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

A technology of carbon aerogels and organic gels, which is applied in the field of preparing organic aerogels and carbon aerogels, can solve the problems of demanding replacement, high cost, and time-consuming preparation cycle, and achieves low equipment requirements and low preparation process simple effect

Inactive Publication Date: 2005-05-04
SUN YAT SEN UNIV
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  • 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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Experimental program
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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; carbon airgel has a density of 0.244 g cm -3 The BET spe...

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, Under the protection of the environment, the temperature was raised from room temperature to 900°C at a heating rate of 5°C / min, 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

The invention relates to a method for preparing organic airgel and carbon airgel by normal pressure drying method. In this method, resorcinol and furfural are used as reaction monomers, hexamethylenetetramine is used as a catalyst, organic reagents such as isopropanol are used as solvents, and organic gel is obtained by heating and curing; then, it is directly dried or heated under normal pressure. Organic aerogels are obtained by drying; afterward, charcoal aerogels with high specific surface area are obtained by carbonization in an inert atmosphere. The carbon airgel preparation process of the present invention avoids the complex process of the conventional supercritical drying method, the technology is simple, fast, and has low equipment requirements, and can realize the industrialized production of the carbon airgel.

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, Pekala R.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 m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/02
Inventor 符若文吴丁财
Owner SUN YAT SEN UNIV
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