Method for preparing graphene crosslinked type organic aerogel and carbon aerogel by normal-pressure drying

A carbon aerogel, graphene technology, applied in carbon preparation/purification, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as high drying shrinkage rate, and achieve simplified operation process, not easy to shrink, simple and fast The effect of preparation

Inactive Publication Date: 2014-08-20
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few studies on the atmospheric pressure drying of organogels, which are mainly related to the high drying shrinkage caused by atmospheric pressure drying.

Method used

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  • Method for preparing graphene crosslinked type organic aerogel and carbon aerogel by normal-pressure drying
  • Method for preparing graphene crosslinked type organic aerogel and carbon aerogel by normal-pressure drying
  • Method for preparing graphene crosslinked type organic aerogel and carbon aerogel by normal-pressure drying

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Experimental program
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Effect test

Embodiment 1

[0019] Embodiment 1: Using phenol (P), formaldehyde (F) as reaction monomer, sodium hydroxide as catalyst (C), water as solvent, according to the ratio of P / F=0.33, P / C=20, dubbed solid A solution with a content of 30wt% was added with 2wt% graphene oxide as a crosslinking agent, mixed evenly, heated at 60°C for 60 minutes to obtain a graphene crosslinked organic hydrogel, and aged in a water bath at 85°C for 72h. Then the gel column was taken out and dried at 60° C. under normal pressure for 24 hours to form an organic aerogel. Put the organic airgel into a carbonization furnace, pass through the nitrogen protection, and carry out carbonization at a constant temperature of 900 ° C for 2 hours, and finally form a carbon aerogel. The specific surface area of ​​carbon airgel is 485m 2 / g, pore volume 0.72cm 3 / g, the carbonization shrinkage rate is 49.9%.

Embodiment 2

[0020] Embodiment 2: Using resorcinol (R) and formaldehyde (F) as the reaction monomer, sodium carbonate as the catalyst, and water as the solvent, according to the ratio of R / F=0.5, R / C=200, the solid content is formulated To a 5wt% solution, add 20wt% functionalized graphene oxide as a crosslinking agent and mix evenly, obtain a graphene crosslinked organic hydrogel at 20°C for 5 minutes, and put it in a 75°C water bath for aging for 7 days. Then the hydrogel column was taken out and dried under infrared light for 10 h to form an organic aerogel. Put the organic airgel into a carbonization furnace, pass through the nitrogen protection, and carry out carbonization at a constant temperature of 800 ° C for 1 hour, and finally form a carbon aerogel. The specific surface area of ​​carbon airgel is 382m 2 / g, pore volume 0.42cm 3 / g, the carbonization shrinkage rate is 61.9%.

Embodiment 3

[0021] Embodiment 3: Using resorcinol (R) and formaldehyde (F) as the reaction monomer, sodium carbonate as the catalyst, and ethanol as the solvent, according to the ratio of R / F=0.5, R / C=200, the solid content is formulated To a 40wt% solution, add 0.5wt% graphene oxide as a crosslinking agent and mix evenly, heat at 80°C for 180 minutes to obtain a graphene crosslinked organic hydrogel, and put it in an 80°C water bath for aging for 72h. Then the gel column was taken out and dried at room temperature under normal pressure for 48 hours, and then dried at 120° C. for 5 hours to form an organic airgel. Put the organic airgel into a carbonization furnace, pass through nitrogen protection, and carry out carbonization at a constant temperature of 1100 ° C for 2 hours, and finally form carbon aerogel. The specific surface area of ​​carbon airgel is 732m 2 / g, pore volume 1.03cm 3 / g, the average pore diameter is 5.2nm.

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Abstract

The invention relates to a method for preparing graphene crosslinked type organic aerogel and carbon aerogel by normal-pressure drying, which takes phenols (P), amines, aldehydes, catalyst and solvent as a reaction system and graphene substances containing active functional groups as a cross-linking agent. The method comprises the steps of: curing to obtain organogel, and then carrying out normal-pressure drying to obtain the organic aerogel; and carrying out pyrolysis on the organic aerogel in the inert atmosphere at the temperature of 500-1600 DEG C to obtain the graphene crosslinked type carbon aerogel. The preparation method of the organic aerogel and the carbon aerogel is simple and rapid in technology; the conventional supercritical drying technology is avoided, and the prepared novel organic aerogel and carbon aerogel materials taking graphene as framework have new performances and wide application prospect; and the industrial production of the carbon aerogel can be expected to be realized.

Description

technical field [0001] The invention relates to a method for preparing graphene cross-linked organic airgel and carbon airgel by drying under normal pressure. Background technique [0002] Airgel is a porous amorphous solid material composed of nano-scale colloidal particles or polymer molecules, and it is also the lightest condensed material among synthetic materials. Its unique open nanoporous structure and continuous three-dimensional network make it have extremely low density, high specific surface area and high porosity, showing strong adsorption and catalytic ability, low thermal conductivity, low acoustic impedance and low refractive index, etc. Therefore, airgel has become a good catalyst and its carrier, adsorbent and gas filter material, and has been successfully applied to Cherenkov detectors, acoustic impedance coupling materials, high-efficiency heat insulation materials, etc. Its unique fractal structure, dynamic characteristics and low-temperature thermal pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/02C01B31/04C01B32/05C01B32/194
Inventor 刘玲孟庆函杨杰
Owner BEIJING UNIV OF CHEM TECH
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