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

A carbon aerogel, atmospheric drying technology, used 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, resistance to tension, simple and fast The effect of preparation

Inactive Publication Date: 2012-11-14
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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: Using phenol (P) and formaldehyde (F) as the reaction monomers, sodium hydroxide as the catalyst (C), and water as the solvent, according to the ratio of P / F=0.33, P / C=20, the solid For a solution with a content of 30wt%, add 2wt% of graphene oxide as a crosslinking agent and mix uniformly, heat at 60°C for 60 minutes to obtain a graphene crosslinked organic hydrogel, and put it in a water bath at 85°C for 72h aging. Then take out the gel column and dry it at 60°C for 24 hours under normal pressure to form an organic aerogel. The organic aerogel is put into a carbonization furnace, is protected by nitrogen, and is carbonized at a constant temperature of 900° C. for 2 hours to form a carbon aerogel. The specific surface area of ​​carbon aerogel is 485m 2 / g, pore volume 0.72cm 3 / g, the carbonization shrinkage rate is 49.9%.

Embodiment 2

[0020] Example 2: Using resorcinol (R) and formaldehyde (F) as reaction monomers, sodium carbonate as catalyst, and water as solvent, according to the ratio of R / F=0.5 and R / C=200, the solid content is formulated For a 5wt% solution, add 20wt% of functionalized graphene oxide as a crosslinking agent and mix uniformly, obtain a graphene crosslinked organic hydrogel at 20°C for 5 minutes, and place it in a 75°C water bath for aging for 7 days. Then take out the hydrogel column and dry it under infrared light for 10 hours to form organic aerogel. The organic aerogel is put into a carbonization furnace, is protected by nitrogen, and is carbonized at a constant temperature of 800° C. for 1 hour to form a carbon aerogel. The specific surface area of ​​carbon aerogel is 382m 2 / g, pore volume 0.42cm 3 / g, the carbonization shrinkage rate is 61.9%.

Embodiment 3

[0021] Example 3: Using resorcinol (R) and formaldehyde (F) as the reaction monomers, sodium carbonate as the catalyst, ethanol as the solvent, according to the ratio of R / F=0.5, R / C=200, the solid content For a 40wt% solution, add 0.5wt% of graphene oxide as a crosslinking agent to mix uniformly, heat at 80°C for 180 minutes to obtain a graphene crosslinked organic hydrogel, and put it in a water bath at 80°C for 72h aging. Then take out the gel column and dry it at room temperature under normal pressure for 48 hours, and then dry it at 120°C for 5 hours to form an organic aerogel. The organic aerogel is put into a carbonization furnace, is protected by nitrogen, and is carbonized at a constant temperature of 1100°C for 2 hours to form a carbon aerogel. The specific surface area of ​​carbon aerogel 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 aerogel and carbon aerogel by drying at normal pressure. Background technique [0002] Aerogel is a porous amorphous solid material composed of nano-scale colloidal particles or high polymer molecules, and it is also the lightest condensed material among synthetic materials. Its unique open nano-scale porous structure and continuous three-dimensional network make it have extremely low density, high specific surface area and high porosity, showing strong adsorption catalytic ability, low thermal conductivity, low acoustic impedance and low refractive index, etc. Therefore, aerogel 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 thermal insulation materials, etc. Its unique fractal structure, dynamic characteristics and low-temperature ther...

Claims

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Application Information

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Patent Type & Authority Applications(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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