Preparation method of carbon-silicon compound aerogel

A composite airgel and silica sol technology, which is applied in the preparation of microspheres and microcapsule preparations, can solve the problems of destroying the pore structure and distribution of airgel, reducing the specific surface area and pore volume, and collapsing the gel network structure. Achieve the effect of preventing network collapse, preventing volume shrinkage, and low density

Inactive Publication Date: 2008-10-22
EAST CHINA UNIV OF SCI & TECH
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Problems solved by technology

[0003] However, in the process of synthesis, there is such a problem: due to the existence of capillary tension, the structure of the gel network will collapse when it is dried, destroying the pore structure and distribution of the airgel, and shrinkage will also occur during the carbonization process. , leading to a decrease in specific surface area and pore volume

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  • Preparation method of carbon-silicon compound aerogel
  • Preparation method of carbon-silicon compound aerogel

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Experimental program
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Effect test

Embodiment 1

[0019] (1) Mix resorcinol, formaldehyde, and silica sol No. 1 in a molar ratio of 1:2:2, R / C=500, and mix them into an aqueous solution with a solid content of 35g / 100ml, then put it into an ampoule and seal it , aged in a water bath at 85°C for 4 days to obtain a hydrogel.

[0020] (2) Replace the hydrogel with absolute ethanol to make it an organic aerogel, and dry it in a mixed solution of ethanol and petroleum ether at 250° C. and 9 MPa for 4 hours in a supercritical state to obtain a dried organic aerogel.

[0021] (3) The organic airgel was carbonized at 800° C. for 3 h in a carbonization furnace under the protection of nitrogen to obtain a carbon-silicon composite airgel.

[0022] The true density of the prepared composite gel is 0.55g / m 3 , BET specific surface area is 405m 2 / g, the pore volume is 2.01cm 3 / g.

Embodiment 2

[0024] (1) Mix resorcinol, formaldehyde, and silica sol No. 2 in a molar ratio of 1:2:2, R / C=500, mix and prepare an aqueous solution with a solid content of 35g / 100ml, and then put it into an ampoule and seal it , aged in a water bath at 85°C for 4 days to obtain a hydrogel.

[0025] (2) Replace the hydrogel with absolute ethanol to make it an organic aerogel, and dry it in a mixed solution of ethanol and petroleum ether at 250° C. and 9 MPa for 4 hours in a supercritical state to obtain a dried organic aerogel.

[0026] (3) The organic airgel was carbonized at 800° C. for 3 h in a carbonization furnace under the protection of nitrogen to obtain a carbon-silicon composite airgel.

[0027] The true density of the composite gel is 0.54g / m 3 , BET specific surface area is 420m 2 / g, the pore volume is 1.97cm 3 / g.

Embodiment 3

[0029] (1) Mix resorcinol, formaldehyde, and silica sol No. 1 in a molar ratio of 1:2:3, R / C=500, mix and prepare an aqueous solution with a solid content of 40g / 100ml, and then put it into an ampoule and seal it , aged in a water bath at 85°C for 4 days to obtain a hydrogel.

[0030] (2) Replace the hydrogel with absolute ethanol to make it an organic aerogel, and dry it in a mixed solution of ethanol and petroleum ether at 250° C. and 9 MPa for 4 hours in a supercritical state to obtain a dried organic aerogel.

[0031] (3) The organic airgel was carbonized at 800° C. for 3 h in a carbonization furnace under the protection of nitrogen to obtain a carbon-silicon composite airgel.

[0032] The true density of the composite gel is 0.53g / m 3 , BET specific surface area is 354m 2 / g, the pore volume is 1.92cm 3 / g.

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Abstract

The invention relates to a preparation method for carbon-silicon composite aerogel with low density, high ratio surface area and high pore volume. The method takes silicone gel grains as a framework structure, takes resorcinol and formaldehyde as reactant and prepares the hydrogels by the sol-gel reaction under the catalysis of alkaline catalyst. After the hydrogels are dried, high-temperature carbonization is carried out on the hydrogels under the protection of inert gases, so as to gain the carbon-silicon composite aerogel. The carbon-silicon composite aerogel prepared by the method of the invention has the characteristics of high ratio surface area, large pore volume and low density.

Description

technical field [0001] The invention relates to a preparation method of carbon-silicon composite airgel, in particular to a method for preparing carbon-silicon composite airgel by forming a network skeleton structure of silica gel particles in the process of sol-gel synthesis of airgel Methods. Background technique [0002] In the late 1980s, Pekala R.W. of Lawrence Livermore National Laboratory in the United States first prepared RF (resorcinol formaldehyde) organic airgel, and carbonized it to obtain carbon aerogel. Carbon airgel is a new type of porous nanomaterial aerogel, which is a kind of nanoporous amorphous carbon material with controllable structure. The diameter of colloidal network particles is 3nm-20nm, the porosity is as high as 80%-98%, the typical pore size is less than 50nm, and the specific surface area is as high as 600m 2 / g~1000m 2 / g. Due to its high specific surface area, wide range of density variation, and adjustable structure, carbon aerogels ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/14
Inventor 张睿陈亮龙东辉卢丰凌立成
Owner EAST CHINA UNIV OF SCI & TECH
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