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Preparation method of zirconium oxide-silicon oxide composite aerogel

A composite airgel and silicon oxide technology, which is applied in zirconia, chemical instruments and methods, silicon compounds, etc., can solve problems such as less research, and achieve good high temperature stability and low thermal conductivity.

Active Publication Date: 2013-07-24
霖晓(天津)科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] It can be seen from the above that scientific research institutions at home and abroad have studied the preparation method, composite uniformity, and high-temperature stability mechanism of zirconia-silica composite airgel powder, but the preparation of the block and its use as a high-temperature insulation material There are few related studies

Method used

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  • Preparation method of zirconium oxide-silicon oxide composite aerogel
  • Preparation method of zirconium oxide-silicon oxide composite aerogel
  • Preparation method of zirconium oxide-silicon oxide composite aerogel

Examples

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Effect test

Embodiment 1

[0033] A preparation method of zirconia-silicon oxide composite airgel, the zirconium alkoxide is selected from zirconium n-propoxide, the siloxane is selected from ethyl orthosilicate, the alcohol solvent is selected from ethanol, and the aging solution is the volume ratio of absolute ethanol:orthosilicon A mixture of ethyl acetate = 1:0.25, the drying medium is absolute ethanol, the molar ratio of siloxane: zirconium alkoxide = 1:0.11, the concentration of zirconium alkoxide and siloxane in the zirconia-silica composite sol The sum is 0.25mol / L. Follow the steps in order:

[0034] (1) Preparation of prehydrolyzed siloxane solution

[0035] At 4°C, dissolve ethyl orthosilicate in ethanol, stir and mix to obtain a 0.225mol / L mixed solution; according to mol Si: mol HNO 3 =1: 0.06 drops concentrated nitric acid with a mass concentration of 65-68%. According to mol Si: mol H 2 O=1:3, add deionized water dropwise, and continue to stir for 60 minutes to obtain a prehydrolyzed ...

Embodiment 2

[0046] A preparation method of zirconia-silica composite airgel, the zirconium alkoxide is selected from zirconium n-propoxide, the siloxane is selected from tetramethoxysilane, the alcohol solvent is selected from n-propanol, and the aging solution is anhydrous ethanol by volume ratio: Ethyl orthosilicate = 1:1 mixed solution, the drying medium is absolute ethanol, the molar ratio of siloxane: zirconium alkoxide = 1:1, zirconium alkoxide and siloxane in the zirconia-silica composite sol The sum of the concentrations is 0.5mol / L. Follow the steps in order:

[0047] (1) Preparation of prehydrolyzed siloxane solution

[0048] At 20°C, dissolve tetramethoxysilane in n-propanol, stir and mix to obtain a 0.25mol / L mixed solution; according to mol Si: mol HNO 3 =1: 0.09 drops concentrated nitric acid with a mass concentration of 65-68%. According to mol Si: mol H 2 O=1:2.5 Add distilled water dropwise, and continue stirring for 30 minutes to obtain a prehydrolyzed siloxane solut...

Embodiment 3

[0059] A preparation method of zirconia-silicon oxide composite airgel, zirconium alkoxide is selected from zirconium isopropoxide, siloxane is selected from methyltriethoxysilane, alcohol solvent is selected from isopropanol, and the aging solution is volume ratio anhydrous Ethanol: tetraethyl orthosilicate = 1:2 mixture, the drying medium is isopropanol, the molar ratio of siloxane: zirconium alkoxide = 1:1, zirconium alkoxide and silicon in the zirconia-silica composite sol The sum of the concentrations of oxanes is 1.0 mol / L. Follow the steps in order:

[0060] (1) Preparation of prehydrolyzed siloxane solution

[0061] At 20°C, dissolve methyl triethoxy silicon in isopropanol, stir and mix to obtain a 0.5mol / L mixed solution; according to molSi:mol HNO 3 =1: 0.09 drops concentrated nitric acid with a mass concentration of 65-68%. According to mol Si: mol H 2 O=1:2.5 Add distilled water dropwise, and continue stirring for 30 minutes to obtain a prehydrolyzed siloxane s...

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Abstract

The invention relates to a preparation method of zirconium oxide-silicon oxide composite aerogel. The method comprises the following steps of: dissolving siloxane in alcohol and uniformly stirring the solution to obtain alcohol solution of the siloxane; titrating concentrated nitric acid with 65-68% of mass concentration, titrating deionized water after stirring uniformly and continuously stirring; titrating the concentrated nitric acid to the pre-hydrolyzed siloxane solution, titrating zirconium alkoxide after mixing uniformly, adding the deionized water after stirring uniformly and stirring continuously to obtain clear and transparent gel; transferring the gel to a mould, and still standing and aging the gel to obtain the zirconium oxide-silicon oxide composite wet gel; soaking the wet gel by using aging solution; and finally soaking the gel by using absolute ethyl alcohol or isopropanol solvent. The blocky zirconium oxide-silicon oxide composite aerogel featured with low density and low thermal conductivity prepared by the invention basically keeps the former microcosmic undefined structure after thermal treatment at 1000 DEG C, and has specific area up to 353m<2> / g and good high-temperature stability.

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 bulk zirconia-silicon oxide composite gasification with good high-temperature stability by using zirconium alkoxide and siloxane as precursors and adopting supercritical drying method Glue preparation method. Background technique [0002] Airgel is a low-density solid material composed of nanoscale gel particles, which has a three-dimensional continuous nanoscale porous network structure. The airgel density can be as low as one-sixth of air, the porosity can reach 80-99.8%, and the pore size is generally between 1 and 100nm. This unique nanoporous network structure makes airgel have the advantages of high specific surface area, high adsorption, low density, low thermal conductivity, low refractive index, etc., so it has a wide range of applications in catalysis, environmental protection, heat insulation, ...

Claims

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Application Information

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IPC IPC(8): C01G25/02C01B33/158
Inventor 王庆浦李晓雷季惠明孙晓红何健
Owner 霖晓(天津)科技有限公司
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