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Preparation method of carbon aerogel

A technology of carbon aerogel and wet gel, applied in the field of aerogel, can solve the problems of low specific surface area of ​​carbon aerogel, difficult control of doping amount and metal particle size, etc. The effect of controllable structure and low cost

Inactive Publication Date: 2015-09-16
BEIJING UNIV OF CHEM TECH
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Problems solved by technology

[0005] At present, metal-doped carbon aerogels mainly include sol-gel method, ion exchange method and impregnation method, and the doped metals include Zr, Mo, Pd, Pt and magnetic metals (Moreno-Castilla C, et al.Langmuir ,2003,19:5650-5655; Maldonado-Hodar F J,et al.Microporous and Mesoporous Materials,2004,69:119-125), etc. The size of the metal particles prepared by the sol-gel method is relatively large, and the carbon aerogel The specific surface area is low, which has a certain impact on its adsorption performance; the amount of metal doping can be increased by ion exchange, but it is difficult to control the amount of doping and the size of metal particles; the impregnation method can well control the presence of metal salts on carbon. distribution and content in airgel, but it is necessary to prepare carbon airgel with good pore structure first

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  • Preparation method of carbon aerogel
  • Preparation method of carbon aerogel
  • Preparation method of carbon aerogel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Step 1: Weigh 4.404g resorcinol, 5.6ml formaldehyde, 15ml deionized water and 0.0424g sodium carbonate according to the molar ratio of 1:2:20:0.01; Take 5.816g of nickel nitrate, stir at room temperature for 30 minutes and mix evenly to obtain a dark green resorcinol-formaldehyde-nickel nitrate sol. After adding nickel nitrate, the pH value is 2.8;

[0027] According to the volume ratio of 1:9, measure 5mL of surfactant Span-80 and 45mL of cyclohexane, stir at 400r / min to form a uniform mixed solution, and then according to the volume of the mixed solution and resorcinol-formaldehyde sol Add 25mL of resorcinol-formaldehyde sol at a ratio of 2:1, continue to stir and react in a water bath at 25°C for 72h, then wash the product with acetone, ethanol and water to clean cyclohexane and Span-80 respectively to obtain intermolecular Hydroquinone-formaldehyde-nickel nitrate organic wet gel microspheres;

[0028] The obtained sample was naturally dried at room temperature to o...

Embodiment 2

[0033] Weigh 8.808g resorcinol, 11.2ml formaldehyde, 30ml deionized water, 0.0848g sodium carbonate according to the molar ratio of 1:2:0.2:20:0.01, and weigh 0.421g of nickel sulfate, stirred at room temperature for 0.1h and mixed evenly to obtain a grassy green resorcinol-formaldehyde-nickel sulfate sol. Add 0.1mol / L to 2mol / L of resorcinol-formaldehyde-nickel nitrate dropwise Sulfuric acid solution, adjust its pH value to 6.5;

[0034]Weigh 6.67ml of surfactant Span-80 and 33.3ml of cyclohexane according to the volume ratio of 1:5, stir at 1200r / min to form a uniform mixed solution, and then mix the mixed solution with resorcinol-formaldehyde sol Add 40mL of resorcinol-formaldehyde sol at a volume ratio of 1:1, continue to stir and react in a water bath at 100°C for 1h, then wash the product with acetone, ethanol and water to clean cyclohexane and Span-80 respectively to obtain Resorcinol-formaldehyde-nickel sulfate organic wet gel microspheres;

[0035] The obtained samp...

Embodiment 3

[0038] Weigh 3.303g of resorcinol, 4.2ml of formaldehyde, 11.25ml of deionized water and 0.0363g of sodium carbonate, weigh 0.599g of copper acetate according to the molar ratio of 1:10 to resorcinol, stir at room temperature for 1h and mix evenly to obtain Blue-green resorcinol-formaldehyde-copper acetate sol, measured after adding copper acetate, its pH value is 4.8;

[0039] According to the volume ratio of 1:80, measure 2ml of surfactant Span-80 and 160mL of cyclohexane, stir at 200r / min to form a uniform mixed solution, and then according to the volume of the mixed solution and resorcinol-formaldehyde sol Add 16.2mL of resorcinol-formaldehyde sol at a ratio of 10:1, continue to stir and react in a water bath at 20°C for 96h, then clean the cyclohexane and Span-80 with acetone, ethanol and water respectively to obtain Resorcinol-formaldehyde-copper acetate organic wet gel microspheres;

[0040] The obtained sample was naturally dried at room temperature to obtain copper a...

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Abstract

The invention provides a preparation method of metal doped carbon aerogel. A metal salt is added in the sol-gel process for forming resorcinol-formaldehyde organic aerogel, the skeleton strength of metal salt-containing carbon aerogel microspheres is high, and the microspheres can effectively oppose shrinkage stress, so fragmentation and deformation of the carbon aerogel are avoided in the drying process; and the metal doped carbon aerogel material with hemisphere, hollow sphere or capsule morphology can be obtained by changing experiment conditions. The method has the advantages of simple process, low cost, and preparation of the carbon aerogel material with different performance requirements through removing or reserving doped metal according to application requirements.

Description

technical field [0001] The invention relates to the technical field of aerogels, in particular to a method for preparing metal-doped carbon aerogels. Background technique [0002] Carbon airgel is a new type of porous material, which has the advantages of high porosity, high specific surface area, controllable pore size distribution, ultra-low thermal conductivity and low density. Carbon airgel materials have excellent performance and have been used in Chromatographic analysis, adsorption catalysis, heat insulation and electrochemical fields. [0003] At present, the preparation of carbon aerogels is mainly to prepare organic aerogels by supercritical drying method. The carbon aerogels obtained by carbonization have a high specific surface area and excellent adsorption performance, but the cost of supercritical drying process is very high, which restricts the Application and development of carbon airgel materials (Qin Renxi, Shen Jun et al., The Chinese Journal of Process E...

Claims

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Application Information

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IPC IPC(8): B01J13/00
Inventor 宋怀河雷倩陈晓红
Owner BEIJING UNIV OF CHEM TECH
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