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Method for preparing fibrous zirconium dioxide aerogel

A zirconia, aerogel technology, applied in zirconia, chemical instruments and methods, colloidal chemistry, etc., can solve problems such as single morphology

Pending Publication Date: 2022-08-09
CHUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention: solve the problem that the microscopic morphology of traditional zirconia airgel is nano-particles, and the morphology is single

Method used

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  • Method for preparing fibrous zirconium dioxide aerogel
  • Method for preparing fibrous zirconium dioxide aerogel
  • Method for preparing fibrous zirconium dioxide aerogel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: Fibrous zirconia aerogel was prepared as follows:

[0027] 1) Configure zirconium salt precursor solution: 1.93g ZrOCl 2 ·8H 2 O was added to 60 mL of absolute ethanol, where [Zr 4 + ]=0.1mol / L, sealed with plastic wrap, and stirred on a magnetic stirrer until completely dissolved.

[0028] 2) Add 6 mL of 30% hydrogen peroxide solution (with a volume ratio of 1 / 10 to the zirconium salt precursor solution) into the above solution, and stir to obtain a mixed solution;

[0029]3) Configure gel accelerator solution: add 0.09 g of mercaptosuccinic acid to 6 mL of ethanol, stir until dissolved, and the concentration of mercaptosuccinic acid in the solution is 0.1 mol / L. All the mercaptosuccinic acid ethanol solution was added to the mixed solution, stirred rapidly, sealed and placed in a 25°C oven for 2 hours to obtain a wet gel;

[0030] 4) Put the wet gel into a glass dish filled with absolute ethanol, seal it, and put it into an oven at 40° C. for 5 days of...

Embodiment 2

[0035] 1) Configure zirconium salt precursor solution: 57.9g ZrOCl 2 ·8H 2 O was added to 60 mL of absolute ethanol, where [Zr 4 + ]=3mol / L, sealed with plastic wrap, and stirred on a magnetic stirrer until completely dissolved.

[0036] 2) Add 60 mL of 0.1% hydrogen peroxide solution (with a volume ratio of 1 / 1 to the zirconium salt precursor solution) into the above solution, and stir to obtain a mixed solution;

[0037] 3) Configure gel accelerator solution: add 9 g of mercaptosuccinic acid into 30 mL of ethanol, stir until dissolved, and the concentration of mercaptosuccinic acid in the solution is 10 mol / L. All the ethanol solution of mercaptosuccinic acid was added to the mixed solution, stirred rapidly, sealed and placed in an oven at 45°C for 12 hours to obtain a wet gel;

[0038] 4) Put the wet gel into a glass dish filled with absolute ethanol, seal it, and put it into an oven at 70° C. for aging for 2 d.

[0039] 5) the wet gel obtained after aging is put into ...

Embodiment 3

[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) Add 18 mL of 10% hydrogen peroxide solution (with a volume ratio of 1 / 3 to the zirconium salt precursor solution) into the above solution, and stir to obtain a mixed solution;

[0044] 3) Configure the gel accelerator solution: add 2.7 g of mercaptosuccinic acid to 18 mL of ethanol (with a volume ratio of 1 / 3 to the zirconium salt precursor solution), stir until dissolved, and the concentration of mercaptosuccinic acid in the solution is 1 mol / L. All the ethanol solution of mercaptosuccinic acid was added to the mixed solution, stirred rapidly, sealed and placed in a 70°C oven for 1 hour to obtain a wet gel;

[0045] 4) Put the wet gel into a glass dish filled with absolute ethanol, seal it, and put it into an oven at 25° C. for aging for 7 da...

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Abstract

The invention discloses a method for preparing fibrous zirconium dioxide aerogel, and particularly relates to a method for preparing nano fibrous zirconium dioxide aerogel by taking hydrogen peroxide as a nucleation inducer and taking mercaptosuccinic acid as a gel accelerator, 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) taking hydrogen peroxide as a nucleation inducer, adding the hydrogen peroxide into the dissolved zircon salt, adding a gel accelerator mercaptosuccinic 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 nanofiber-shaped zirconium dioxide aerogel. The nano fibrous zirconium dioxide aerogel with low density, high specific surface area and high porosity can be successfully prepared by adjusting the concentration of the inorganic metal zirconium salt and the addition amount of the hydrogen peroxide and the mercaptosuccinic acid.

Description

technical field [0001] The invention relates to the technical field of aerogel preparation, in particular to a method for preparing fibrous zirconia aerogel. Background technique [0002] To analyze the temperature resistance of materials from the perspective of material structure chemistry, internal energy, etc., zirconia has a melting point (2900°C) much higher than that of silicon oxide (1670°C) and alumina (2050°C), and has a very low The room temperature thermal conductivity of the bulk material is about (about 2.4W m -1 ·K -1 ), it can be expected that theoretically zirconia aerogel materials should have higher temperature resistance, becoming a breakthrough in the current SiO 2 The 1000 ℃ temperature limit of aerogel is the preferred material system for the development of a new generation of higher temperature resistant, lightweight and efficient aerospace insulation materials. [0003] In 1976, Teichner et al. have reported the preparation of ZrO from organic zirc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02B82Y40/00B01J13/00
CPCC01G25/02B82Y40/00B01J13/0091C01P2006/12C01P2006/10C01P2006/90Y02P20/54
Inventor 王晓青史振宇洪樟连支明佳欧德志杨柏冰张心如
Owner CHUZHOU UNIV
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