7/00H01G11/86H01G11/38H01G11/44H01G11/32
CPCY02E60/13C01D7/00C01P2002/72C01P2002/80C01P2002/85C01P2006/12C01P2006/14H01G11/32H01G11/38H01G11/44H01G11/86
Inventor 张亚刚周鑫王朋磊徐鲁张乐涛王璐璐郅柯柯张岚姜莹芳
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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