A preparation method for oil-soluble nano zirconium dioxide particles in a tetragonal crystal form by adopting an oil-water interface method

A technology of nano-zirconia and oil-water interface method, which is applied in the direction of zirconia, nanotechnology for materials and surface science, nanotechnology, etc. It can solve the problems of low particle purity and large particle size that are not conducive to large-scale industrial production. and other problems, to achieve the effect of good application prospect, simple operation method and uniform particle size distribution

Inactive Publication Date: 2013-11-13
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The hydrothermal method is inconvenient to operate, the prepared particles have low purity and are easy to agglomerate, the particle size is not easy to control, the particle size is large, the product loss is large, and the yield is low
The raw material cost of sol-gel method is high, which is not conducive to large-scale industrial production. When heat treatment is performed at high temperature, the particles will be quickly agglomerated, and the formation of colloidal particles and gel filtration and washing processes are difficult to control.
The microemulsion method also has the disadvantages of complex production process, high cost, low yield and the need for roasting.

Method used

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  • A preparation method for oil-soluble nano zirconium dioxide particles in a tetragonal crystal form by adopting an oil-water interface method
  • A preparation method for oil-soluble nano zirconium dioxide particles in a tetragonal crystal form by adopting an oil-water interface method
  • A preparation method for oil-soluble nano zirconium dioxide particles in a tetragonal crystal form by adopting an oil-water interface method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Weigh 1.5222g of sodium oleate and dissolve it in 10ml of deionized water at 45°C. After the sodium oleate was completely dissolved, 5 ml of 0.5 mol / L zirconium oxychloride solution was added to obtain a precipitate. Then add 25ml of cyclohexane to the system, stir magnetically at room temperature for 2-3 hours, until the water phase is colorless and transparent, and the oil phase is milky white, then transfer to a 100ml high-pressure hydrothermal reaction kettle.

[0027] (2) Weigh 3g of sodium hydroxide, dissolve it in 10ml of deionized water, and add it dropwise to the reaction kettle.

[0028] (3) Place the reaction kettle in a blast drying oven and react at 100°C for 24 hours.

[0029] (4) After the reaction, after the high-pressure hydrothermal reactor is naturally cooled to room temperature, wash with absolute ethanol, centrifuge at 10,000rpm for 15min to remove the supernatant, then wash with deionized water, and centrifuge at 10,000rpm for 15min Remove th...

Embodiment 2

[0031] (1) Weigh 1.5222g of sodium oleate and dissolve it in 10ml of deionized water at 45°C. After the sodium oleate was completely dissolved, 5 ml of 0.5 mol / L zirconium oxychloride solution was added to obtain a precipitate. Then add 25ml of cyclohexane to the system, stir magnetically at room temperature for 2-3 hours, until the water phase is colorless and transparent, and the oil phase is milky white, then transfer to a 100ml high-pressure hydrothermal reaction kettle.

[0032] (2) Weigh 3g of sodium hydroxide, dissolve it in 10ml of deionized water, and add it dropwise to the reaction kettle.

[0033] (3) Place the reaction kettle in a blast drying oven and react at 120°C for 24 hours.

[0034] (4) After the reaction, after the high-pressure hydrothermal reactor is naturally cooled to room temperature, wash with absolute ethanol, centrifuge at 10,000rpm for 15min to remove the supernatant, then wash with deionized water, and centrifuge at 10,000rpm for 15min Remove th...

Embodiment 3

[0036] (1) Weigh 1.5222g of sodium oleate and dissolve it in 10ml of deionized water at 45°C. After the sodium oleate was completely dissolved, 5 ml of 0.5 mol / L zirconium oxychloride solution was added to obtain a precipitate. Then add 25ml of cyclohexane to the system, stir magnetically at room temperature for 2-3 hours, until the water phase is colorless and transparent, and the oil phase is milky white, then transfer to a 100ml high-pressure hydrothermal reaction kettle.

[0037] (2) Weigh 2g of sodium hydroxide, dissolve it in 10ml of deionized water, and add it dropwise into the reaction kettle.

[0038] (3) Put the reaction kettle in a blast drying oven and react at 120°C for 72 hours.

[0039] (4) After the reaction, after the high-pressure hydrothermal reactor is naturally cooled to room temperature, wash with absolute ethanol, centrifuge at 10,000rpm for 15min to remove the supernatant, then wash with deionized water, and centrifuge at 10,000rpm for 15min Remove th...

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Abstract

The invention relates to a preparation method for oil-soluble nano zirconium dioxide particles in a tetragonal crystal form by adopting an oil-water interface method. The preparation method comprises (1) a step of dropwise adding, at the room temperature, a zirconium oxychloride solution into a sodium oleate water solution, adding cyclohexane and stirring magnetically to obtain a mixture; (2) a step of transferring the mixture into a high-pressure hydrothermal reaction kettle, adding a sodium hydroxide solution until an oil-water volume ratio of the system is 1:1, and then reacting at 100-120 DEG C for 24-72 h; and (3) a step of separating the oil phase after the reaction is finished to obtain an oil phase product, washing alternately with ethanol and deionized water, and finally drying. The method has a simple operation method, good repeatability, easily controllable reaction conditions, and low requirements of temperature. The oil-soluble nano zirconium dioxide particles in the tetragonal crystal form having uniform particle size distribution and good dispersibility can be prepared without the need of calcination. Applications of the nano zirconium dioxide particles in oil phases are greatly improved. The method has a good application prospect.

Description

technical field [0001] The invention belongs to the field of preparation of zirconia nano particles, in particular to a method for preparing oil-soluble tetragonal nano zirconia particles by an oil-water interface method. Background technique [0002] Zirconium dioxide is a very important structural and functional material with excellent physical and chemical properties. For a long time, zirconium dioxide has been widely used in the preparation of high-temperature structural ceramics because it can improve the toughness and strength of ceramic materials and improve the wear resistance of polymers. In recent years, the work of zirconium dioxide as a heterogeneous catalyst or adsorbent support has received great attention. In the catalytic reaction and adsorption process, ZrO with high specific surface area 2 Usually, it has more active centers itself or can be used as a carrier to carry more active components, thus showing higher catalytic and adsorption activities. Due to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02B82Y30/00
Inventor 周兴平刘力
Owner DONGHUA UNIV
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