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Method for preparing self-stabilized nano zirconium oxide sol by adopting hydrothermal method

A nano-zirconia and nano-oxidation technology, applied in zirconia and other directions, can solve the problems of few research reports on zirconia sol, and achieve the effects of short preparation period, high purity and simple process operation.

Inactive Publication Date: 2021-12-17
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Relatively speaking, there are various methods for synthesizing zirconia nanopowders, but there are few reports on the preparation of zirconia sol by hydrothermal method.

Method used

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  • Method for preparing self-stabilized nano zirconium oxide sol by adopting hydrothermal method
  • Method for preparing self-stabilized nano zirconium oxide sol by adopting hydrothermal method
  • Method for preparing self-stabilized nano zirconium oxide sol by adopting hydrothermal method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A kind of method that the present invention implements adopts hydrothermal method to prepare self-stabilizing nano-zirconia sol, and its specific steps are:

[0041] The consumption of table 1 embodiment 1 oxalic acid and zirconyl nitrate

[0042] Molar ratio of oxalic acid to zirconyl nitrate Oxalic acid / g Zirconium oxynitrate / g 0.6：1 0.5702 1.7429 0.7：1 0.6652 1.7429 0.8：1 0.76024 1.7429 0.9：1 0.8553 1.7429 1：1 0.9503 1.7429 1.5：1 1.4255 1.7429 2：1 1.9006 1.7429

[0043] At room temperature, according to the molar ratio of oxalic acid to zirconyl nitrate shown in Table 1, accurately weigh the corresponding weights of zirconyl nitrate and oxalic acid with an electronic balance, dissolve them in 34 mL of deionized water, and the concentration of zirconyl nitrate solution is 0.15 mol / L, seal the mouth of the beaker with plastic wrap. Continue magnetic stirring for 1 hour, slowly add 25 wt% tetramethylammonium h...

Embodiment 2

[0045] A kind of method that the present invention implements adopts hydrothermal method to prepare self-stabilizing nano-zirconia sol, and its specific steps are:

[0046] The consumption of table 2 embodiment 2 oxalic acid and zirconyl nitrate

[0047] PH value Oxalic acid / g Zirconium oxynitrate / g Precipitation 7.0 1.5838 2.9049 no precipitation, transparent 8.0 1.5838 2.9049 no precipitation, transparent 10.0 1.5838 2.9049 no precipitation, transparent

[0048] At room temperature, according to the molar ratio of oxalic acid to zirconyl nitrate 1:1, use an electronic balance to accurately weigh 2.9049g of zirconyl nitrate and 1.5838g of oxalic acid, and dissolve them in 34mL of deionized water. The concentration of the zirconyl nitrate solution is 0.25mol / L, seal the mouth of the beaker with plastic wrap. Continue magnetic stirring for 1 hour, slowly add 25 wt% tetramethylammonium hydroxide to the stock solution at a rate of 10-1...

Embodiment 3

[0050] A kind of method that the present invention implements adopts hydrothermal method to prepare self-stabilizing nano-zirconia sol, and its specific steps are:

[0051] At room temperature, according to the molar ratio of oxalic acid to zirconyl nitrate 1:1, use an electronic balance to accurately weigh 2.9049g of zirconyl nitrate and 1.5838g of oxalic acid, and dissolve them in 34mL of deionized water. The concentration of the zirconyl nitrate solution is 0.25mol / L, seal the mouth of the beaker with plastic wrap. Continue magnetic stirring for 1 hour, slowly add 25 wt% tetramethylammonium hydroxide to the stock solution at a rate of 10-15 drops / min, adjust the pH to 8.0, and continue stirring for 1 hour. The stock solution was then transferred to a 50 mL polytetrafluoroethylene-lined stainless steel autoclave, the autoclave was sealed, placed in a constant temperature drying oven, and reacted at 140° C. for 8 hours. After the autoclave was naturally cooled to room temper...

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Abstract

The invention belongs to the technical field of nano materials, and discloses a method for preparing self-stabilized nano zirconia sol by adopting a hydrothermal method. The method comprises the steps of (1) weighing zirconyl nitrate and oxalic acid, dissolving in deionized water, stirring and hydrolyzing to obtain a mixed solution; (2) adjusting the pH value to 7.0-10.0 by using tetramethylammonium hydroxide, and continuously stirring to obtain a precursor solution; (3) carrying out hydrothermal reaction on the precursor solution at the temperature of 140-170 DEG C for 4-8 hours; and (4) cooling to obtain clear and transparent liquid, namely, the zirconium oxide sol. According to the preparation method, the action mechanism and reaction participants of the preparation method are improved, zirconium oxynitrate with lower price is adopted as a precursor, oxalic acid is adopted as a complexing agent, a hydrothermal method with more economical efficiency is utilized, and meanwhile, reaction parameter conditions and the like are controlled, so that the self-stabilized nano zirconium oxide sol is successfully prepared, and a new way is provided for the market batch production of the zirconium oxide sol.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and more specifically relates to a method for preparing self-stabilizing nanometer zirconia sol by using a hydrothermal method. Background technique [0002] Zirconia sol is a colloidal solution containing charged zirconium fine particles uniformly dispersed in water, which has the characteristics of high light transmittance and high refractive index. Due to its high strength, toughness, high fluidity, low thermal conductivity, and high wear resistance, zirconia sol is widely used in the fields of coatings, adhesives, and catalysts, especially for the protective coating of resin lenses. [0003] At present, the methods for preparing zirconia mainly include coprecipitation method, sol-gel method and hydrothermal method. [0004] The ions introduced by the co-precipitation method are not easy to remove; the cost of the sol-gel method is relatively high, and in order to prevent the form...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02
CPCC01G25/02
Inventor 孙瑀瞳李家欣徐业彬
Owner HUAZHONG UNIV OF SCI & TECH
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