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Method for preparing ZrO2 aerogel

An airgel and post-gel technology, which is applied in the field of preparing ZrO2 airgel at normal pressure, can solve problems such as unsatisfactory effects, achieve uniform and stable structure, solve high cost, and improve safety

Active Publication Date: 2011-02-02
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the airgel is prepared according to the normal pressure drying method of the above-mentioned published patent, and the effect is not ideal.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1, a kind of ZrO 2 The preparation method of the airgel comprises the following steps: zirconium oxynitrate for zirconium inorganic salt, propylene oxide for epoxy, acetic acid for chelating agent, formamide as drying control chemical additive, and ethanol solution of ethyl orthosilicate ( The volume percent concentration of tetraethyl orthosilicate is 15%), and the low surface tension solvent is dehydrated alcohol; Carry out the following steps successively:

[0029] 1) Dissolve zirconyl nitrate in alcoholic water solvent at a temperature of 30-40°C, and stir magnetically; the dosage ratio of zirconyl nitrate to alcoholic water solvent is 0.3mol / L, and alcoholic water solvent has ethanol and water according to 3 : Mixed at a volume ratio of 1;

[0030] After the zirconyl nitrate is completely dissolved, add acetic acid and continue to stir for 30 minutes; then add formamide and continue to stir for 60 minutes; finally slowly add propylene oxide and continue...

Embodiment 2

[0039] Embodiment 2, a kind of ZrO 2 The preparation method of the airgel, the zirconium inorganic salt is selected from zirconium tetrachloride, the epoxide is selected from propylene oxide, the chelating agent is acetylacetone, the drying control chemical additive is polyethylene glycol, and the surface modification agent solution is trimethylchlorosilane ethanol solution (the volume percentage concentration of trimethylchlorosilane is 15%), and the low surface tension solvent is acetone; Carry out the following steps successively:

[0040] 1), at a temperature of 5-20°C, dissolve zirconium tetrachloride in alcoholic water solvent, and stir magnetically; the dosage ratio of zirconium tetrachloride and alcoholic water solvent is 0.5mol / L, and alcoholic water solvent is ethanol and water according to Mixed at a volume ratio of 3:1;

[0041] After the zirconium tetrachloride is completely dissolved, add acetylacetone and continue to stir for 60 minutes; then add polyethylene g...

Embodiment 3

[0049] Embodiment 3, a kind of ZrO 2 The preparation method of the airgel, the zirconium inorganic salt is selected from zirconium oxychloride, the epoxide is selected from propylene oxide, the chelating agent is acetic acid, the drying control chemical additive is dimethylformamide, and the surface modification agent solution is trimethylchlorosilane ethanol solution (the volume percentage concentration of trimethylchlorosilane is 20%), and the low surface tension solvent is normal hexane; Carry out the following steps successively:

[0050] 1), at a temperature of 5-40°C, dissolve zirconium oxychloride in alcoholic water solvent, and stir magnetically; the dosage ratio of zirconium oxychloride and alcoholic water solvent is 0.8mol / L, and alcoholic water solvent is ethanol and water according to Mixed at a volume ratio of 4:1;

[0051] After the zirconium oxychloride is completely dissolved, add acetic acid and continue to stir for 100 minutes; then add dimethylformamide and...

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Abstract

The invention discloses a method for preparing ZrO2 aerogel. The method sequentially comprises the following steps of: (1) dissolving a zirconium inorganic salt into an alcohol aqueous solvent, then sequentially adding a chelating agent, a drying control chemical additive and an epoxide and stirring for mixing; (2) carrying out a water bath on the obtained sol; (3) sequentially ageing, cleaning and soaking the sol subjected to the water bath; (4) drying the substance obtained in the step (3); and (5) carrying out heat treatment on the substance obtained in the step (4) at 400-700 DEG C for 3-8 hours to obtain the ZrO2 aerogel. In the invention, the specific surface area of the prepared ZrO2 aerogel is 400-800m<2> / g, the density is 100-500kg.m<-3>, the pore size distribution is narrow, and the ZrO2 aerogel is a nano scale. The ZrO2 aerogel has uniform and stable structure and can be widely applied to the fields of heat insulation, catalysis, environmental protection, and the like.

Description

technical field [0001] The invention belongs to the technical field of inorganic material preparation and sol-gel method, and specifically relates to a method of preparing ZrO at normal pressure using zirconium inorganic salt as a precursor 2 Airgel method. Background technique [0002] Airgel is a highly dispersed solid material in which colloidal particles or polymer molecules coalesce to form a nanoporous network structure, and the pores are filled with a gaseous dispersion medium. The solid phase and pore structure are both on the nanometer scale. The airgel porosity can reach 80-99.8%, the pore size is generally between 1-100nm, and the density range can reach 3-600kg m -3 . Due to its unique structure, airgel has many characteristics such as high specific surface area, high porosity, high adsorption, low density, low thermal conductivity, small Young's modulus, and small refractive index. Thermal, environmental protection, catalysis, chemical industry, high energy p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/00C01G25/02
Inventor 郭兴忠杨辉颜立清李文彦张玲洁
Owner ZHEJIANG UNIV
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