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Preparation method of spherical charcoal-aero gel

A carbon aerogel and spherical technology, applied in the field of preparation of spherical carbon aerogel, can solve the problems of high price, poor sphericity, limited commercial application prospects, etc., and achieve the effect of shortening the synthesis process and broadening the application field.

Inactive Publication Date: 2007-09-26
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

Pekala et al first reported the preparation of resorcinol-formaldehyde spherical organic aerogels by inverse emulsion sol-gel polymerization in the mid-1990s (Alviso CT, Pekala RW, GrossJ, Lu X, Caps R, Fricke J.Resorcinol-formaldehyde and carbon aerogel microspheres.Mater ResSoc Symp Proc 1996; 431:521-525.), but this method uses relatively expensive resorcinol as a raw material, which limits its commercial application prospects
US.Pat.No 4997804 discloses a method for preparing organic airgel and carbon airgel microspheres by polymer cross-linking molding method, but this method only prepares microspheres with smaller diameters and poor sphericity

Method used

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  • Preparation method of spherical charcoal-aero gel
  • Preparation method of spherical charcoal-aero gel
  • Preparation method of spherical charcoal-aero gel

Examples

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preparation example Construction

[0022] Synthetic method of the present invention comprises the steps:

[0023] (1) Mix the various components constituting the organogel to form a sol monomer, and perform pre-polymerization at an appropriate temperature for 0-10 hours.

[0024] (2) Prepare an organic solvent containing a certain concentration of surfactant. Add 10 to 50 times the volume of the sol volume of the organic solvent into the reactor, raise the temperature to 60°C to 85°C, stir at a speed of 50 to 400 rpm, add an appropriate volume of sol after prepolymerization, and stir at a constant temperature and speed 3~24h. The spherical hydrogel can be obtained by further aging at room temperature to 85°C.

[0025] (3) replacing the water in the hydrogel with an organic solvent to obtain an organogel.

[0026] (4) Put the organogel in an autoclave and fill it with petroleum ether, and dry it under supercritical conditions at 240-300°C and 4.5-12Mpa for 1-3 hours, or use carbon dioxide as the drying medium...

Embodiment 1

[0034] Mix phenol, melamine and formaldehyde in a molar ratio of 1:0.4:3, add catalyst NaOH with 1% of the total mass of the reactant, then add a certain amount of deionized water to make the total concentration of the reactant 18g / 100ml, and react at 85°C for 5 Hours. Then 20 ml of the reaction solution was poured into 500 ml of cyclohexane containing 0.1 ml of Span80, and stirred at 67° C. at a stirring speed of 400 rpm for 4 h. Continue heating for 72 hours after stopping stirring, and centrifuge to obtain hydrogel balls. Acetone was used to replace the water in the gel to obtain a spherical ketone gel. Put the ketone gel in an autoclave and fill it with petroleum ether, raise the temperature to 250°C, and keep the pressure in the autoclave at 8Mpa, supercritically dry for 3 hours, then slowly release the pressure at a constant temperature and cool naturally to obtain a spherical organic aerogel; Put the obtained airgel into a high-temperature cracking furnace, raise the ...

Embodiment 2

[0036] Mix phenol, melamine and formaldehyde in a molar ratio of 1:0.2:3, add catalyst NaOH with 1% of the total mass of the reactant, then add a certain amount of deionized water to make the total concentration of the reactant 18g / 100ml, and react at 85°C for 5 Hours. Then 20 ml of the reaction solution was poured into 500 ml of cyclohexane containing 0.1 ml of Span80, and stirred at 67° C. at a stirring speed of 400 rpm for 4 h. Continue heating for 72 hours after stopping stirring, and centrifuge to obtain hydrogel balls. Acetone was used to replace the water in the gel to obtain a spherical ketone gel. Put the ketone gel in an autoclave and fill it with petroleum ether, raise the temperature to 250°C, and keep the pressure in the autoclave at 8Mpa, supercritically dry for 3 hours, then slowly release the pressure at a constant temperature and cool naturally to obtain a spherical organic aerogel; Put the obtained airgel into a high-temperature cracking furnace, raise the ...

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Abstract

The invention discloses a preparing method of globular char gas gel, which comprises the following steps: making phenol- melamine-formaldehyde or water soluble phenol resin- melamine-formaldehyde as raw material; forming colloidal sols through pre-polymerization; adding into discontinuous phase with surface activator; forming floating system under the function of stirring; generating colloidal sols- gel transition at 60-85 deg.c; forming globular aquagel; proceeding organic solvent replace and hypercritical dry; getting organic aerogel; proceeding high temperature degradation; getting globular char gas gel; setting the specific surface area at 400-1000m2 / g, bore diameter at 3-20 nanometer and ball calipers at 0.01-3 millimeter.

Description

technical field [0001] The invention relates to a method for preparing spherical carbon airgel. Background technique [0002] Carbon aerogel is a carbonaceous porous material rich in mesoporous nanostructures. It has good electrical conductivity, biocompatibility, corrosion resistance, high specific strength, radiation resistance and low density. It is used in electronics, military, It has broad application prospects in the fields of medicine, environmental protection and chemical industry. [0003] Most of the existing carbon aerogels are in the form of a single block, which mainly has defects such as extremely poor elasticity and unsuitable processing. This limits the application of carbon aerogels in some aspects (such as fixed bed adsorption, catalyst support and medical support, etc.). Therefore, how to change the morphology of the existing carbon aerogels becomes a technical problem to be solved in the present invention. Pekala et al first reported the preparation o...

Claims

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Application Information

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IPC IPC(8): C01B31/02B82B3/00
Inventor 张睿张洁龙东辉詹亮梁晓怿凌立成
Owner EAST CHINA UNIV OF SCI & TECH
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