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Block zirconia-based aerogel prepared with na2sio3 function as both gel accelerator and structure modifier and preparation method

A technology of structure modifier and gel accelerator, applied in the field of bulk zirconia-based aerogel and its preparation, can solve the problems of fast hydrolysis rate, flammability, weak particle bonding strength, etc. Improve the overall strength and the effect of adjustable bonding strength

Active Publication Date: 2018-10-19
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are two problems in this method of preparing zirconia aerogels using organic zirconium alkoxides as precursors: first, the raw materials are difficult to obtain and expensive, and it is impossible to prepare zirconia oxide aerogels on a large scale; The reaction rate is difficult to control. Zirconia nanoparticles cannot form a continuous network structure similar to silica, and the bonding strength between particles is weak. Therefore, most of the zirconia aerogels studied in the initial stage are in powder form and block zirconia aerogels cannot be obtained.
However, epoxy compounds are generally toxic and flammable, which pose certain risks during the experiment
Moreover, this method also has problems such as too fast hydrolysis rate, the formation of the three-dimensional continuous network structure of the gel and the difficulty in its regulation, and it is difficult to obtain a stable and uniformly structured zirconia airgel material; The connection strength of medium-nanoparticles is weak, and it is impossible to obtain large-sized bulk zirconia airgel
This greatly limits the application of zirconia airgel in the field of high temperature insulation

Method used

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  • Block zirconia-based aerogel prepared with na2sio3 function as both gel accelerator and structure modifier and preparation method
  • Block zirconia-based aerogel prepared with na2sio3 function as both gel accelerator and structure modifier and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023](1) Configure the precursor solution: mix 8.3g ZrOCl 2 ·8H 2 O and 2.2g Y(NO 3 ) 3 ·6H 2 O was added to the mixed solution of 69 ml of absolute ethanol and 17.25 ml of deionized water, then added 4.68 ml of acetic acid, 2.76 ml of polyethylene glycol, and 0.52 ml of formamide, sealed with plastic wrap, and stirred on a magnetic stirrer until completely dissolved.

[0024] (2) Preparation of Na 2 SiO 3 solution, the Na 2 SiO 3 Added to dilute ammonia water (0.1mol / L), Na 2 SiO 3 The concentration is 0.35mol / L.

[0025] (3) 60ml of the above-mentioned Na 2 SiO 3 The solution is added dropwise into the precursor solution and stirred evenly to form a sol. The above sol was poured into a petri dish, sealed with a plastic wrap, placed in a tray, and placed in an oven at 60°C to form a wet gel.

[0026] (4) Add absolute ethanol until the wet gel is completely submerged, and put it in an oven at 40°C for aging treatment for 72 hours.

[0027] (5) Put the wet gel o...

Embodiment 2

[0030] (1) Configure the precursor solution: mix 8.3g ZrOCl 2 ·8H 2 O and 2.2g Y(NO 3 ) 3 ·6H 2 O was added to the mixed solution of 69 ml of absolute ethanol and 17.25 ml of deionized water, then added 4.68 ml of acetic acid, 2.76 ml of polyethylene glycol, and 0.52 ml of formamide, sealed with plastic wrap, and stirred on a magnetic stirrer until completely dissolved.

[0031] (2) Preparation of Na 2 SiO 3 solution, the Na 2 SiO 3 Added to dilute ammonia water (0.2mol / L), Na 2 SiO 3 The concentration is 0.29mol / L.

[0032] (3) 60ml of the above-mentioned Na 2 SiO 3 The solution is added dropwise into the precursor solution and stirred evenly to form a sol. The above sol was poured into a petri dish, sealed with a plastic wrap, placed in a tray, and placed in an oven at 60°C to form a wet gel.

[0033] (4) Add absolute ethanol until the wet gel is completely submerged, and put it in an oven at 40°C for aging treatment for 72 hours.

[0034] (5) Put the wet gel ...

Embodiment 3

[0037] (1) Configure the precursor solution: mix 8.3g ZrOCl 2 ·8H 2 O and 2.2g Y(NO 3 ) 3 ·6H 2 O was added to 69 ml of absolute ethanol, 17.25 ml of deionized water, 4.68 ml of acetic acid, 2.76 ml of polyethylene glycol, and 0.52 ml of formamide, sealed with plastic wrap, and stirred on a magnetic stirrer until completely dissolved.

[0038] (2) Preparation of Na 2 SiO 3 solution, the Na 2 SiO 3 Added to deionized water, Na 2 SiO 3 The concentration is 0.50mol / L.

[0039] (3) 60ml of the above-mentioned Na 2 SiO 3 The solution is added dropwise into the precursor solution and stirred evenly to form a sol. The above sol was poured into a petri dish, sealed with a plastic wrap, placed in a tray, and placed in an oven at 60°C to form a wet gel.

[0040] (4) Add absolute ethanol until the wet gel is completely submerged, and put it in an oven at 40°C for aging treatment for 72 hours.

[0041] (5) Put the wet gel obtained after aging in step 4) into the autoclave of...

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Abstract

The invention discloses a massive zirconium-oxide-base aerogel prepared by using Na2SiO3 as a gel accelerator and structure modifier and a preparation method thereof. The preparation method comprises the following steps: 1) dissolving an inorganic zirconium salt in an ethanol-water mixed solution, and adding a right amount of additives to form an inorganic zirconium salt solution; 2) dissolving Na2SiO3 in ammonia water with a certain concentration to form a Na2SiO3 solution; (3) dropwisely adding the Na2SiO3 solution into the inorganic zirconium salt solution, uniformly stirring the solution, and pouring the solution into a mold to form a wet gel; 4) adding anhydrous ethanol until the wet gel is completely immersed, and carrying out aging treatment; and 5) carrying out supercritical drying on the aged wet gel to obtain the massive zirconium-oxide-base aerogel. The zirconium-oxide-base aerogel prepared by the method has favorable lumping property; and the inorganic zirconium salt / water glass proportion is regulated to implement controllable regulation on density, specific area and porosity of the zirconium-oxide-base aerogel as well as bonding strength among nanoparticles and other performance parameters of the structural unit. The preparation method has the advantages of cheap and accessible raw materials, simple technique and short reaction period. The prepared zirconium-oxide-base aerogel has the advantages of high structural strength, and can easily implement scale-up production.

Description

technical field [0001] The invention belongs to the technical field of airgel material preparation, in particular to a 2 SiO 3 A bulk zirconia-based aerogel prepared with dual functions of a gel accelerator and a structure modifier at the same time and a preparation method thereof. Background technique [0002] Zirconia aerogels are recognized as potential candidates for next-generation high-temperature-resistant, high-efficiency thermal insulation materials. The characteristics of low intrinsic thermal conductivity (thermal conductivity at room temperature: 1.8W / m K) and high melting point (~2700°C) of zirconia materials, the nanoparticle size and pore distribution structure of the airgel material unit are similar Under certain circumstances, it can be expected that the working temperature range and thermal insulation performance of zirconia airgel will exceed those of currently commonly used silica (thermal conductivity at room temperature 8.0W / m K, melting point ~ 1650°...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/48C04B35/624
CPCC04B35/48C04B35/624C04B2235/3418
Inventor 洪樟连高海波支明佳张家正史振宇
Owner ZHEJIANG UNIV