Preparation method of block high temperature resistant silicon-charcoal composite aerogel material

A technology of high temperature resistance and airgel, which is applied in the field of preparation of airgel materials, can solve the problems of poor airgel pore structure, large specific surface area, high strength, etc., and achieve reduced operation steps, low density, and high molding performance Good results

Active Publication Date: 2012-02-15
NANJING UNIV OF TECH
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  • Abstract
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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing block high temperature resistant silicon-carbon composite airgel in order to improve the deficiencies in the prior art. The airgel samples have the characteristics of low density, large specific surface area, large pore volume, high strength and high temperature resistance, which solves the shortcomings of poor airgel pore structure and low strength, and can process samples of various shapes according to requirements , which has positive practical significance for the realization of large-scale production and application of airgel thermal insulation materials

Method used

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  • Preparation method of block high temperature resistant silicon-charcoal composite aerogel material
  • Preparation method of block high temperature resistant silicon-charcoal composite aerogel material
  • Preparation method of block high temperature resistant silicon-charcoal composite aerogel material

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example 1

[0024] (1) The molar ratio of resorcinol, formaldehyde, 3-aminopropyltriethoxysilane and deionized water is 1: 2: 0.5: 10, and the mol ratio of resorcinol and sodium carbonate is 1: 500, using methanol as a solvent to form a reactant solution (resorcinol, formaldehyde and 3-aminopropyltriethoxysilane) with a mass concentration of 6%, and place the reactant solution in a 60°C oven at a constant temperature The reaction was carried out for 70 minutes to obtain a wet gel.

[0025] (2) After the wet gel was aged in a water bath at 75°C for 10 days, the solvent was replaced with methanol, and the methanol was replaced every 6 hours for a total of 6 replacements. The degassing rate was replaced for 6 hours, then the temperature was raised to 50°C, and at 15 MPa, the degassing rate was 10 liters / minute for 4 hours, and finally the pressure was released to balance with the external atmospheric pressure at a degassing rate of 1 liters / minute, and organic gas condensation was obtained. ...

example 2

[0029] (1) The molar ratio of resorcinol, formaldehyde, and 3-aminopropyl triethoxysilane is 1: 2: 0.5: 4, and the molar ratio of resorcinol and sodium hydroxide is 1: 300, with Ethanol was used as a solvent to prepare a reactant solution with a mass concentration of the reactant of 4%, and the reactant solution was placed in an oven at 60° C. for constant temperature reaction for 300 minutes to obtain a wet gel.

[0030] (2) After the wet gel was aged in a water bath at 60°C for 15 days, the solvent was replaced with acetone, and the acetone was replaced every 12 hours for a total of 3 replacements, and then carbon dioxide supercritical drying was carried out at 10MPa and 25°C at 20 liters / hour. The degassing rate of 1 minute was replaced for 4 hours, then the temperature was raised to 80 ° C, and at 15 MPa, the degassing rate was 5 liters / minute for 8 hours, and finally the pressure was released at a degassing rate of 1 liter / minute to balance with the external atmospheric pr...

example 3

[0034](1) The molar ratio of resorcinol, formaldehyde, and 3-aminopropyltriethoxysilane is 1:2:1:4, and the molar ratio of resorcinol and sodium carbonate is 1:1000, with ethanol Prepare a solution with a mass concentration of 10% of the reactant as a solvent, and place the reactant solution in an oven at 60°C for 80 minutes at a constant temperature to obtain a wet gel.

[0035] (2) After aging for 10 days in a water bath at 65°C, the wet gel was replaced with absolute ethanol, and the absolute ethanol was replaced every 6 hours for a total of 3 replacements, followed by supercritical carbon dioxide drying at 10MPa and 25°C Displace with a gas release rate of 10 liters / min for 12 hours, then raise the temperature to 60°C, under 10 MPa, replace with a gas release rate of 5 liters / min for 8 hours, and finally release the pressure at a gas release rate of 3 liters / min to balance with the external atmospheric pressure , to obtain organic aerogels.

[0036] (3) The organic airgel...

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Abstract

The invention a preparation method of a block high temperature (>=1000 DEG C) resistant silicon-charcoal composite aerogel material. According to the invention, reactants of resorcinol, formaldehyde, 3-amino propyl triethoxysilane, a hydrolysis agent of deionized water and a solvent of alcohols are prepared into wet gel through a one-step sol-gel reaction under effect of a basic catalyst. The wetgel is treated with ageing, solvent displacement, supercritical drying and high temperature heat treatment to obtain the block high temperature resistant silicon-charcoal composite aerogel. The preparation method of the invention has simple technology and good controllability. The silicon-charcoal composite aerogel prepared by the method of the invention overcomes defects of weak high temperature resistance and uneasy moulding due to low strength of aerogel; and the prepared aerogel can be used at a high temperature higher than 1000 DEG C for a long time and has characteristics of low density, large specific surface area, large pore volume, high strength and high temperature resistance.

Description

technical field [0001] The invention belongs to the field of preparation technology of airgel materials, and relates to a method for preparing block high temperature resistant silicon-carbon composite airgel materials; in particular, it relates to a one-step sol-gel method combined with a supercritical drying process and A heat treatment process prepares a block-shaped high-temperature-resistant (≥1000°C) silicon-carbon composite airgel. Background technique [0002] Airgel is a lightweight solid material with a nanoporous network structure. It has structural characteristics such as low density, high specific surface area, and high porosity. It has broad application prospects in adsorption, catalysis, and impedance coupling, especially in In terms of heat insulation, its structural characteristics make it have extremely low thermal conductivity, which has obvious advantages compared with traditional heat insulation materials. People call this airgel material with extremely l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B30/00
Inventor 沈晓冬孔勇崔升仲亚
Owner NANJING UNIV OF TECH
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