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Method for preparing organic aerogel and carbon aerogel by using normal pressure exsiccation

A carbon aerogel and organogel technology, which is applied in the field of preparing organic aerogel and carbon aerogel, can solve the problems of demanding replacement, expensive, shortened preparation cycle, etc., and achieve low equipment requirements and simple preparation process Effect

Inactive Publication Date: 2004-03-10
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, CO 2 Supercritical drying is the most typical, but the preparation cycle is time-consuming due to the lengthy solvent exchange required by this method; subsequently, supercritical drying with organic solvents such as acetone [10] and isopropanol [11] has been proposed. Shorten the preparation cycle to some extent
However, the airgel products obtained by supercritical drying are extremely expensive. Therefore, it was proposed to replace the solvent with high surface tension with a solvent with low surface tension to achieve normal pressure drying of organogels [12]. However, Solvent replacement also has the disadvantage of a long preparation cycle, and the method is demanding on the degree of replacement, which greatly increases the difficulty of preparing bulk aerogels

Method used

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  • Method for preparing organic aerogel and carbon aerogel by using normal pressure exsiccation
  • Method for preparing organic aerogel and carbon aerogel by using normal pressure exsiccation
  • Method for preparing organic aerogel and carbon aerogel by using normal pressure exsiccation

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Embodiment 1

[0016] Embodiment 1: According to R / F=0.5, R / H=25, R / I=0.1g·cm -3 (R / I represents the mass ratio of resorcinol to the volume of isopropanol), 0.0509 gram of hexamethylenetetramine is dissolved in 10 ml of isopropanol, 1 gram of resorcinol is dissolved in 1.5 ml In the furfural, then the two solutions were mixed and stirred evenly, then poured into an ampoule bottle and sealed, and reacted at 75°C for 7 days to obtain an organic gel; then dried at 60°C for 10 hours to obtain an organic aerogel ; Afterwards, place the organic airgel in a desktop carbonization furnace, raise the temperature from room temperature to 900°C at a heating rate of 5°C / min under the protection of high-purity nitrogen, carbonize at a constant temperature for 180 minutes, cool down naturally, and take out the charcoal to condense glue. The measured density of organic airgel is 0.226g cm -3 , with a theoretical density of 0.226g cm -3 Very close; the density of carbon airgel is 0.244g cm -3 ; The BET s...

Embodiment 2

[0017] Embodiment 2: According to R / F=0.5, R / H=45, R / I=0.1g·cm -3 , 0.0283 g of hexamethylenetetramine was dissolved in 10 ml of isopropanol, 1 g of resorcinol was dissolved in 1.5 ml of furfural, the two solutions were mixed and stirred well, and poured into ampoules neutralized and sealed, reacted at 75°C for 7 days to obtain an organic gel; then dried naturally for 3 days and dried at 85°C for about 2 hours (or directly dried at 60°C for 10 hours) to obtain an organic aerogel; after that , put the organic aerogel in a bench-top carbonization furnace, raise the temperature from room temperature to 900°C at a heating rate of 5°C / min under the protection of high-purity nitrogen, carbonize at a constant temperature for 180 minutes, cool down naturally, and take out the carbon aerogel. The measured density of organic airgel is 0.239g cm -3 , with a theoretical density of 0.225g cm -3 Close; the density of carbon airgel is 0.282g cm -3 ; The BET specific surface area of ​​carb...

Embodiment 3

[0018] Embodiment 3: According to R / F=0.5, R / H=50, R / I=0.072g*cm -3 , 0.0254 g of hexamethylenetetramine was dissolved in 13.96 ml of isopropanol, 1 g of resorcinol was dissolved in 1.5 ml of furfural, the two solutions were mixed and stirred well, and then poured into an ampoule and seal it, and react at 75°C for 7 days to obtain an organic gel; then directly dry at 60°C for 10 hours to obtain an organic aerogel; after that, place the organic aerogel in a table-top carbonization furnace, The temperature was raised from room temperature to 900°C at a heating rate of 5°C / min under the protection of 100°C, carbonized at a constant temperature for 180 minutes, cooled naturally, and the carbon airgel was taken out. The measured density of the organic airgel is 0.238g cm -3 , with a theoretical density of 0.169g cm -3 Close; the density of carbon airgel is 0.223g cm -3 .

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Abstract

A process for preparing the organic aerogel and carbon aerogel by ordinary-pressure drying method includes reaction between resorcin and furaldehyde, in which the hexamethylene tetraamine is used as catalyst and organic reagent (isopropanol) is used as solvent, thermal setting to obtain organic gel, drying or baking to obtain organic aerogel, and charring in inertial gas to obtain carbon aerogel.

Description

technical field [0001] The invention relates to a method for preparing organic airgel and carbon airgel by normal pressure drying method. technical background [0002] In the late 1980s, PekalaR.W. of Lawrance Livermore National Laboratory in the United States prepared RF (resorcinolformaldehyde) organic airgel for the first time, and carbonized it to obtain carbon aerogel. Carbon airgel is a lightweight nanoporous material made up of spherical nanoparticles connected to each other. Its porosity is as high as 80-98%, and the typical pore size is less than 50nm. Generally, the diameter of network particles is about 3-20nm, and the specific surface area Up to 600~1100m 2 g -1 , the density is 0.05~0.80g / cm 3 . Due to this unique nano-network structure, carbon aerogels and their organic aerogel precursors are widely used in Cerenkov detectors, acoustic impedance coupling materials, catalysts and catalyst supports, gas filter materials, and high-efficiency heat insulation ma...

Claims

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Application Information

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IPC IPC(8): C01B31/02
Inventor 符若文吴丁财
Owner SUN YAT SEN UNIV
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