A kind of preparation method of ultra-high specific surface area carbon aerogel material

A technology of ultra-high specific surface area and carbon airgel, which is applied in the fields of airgel preparation, carbon preparation/purification, chemical instruments and methods, etc. It can solve the problems of uneven bleaching and lye treatment, high reaction temperature, and porosity Low-level problems, to achieve the effect of economical and easy realization of equipment and preparation process, simple preparation process, and increase of carboxyl density

Active Publication Date: 2022-07-19
NANKAI UNIV
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation process uses an organic solvent as the reaction medium, the reaction temperature is high, the steps are complicated, and it takes a long time
Zhang Tao of Jiangsu University and others used the cellulose in agricultural waste such as corn husks and cotton straw husks to obtain cellulose extracts after being washed with relatively simple ethanol and deionized water, and then treated with lye, and then bleached with acetic acid and sodium hypochlorite. 1. After washing and purifying, freeze-dry for 35 hours, and finally carbonize in a tube furnace to obtain the corresponding cellulose carbon airgel. Although this method is relatively simple, the agricultural waste particles in the preparation process are large, and the bleaching and lye treatment are not uniform, so it is difficult to Ensure the chemical properties and structural homogeneity of the final product carbon airgel, and its maximum surface area is only 675.8m 2 / g
Lu Yun of the Chinese Academy of Forestry Sciences also used the TEPMPO oxidation method to modify cellulose nanocrystals, but the degree of oxidation was not high, and the specific surface area of ​​the prepared carbon airgel was still relatively small, and the degree of porosity was low. The pretreatment and oxidation degree of cellulose nanocrystals may be the main limiting steps; at the same time, the higher price of cellulose nanocrystals makes the final carbon aerogel more costly
[0007] Therefore, the use of biomass fiber materials to prepare carbon aerogels has the characteristics of strong environmental friendliness, mild reaction conditions, low cost, and superior performance in catalysis, energy storage, and adsorption. The method of preparing carbon airgel from material fibers is relatively scarce

Method used

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  • A kind of preparation method of ultra-high specific surface area carbon aerogel material
  • A kind of preparation method of ultra-high specific surface area carbon aerogel material
  • A kind of preparation method of ultra-high specific surface area carbon aerogel material

Examples

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Embodiment 1

[0041] Step 1. Wet ball ground wood pulp and other biomass fibers

[0042](1) Take 15.0 g of dry biomass fibers such as wood pulp and disperse in 150 ml of distilled water to prepare a biomass fiber suspension such as wood pulp.

[0043] (2) Pour the above suspension into a 500ml agate ball mill jar, and add 100g agate balls to the agate jar at the same time.

[0044] (3) The agate jar is placed in a planetary ball mill, and the ball is milled for 3 hours at a speed of 200 r / min, respectively.

[0045] Step 2. TEMPO oxidation of wood pulp and other biomass fibers after ball milling

[0046] (1) Take an appropriate amount of the ball-milled suspension in step 1, add 100 ml of a mixed aqueous solution containing 0.1 g of sodium bromide and 0.01 g of 2,2,6,6-tetramethylpiperidine oxide, stir and mix well, and then for the pre-oxidation system.

[0047] (2) 100 ml of sodium hypochlorite solution with active chlorine content greater than 9% is added into dilute hydrochloric acid...

Embodiment 2

[0055] Step 1. Wet Ball Milling Newspaper Fiber Material

[0056] (1) Take 25 g of dried newspaper fiber material, disperse in 150 ml of distilled water, and prepare a newspaper fiber suspension.

[0057] (2) Pour the above suspension into a 500ml agate ball mill jar, and add 150g agate balls to the agate jar at the same time.

[0058] (3) The agate jar is placed in a planetary ball mill, and the ball is milled for 4 hours at a speed of 250 r / min. After the ball milling, the ball milled balls and the suspension are separated for use.

[0059] Step 2. TEMPO Oxidation of Ball Milled Newspaper Fibers

[0060] (1) Take an appropriate amount of the ball-milled suspension in step 1 and add 150 ml of a mixed aqueous solution containing 0.1 g of sodium bromide and 0.01 g of 2,2,6,6-tetramethylpiperidine oxide, and stir and mix well. for the pre-oxidation system.

[0061] (2) 150ml of sodium hypochlorite solution with active chlorine content greater than 9% is added into dilute hydr...

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Abstract

The invention discloses a preparation method of a carbon aerogel material with ultra-high specific surface area. The method comprises four steps: wet ball milling of biomass fibers, TEMPO oxidation of the ball-milled biomass fibers, preparation of oxidized biomass fiber aerogels, Pyrolytic carbonization. The cellulose carbon aerogel prepared by the invention has a unique three-dimensional sheet-like stacking structure, which provides great potential for its application as a material such as a catalyst, an adsorbent and an electrode capacitor.

Description

technical field [0001] The invention relates to a preparation method of a gel material, in particular to a preparation method of a carbon aerogel material with an ultra-high specific surface area. Background technique [0002] Carbon aerogel is a new type of lightweight, porous, three-dimensional network-like amorphous carbonaceous material with a large specific surface area (400-1000 m 2 / g), low density, nanoscale continuous pores and amorphous structure. Such materials were first synthesized from resorcinol and formaldehyde by sol-gel method and further prepared by high temperature carbonization. At present, common carbon aerogel raw materials mainly include resorcinol and formaldehyde, melamine and formaldehyde, phenolic resin and furfural, linear polymer N-methylol acrylamide and resorcinol, etc., and the above precursors are large Some of them are more toxic compounds, which have certain environmental and health risks to the natural environment and researchers. [0...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/05B01J13/00
CPCC01B32/05B01J13/0091
Inventor 张鹏黄鹏孙红文王翠苹
Owner NANKAI UNIV
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