Preparation method of blocky zirconium oxide aerogel

A gel and block technology, applied in zirconia and other directions, can solve the problems of fast hydrolysis rate, low structural strength, high price, etc., and achieve the effects of broad application prospects, uniform pore size distribution, and low thermal conductivity.

Active Publication Date: 2012-11-07
霖晓(天津)科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the ZrO prepared by these methods 2 Most aerogels are powders, which are mainly used as catalysts and catalyst supports. The small amount of blocks prepared are also not characterized by the thermal and mechanical properties of the samples due to low structural strength and poor repeatability of the preparation process.
Currently prepa

Method used

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

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Experimental program
Comparison scheme
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Embodiment 1

[0025] Zirconium oxychloride is selected for zirconium inorganic salt, ethanol is selected for alcohol solvent, acetic acid is selected for chelating agent, polyethylene glycol 600 is selected for dispersant, formamide is selected for drying control agent, propylene oxide is selected for epoxy, and 80vol% surface modification solution is selected Tetraethyl orthosilicate ethanol solution, ethanol is selected as the low critical point solvent; the following steps are carried out in sequence: 1) Weigh a certain amount of ZrOCl 2 ·8H 2 O, at a temperature of 20-35°C, dissolve in a mixed solution of ethanol and water, the concentration of the precursor is 0.3mol / L, and the volume ratio of ethanol and water is 4:1.

[0026] 2) After the zirconium oxychloride is completely dissolved, add anion exchange resin to the precursor solution according to the volume ratio of the resin to the precursor solution obtained in step 1) at 1:5, stir for 30 minutes, let stand for 2 hours, and then fil...

Embodiment 2

[0035] Zirconium oxynitrate is selected as zirconium inorganic salt, isopropanol is selected as alcohol solvent, oxalic acid is selected as chelating agent, polyethylene glycol 600 is selected as dispersant, N,N-dimethylformamide is selected as drying control agent, and propylene oxide is selected as epoxy , surface modification solution selects 40vol% methyltrimethoxysilane ethanol solution for use, low critical point solvent selects isopropanol for use; Carry out the following steps successively:

[0036] 1) Weigh a certain amount of ZrO(NO 3 ) 2 2H 2 O, at a temperature of 20-35°C, dissolve in a mixed solution of isopropanol and water, the concentration of the precursor is 0.1mol / L, and the volume ratio of isopropanol to water is 2:1.

[0037] 2) After zirconium oxynitrate is completely dissolved, add anion exchange resin in the precursor solution according to the volume ratio of the resin to the precursor solution obtained in step 1) of 1:10, stir for 40 minutes, let sta...

Embodiment 3

[0045] Use zirconium nitrate as the zirconium inorganic salt, n-butanol as the alcohol solvent, citric acid as the chelating agent, polyethylene glycol 600 as the dispersant, glycerol as the drying control agent, epichlorohydrin as the epoxy, and surface modification solution Select 20vol% dimethyldiethoxysilane ethanol solution, and select ethanol as the low critical point solvent; carry out the following steps in sequence:

[0046] 1) Weigh a certain amount of Zr(NO 3 ) 4 ·5H 2 O, at a temperature of 20-35°C, dissolve in a mixed solution of n-butanol and water, the precursor concentration is 0.5mol / L, and the volume ratio of n-butanol and water is 8:1.

[0047] 2) After zirconium nitrate is completely dissolved, add anion exchange resin in the precursor solution according to the volume ratio of the resin and the precursor solution obtained in step 1) of 1:10, stir for 60 minutes, let stand for 4 hours, and then filter out the resin to obtain ion exchange After the precurs...

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Abstract

The invention relates to a preparation method of blocky ZrO2 aerogel. According to the preparation method, ZrO2 aerogel is prepared from zirconium inorganic salt by means of combination of the anion exchange technique and the sol-gel technique and by using epoxides as gel accelerators, and the blocky ZrO2 aerogel which is high in strength, low in density and low in heat conductivity coefficient is prepared by adding chelants, dispersing agents, drying controlling agents and the like to adjust uniformity of gel networks and pore structures, using the gel aging technique to improve and reinforce gel network frame strength and combining the high-temperature supercritical drying technique. The method is used for preparing the high-performance blocky ZrO2 aerogel from the cheap zirconium inorganic salt which is harmless to human bodies, so that the blocky ZrO2 aerogel has wide application prospect in the field of high-temperature thermal-insulation materials.

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 zirconia (ZrO 2 ) method of bulk airgel, so as to realize its application in high temperature insulation materials. Background technique [0002] Airgel is the solid with the smallest density in the world. It has a three-dimensional nano-skeleton structure and nano-scale pores. The porosity can reach 99.8%, and the specific surface area can reach 1000m 2 / g, the minimum apparent density can reach 2Kg / m 3 . The unique structure of airgel determines that it has extremely low thermal conductivity (as low as 0.013W / (m K) at room temperature), and airgel also has many advantages such as high adsorption and low refractive index, so in Optics, electricity, heat insulation, environmental protection, catalysis and other fields have broad application prospects. [0003] The most common aerogels are SiO 2 Aeroge...

Claims

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Application Information

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IPC IPC(8): C01G25/02
Inventor 冯琬评李晓雷季惠明孙晓红王庆浦
Owner 霖晓(天津)科技有限公司
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