Rapid preparation method for aerogel material

An aerogel and gel method technology, which is applied in the field of rapid preparation of aerogel materials, can solve the problems of low specific surface area, large shrinkage, and multi-media solvent of aerogel, so as to shorten the preparation period and save consumption. Effect

Active Publication Date: 2016-05-04
YANTAI ZHONGKE RES INST OF ADVANCED MATERIALS & GREEN CHEM ENG
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0003] Although the research on airgel has become a hot spot, there are still various problems in the preparation of airgel so far. For example, there are two methods of atmospheric pressure drying and supercritical drying in the preparation process of airgel. Atmospheric pressure drying requires a large amount of Solvents are used to continuously replace the solvent in the gel and the long aging and drying process sometimes takes dozens of days, and the prepared airgel generally has a low specific surface area, large pore size, and large shrinkage; supercritical drying generally requires The wet gel is aged before supercritical drying to increase the strength of the airgel skeleton, and then the wet gel is immersed in a supercritical medium and dried under the supercritical condition of the medium, although the prepared airgel has a relatively small specific surface area. High, small pore size, high porosity, but due to the aging process, it still takes several days to complete, and also requires more medium solvent

Method used

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  • Rapid preparation method for aerogel material
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  • Rapid preparation method for aerogel material

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Mix aluminum sec-butoxide, ethanol, and deionized water at a molar ratio of 1:16:0.6, stir at 60°C for 30 minutes to form a clear and transparent solution, cool to room temperature, add a mixed solution of methanol, deionized water, and acetic acid, and mix The amount of solution added is 4.92:016:0.45:1 according to the molar ratio of the three to aluminum sec-butoxide. After stirring for 10 minutes, pour the sol into the hydrothermal kettle, close the lid of the hydrothermal kettle tightly, and let it stand to form a gel. Finally, put it into a 2L autoclave, add 200ml of ethanol, then seal the autoclave, blow nitrogen into the autoclave to purge the air in the autoclave, then pressurize to 3MPa, and heat up to 260°C at 3°C / min. When the internal pressure reaches 12MPa, open the exhaust valve and start to release the pressure at a rate of 0.07MPa / min. After the pressure drops to 0, start to lower the temperature. After cooling, open the autoclave and hydrothermal kettle...

Embodiment 2

[0040]Mix aluminum isopropoxide, isopropanol, and deionized water at a molar ratio of 1:12:1.5, stir at 60°C for 40 minutes to form a clear and transparent solution, cool to room temperature, add a mixed solution of methanol, deionized water, and acetic acid , the amount of the mixed solution added is 4.92:016:0.45:1 according to the molar ratio of the three to aluminum isopropoxide. After stirring for 10 minutes, pour the sol into the hydrothermal kettle, close the lid and let it stand for gel formation, then put into a 2L autoclave, add 100ml of isopropanol, then seal the autoclave, feed nitrogen to purge the air in the autoclave, then pressurize to 5MPa, and heat up to 270°C at 5°C / min. When the pressure reaches 13.5MPa, open the exhaust valve and start to release the pressure at a rate of 0.2MPa / min. After the pressure drops to 0, start to lower the temperature. After cooling, open the autoclave and hydrothermal kettle to obtain alumina with no shrinkage and good formabilit...

Embodiment 3

[0042] Mix aluminum nitrate, isopropanol, and deionized water at a molar ratio of 1:8:0.4, and stir at 60°C for 40 minutes to form a clear and transparent solution. After cooling to room temperature, add a mixed solution of methanol, deionized water, and acetic acid. The amount of the mixed solution to be added is 4.92:016:0.45:1 according to the molar ratio of the three to aluminum nitrate. After stirring for 10 minutes, pour the sol into the hydrothermal kettle, close the lid tightly and wait for the gel to form, then put it into a 2L autoclave , add 400ml of isopropanol, then seal the autoclave, blow nitrogen to purge the air in the autoclave, then pressurize to 2MPa, raise the temperature to 270°C at 5°C / min, at this time, the pressure in the autoclave reaches 9MPa, open The exhaust valve starts to release the pressure at a rate of 0.14MPa / min. After the pressure drops to 0, the temperature starts to drop. After cooling, the autoclave and the hydrothermal kettle are opened ...

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Abstract

The invention discloses a rapid preparation method for an aerogel material. The preparation method is a combination of a sol-gel method and a supercritical drying process. According to the invention, wet gel is formed through the sol-gel method at first and is directly put into a container for sealing without ageing; then the sealed container is put into a supercritical drying device and a supercritical medium solvent is added; and the supercritical drying process is carried out so as to prepare the aerogel material. Compared with the prior art, the preparation method provided by the invention has the following advantages: the ageing procedure in general aerogel preparation is eliminated, so the preparation period for the aerogel material is greatly shortened; and the wet gel does not need to soak in the medium solvent, so the consumption of the medium solvent in preparation is reduced. The aerogel prepared by using the method has an intact skeleton structure and a non-shrink volume.

Description

technical field [0001] The invention relates to a rapid preparation method of an airgel material. The method adopts a sol-gel method combined with a supercritical drying process to rapidly prepare the airgel. Background technique [0002] Airgel is a solid amorphous material with a nanoporous network structure formed by the aggregation of colloidal particles. It has an extremely low density and is known as "solid smoke". Airgel also has high porosity, high specific surface area, low thermal conductivity, low dielectric coefficient, low refractive index, low elastic modulus, low acoustic impedance, strong adsorption, etc., and its performance can be continuous with the control of the structure. Adjustability. The excellent performance of airgel makes it have very broad application prospects in the fields of thermal insulation, catalysis, energy conservation and environmental protection, petrochemical industry, and aerospace. [0003] Although the research on aerogels has be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/00C01B33/16C01B33/158C01F7/44
CPCB01J13/0091C01B33/1585C01B33/163C01F7/44
Inventor 杨景锋王齐华王廷梅梁永民
Owner YANTAI ZHONGKE RES INST OF ADVANCED MATERIALS & GREEN CHEM ENG
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