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Method for preparing zirconium dioxide aerogel with different microtopographies

A technology of zirconia and microscopic morphology, applied in zirconia, chemical instruments and methods, colloid chemistry, etc., can solve the problem of single morphology

Inactive Publication Date: 2022-07-22
CHUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to solve the problem that the microscopic appearance of the zirconia airgel prepared by the traditional method is nano-particles, and the appearance is single

Method used

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  • Method for preparing zirconium dioxide aerogel with different microtopographies
  • Method for preparing zirconium dioxide aerogel with different microtopographies
  • Method for preparing zirconium dioxide aerogel with different microtopographies

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1: Fibrous zirconia aerogel was prepared as follows:

[0028] 1) Configure zirconium salt precursor solution: 19.3g ZrOCl 2 ·8H 2 O was added to 60 mL of absolute ethanol, where [Zr 4 + ]=1mol / L, seal with plastic wrap, stir on a magnetic stirrer until completely dissolved.

[0029] 2) Add 1.5 g of polyethylene oxide to 60 mL of the above-mentioned zirconium salt precursor solution, and stir to obtain solution one;

[0030] 3) Prepare gel accelerator solution: add 1.4713 g of glutamic acid to 10 mL of deionized water, stir until dissolved, and the concentration of glutamic acid in the solution is 1 mol / L.

[0031] 4) All the glutamic acid solution was added to solution one, stirred rapidly, sealed and placed in a 45°C environment for 2 hours to obtain a wet gel; put the wet gel into a glass dish filled with absolute ethanol, After sealing, it was placed in an oven at 40°C for 5d aging.

[0032] 5) the wet gel obtained after aging is put into the autoclave ...

Embodiment 2

[0034] Example 2: The aerogel material was prepared as follows:

[0035] 1) Configure zirconium salt precursor solution: 12.318g Zr(SO 4 ) 2 ·4H 2 O was added to 60 mL of absolute ethanol, where [Zr 4+ ]=1mol / L, seal with plastic wrap, stir on a magnetic stirrer until completely dissolved.

[0036] 2) 5 mL of formamide was added to 60 mL of the above-mentioned zirconium salt precursor solution, and stirred to obtain solution 1;

[0037] 3) Configure gel accelerator solution: add 1.4713 g of glutamic acid to 10 mL of deionized water, stir until dissolved, and the concentration of glutamic acid in the solution is 1 mol / L.

[0038] 4) All the glutamic acid solution was added to solution one, stirred rapidly, sealed and placed in a 25°C environment for 2 hours to obtain a wet gel; put the wet gel into a glass dish filled with absolute ethanol, After sealing, it was placed in an oven at 40°C for 5d aging.

[0039] 5) put the obtained wet gel after aging into the autoclave of th...

Embodiment 3

[0041] Embodiment 3: prepare submicron spherical zirconia aerogel material as follows:

[0042] 1) Configure zirconium salt precursor solution: 19.3g ZrOCl 2 ·8H 2 O was added to 60 mL of absolute ethanol, where [Zr 4 + ]=1mol / L, seal with plastic wrap, stir on a magnetic stirrer until completely dissolved.

[0043] 2) 1 mL of formamide was added to 60 mL of the above-mentioned zirconium salt precursor solution, and stirred to obtain solution 1;

[0044] 3) Configure gel accelerator solution: add 1.4713 g of glutamic acid to 10 mL of deionized water, stir until dissolved, and the concentration of glutamic acid in the solution is 1 mol / L.

[0045] 4) Add all the glutamic acid solution to solution one, stir quickly, seal and put it into a 70°C environment for 1 hour to obtain a wet gel; put the wet gel into a glass dish filled with absolute ethanol, After sealing, it was placed in an oven at 40°C for 5d aging.

[0046] 5) put the obtained wet gel after aging into the autoc...

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Abstract

The invention discloses a method for preparing zirconium dioxide aerogel with different microtopographies, which comprises the following specific steps: 1) taking inorganic metal zirconium salt as a zirconium source, and dissolving the zirconium source in absolute ethyl alcohol; 2) with polyoxyethylene as a phase-splitting agent and formamide as an additive, adding polyoxyethylene or formamide into the dissolved zircon salt, adding a gel accelerator glutamic acid, quickly stirring, sealing, and putting into a drying oven to obtain wet gel; (3) aging the wet gel; and (4) carrying out supercritical drying treatment on the aged wet gel by taking absolute ethyl alcohol and carbon dioxide as supercritical fluid media to finally obtain the zirconium dioxide aerogel with different microtopographies. By adjusting the concentration of the inorganic metal zirconium salt and the addition amount of polyoxyethylene and formamide, the one-dimensional nanofiber and sub-meter microspherical zirconium dioxide aerogel with low density, high specific surface area and high porosity can be successfully prepared.

Description

technical field [0001] The invention relates to the technical field of aerogel material preparation, in particular to a method for preparing zirconia aerogels with different microscopic shapes. Background technique [0002] Aerogel is the least dense solid in the world, with a density of only 3kg / m 3 . While this new material may seem fragile, it is actually very strong and durable. Aerogel materials can withstand a high temperature of up to 1400 ° C, while the current temperature resistance limit of traditional silica aerogel is 1000 ° C, compared with aluminum oxide (melting point 2050 ° C, thermal conductivity of about 10W·m-1· K -1 ) and silica (melting point 1670℃, thermal conductivity about 2.7W m -1 ·K -1 ) of these two materials, zirconium dioxide has a high melting point (2900°C) and a low thermal conductivity (about 2.4W m -1 ·K -1 )The advantages. How to improve the high temperature tolerance of zirconia aerogel materials and realize the application of zir...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02B01J13/00
CPCC01G25/02B01J13/0091C01P2002/72C01P2004/03C01P2004/04
Inventor 王晓青史振宇洪樟连支明佳严梦彤余楠
Owner CHUZHOU UNIV