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Preparation method of zirconium oxide aerogel

A technology of airgel and zirconia, which is applied in the direction of zirconia to achieve the effect of reducing the possibility of cracking, reducing stress and increasing continuity

Active Publication Date: 2013-04-03
蓝烟新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved in the present invention is to use zirconium alkoxide as the precursor and adopt supercritical drying process to prepare low-density and low thermal conductivity block ZrO 2 Preparation method of airgel

Method used

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  • Preparation method of zirconium oxide aerogel
  • Preparation method of zirconium oxide aerogel
  • Preparation method of zirconium oxide aerogel

Examples

Experimental program
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Effect test

Embodiment 1

[0030] a ZrO 2 The preparation method of the airgel, the zirconium alkoxide is selected from zirconium n-butoxide, the epoxy is selected from propylene oxide, and the aging solution is absolute ethanol: tetraethyl orthosilicate: propylene oxide = 5:2:2 (volume ratio) The mixed solution, the low surface tension solvent is absolute ethanol. Follow the steps in order:

[0031] 1) ZrO 2 Preparation of sol: at 4°C, dissolve zirconium n-butoxide in absolute ethanol and mix uniformly to obtain a 0.25mol / L ethanol solution of zirconium n-butoxide; then follow the steps of zirconium n-butoxide: water: nitric acid: formamide: ring Propylene oxide=1:6:1:0:6 (molar ratio) Add 65-68wt% concentrated nitric acid drop by drop, continue to stir for 5 minutes; add water and propylene oxide, continue to stir for 30 minutes to obtain a light yellow transparent sol.

[0032] 2) ZrO 2 Preparation of wet gel: after the above sol stops stirring, transfer the sol to a mold and let it stand for 4 h...

Embodiment 2

[0038] a ZrO 2 The preparation method of the airgel, the zirconium alkoxide is selected from zirconium n-propoxide, the drying control agent is formamide, the epoxide is propylene oxide, and the aging solution is absolute ethanol: tetraethyl orthosilicate: propylene oxide=5: 4: 0.5 (volume ratio) the mixed solution after stirring, the low surface tension solvent is isopropanol. Follow the steps in order:

[0039] 1) ZrO 2 Preparation of sol: Dissolve zirconium n-propoxide in ethanol at 15°C, stir and mix evenly to obtain a 0.5mol / L ethanol solution of zirconium n-propoxide; then follow the steps of zirconium n-butoxide: water: nitric acid: formamide: ring Propylene oxide=1:2:0.856:0.3:3 (molar ratio) Add 65-68wt% concentrated nitric acid drop by drop, continue to stir for 20 minutes; add water, formamide and propylene oxide, continue to stir for 60 minutes to obtain a light yellow transparent sol ;

[0040] 2) ZrO 2 Preparation of wet gel: After stopping the stirring of t...

Embodiment 3

[0046] a ZrO 2 The preparation method of the airgel, the zirconium alkoxide is selected from zirconium isopropoxide, the drying control agent is formamide, and the aging solution is anhydrous ethanol: ethyl orthosilicate: propylene oxide = 5:3:1 (volume ratio) stirring After the mixed solution; the low surface tension solvent is absolute ethanol. Follow the steps in order:

[0047] 1) ZrO 2 Preparation of sol: Dissolve zirconium isopropoxide in ethanol at 40°C, stir and mix evenly to obtain a 2mol / L ethanol solution of zirconium isopropoxide; then follow the steps of zirconium isopropoxide: water: nitric acid: formamide: epoxy Propane=1:2:0.7:2:0 (molar ratio) Add 65-68wt% concentrated nitric acid drop by drop, continue to stir for 60 minutes; add water and formamide, continue to stir for 20 minutes to obtain light yellow transparent sol;

[0048] 2) ZrO 2 Preparation of the wet gel: after the stirring of the above sol was stopped, the sol was transferred to a mold, and th...

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Abstract

The invention provides a preparation method of zirconium oxide aerogel, which comprises the following steps of: dissolving alkoxide into anhydrous ethanol, and stirring and mixing to obtain an ethanol solution containing the alkoxide; dropwise adding concentrated nitric acid, then adding a mixed solution containing deionized water, formamide and epoxy propane, and continuously stirring for 20-60 minutes to obtain clear transparent sols; transferring the sols into a mould, and standing and ageing to obtain ZrO wet gels; respectively soaking the ZrO wet gels at 35-100 DEG C by using ageing liquids; and finally supercritically drying an object obtained by soaking with a drying medium solvent for 2-5 times to obtain a complete block-shaped ZrO aerogel. The method provided by the invention realizes the preparation of the block-shaped ZrO aerogel and solves the technical problem of preparing a low-density medium-intensity block-shaped zirconium oxide; and in addition, the block-shaped zirconium oxide aerogel has the density of 100-250 kg / m<3>, the normal-temperature heat conductivity of 0.018-0.031 w / mk and the compressive strength of 100-300 KPa.

Description

technical field [0001] The invention belongs to the technical field of inorganic material preparation and sol-gel method, and in particular relates to a method of preparing a low-density and low-thermal-conductivity block ZrO by using zirconium alkoxide as a precursor and adopting a supercritical drying method 2 Airgel method. Background technique [0002] Airgel is a porous condensed matter with a three-dimensional network structure that uses gas as a dispersion medium. Oxide aerogels start from inorganic salts or metal alkoxides, and prepare lightweight porous nanomaterials through steps such as sol, gel, aging and supercritical drying. Due to the high porosity, high specific surface area, low density, high adsorption, low thermal conductivity, small refractive index and many other characteristics of airgel, airgel is widely used in optics, electricity, catalysis, heat insulation, chemical industry and aviation. Aerospace and other fields are widely used. [0003] In th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02
Inventor 焦玉娜李晓雷季惠明孙晓红王庆浦
Owner 蓝烟新材料科技有限公司
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