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Method for preparing high-dispersion nano-zirconia powder

A nano-zirconia, high-dispersion technology, applied in the direction of zirconia, nanotechnology, nanotechnology, etc., can solve the problems of high temperature requirements, high energy consumption, and agglomeration of zirconia powder, so as to achieve simple production process, avoid agglomeration, The effect of high surface area

Active Publication Date: 2014-05-07
DONGGUAN DIDA NANO MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN1168785C adopts azeotropic distillation dehydration when preparing nano-zirconia powder, and uses butanol, ethanol, etc. as entraining agents to dehydrate hydrated zirconium hydroxide gel, which can reduce the formation of powder hard agglomeration, but the dehydration temperature Higher requirements; Liang Liping, Dang Shue and others synthesized stabilized ZrO with different CaO concentrations by gel-supercritical fluid drying process. 2 Ultrafine powder, but this method consumes a lot of energy and is easy to cause the agglomeration of zirconia powder (Silicate Bulletin, 2002: 83-85)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Dehydrate the precipitated colloidal hydroxide and put it into a dryer with a pressure vessel structure, evacuate to reduce the pressure in the dryer to -0.08Mpa, pour the same weight of liquid ammonia solvent as the raw material, and perform countercurrent dehydration treatment at a temperature of 50 ℃ (operating pressure is the corresponding vapor pressure), after each treatment for 100 minutes, after a total of 2 treatments, the solvent is evacuated, and the solvent-containing hydroxide precipitate is vaporized under reduced pressure and the gauge pressure reaches 0 MPa and then vacuumed , When the gauge pressure is -0.09MPa, the temperature is 40~50℃, the dry hydroxide precipitate is obtained after 60min, and after crushing, it is calcined in a high temperature furnace at 600℃ for 120min to obtain nano zirconia (ZrO 2 ) Powder 1;

Embodiment 2

[0016] Put the colloidal hydroxide precipitate in a dryer with a pressure vessel structure, evacuate to reduce the pressure in the dryer to -0.08Mpa, pour the same weight of liquid ammonia solvent as the raw material, and perform countercurrent dehydration at a temperature of 70°C ( The operating pressure is the corresponding vapor pressure). After 60 minutes of each treatment for a total of 3 times, the solvent is evacuated, and the solvent-containing hydroxide precipitates are vaporized under reduced pressure and the gauge pressure reaches 0 MPa. The gauge pressure is -0.09MPa, the temperature is 50~60℃, and the dry hydroxide precipitate is obtained after maintaining for 40min. After crushing, it is calcined in a high-temperature furnace at 500℃ for 180min to obtain nano-zirconia (ZrO 2 ) Powder 2;

Embodiment 3

[0018] Precipitate the colloidal hydroxide into a dryer with a pressure vessel structure, apply a vacuum to reduce the pressure in the dryer to -0.08Mpa, pour in liquid ammonia solvent twice the weight of the raw material, and perform countercurrent dehydration at a temperature of 80°C (The operating pressure is the corresponding vapor pressure). After 30 minutes of each treatment for a total of 3 times, the solvent is evacuated, and the solvent-containing hydroxide precipitate is vaporized under reduced pressure, and the gauge pressure reaches 0 MPa and then vacuumed to desolvate. When the gauge pressure is -0.09MPa and the temperature is 50~60℃, the dried hydroxide precipitate will be obtained after maintaining for 60min. After crushing, it will be calcined in a high temperature furnace at 400℃ for 240min to obtain nano-ZrO 2 Powder 3;

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Abstract

The invention discloses a method for preparing high-dispersion nano-zirconia powder. The method comprises the following steps: adding an alkaline precipitant into an aqueous solution containing zircon salt to obtain a colloidal state hydroxide precipitate, sequentially filtering, washing and dehydrating to obtain a dried hydroxide precipitate, and finally, crushing to obtain the zirconia powder, wherein a subcritical fluid dehydration drying mode is adopted in the dehydration process, liquid ammonia serves as a medium in the subcritical fluid drying process, and moisture in the hydroxide precipitate is removed at the temperature of 50-80 DEG C and under the pH value of 8.8-9.2. According to the adopted preparation method, powder agglomeration in the nano-zirconia preparation process can be effectively avoided, and a high-purity high-dispersity and large-specific surface nano-zirconia product is obtained. Moreover, the method has the advantages of simple production process, low cost and energy consumption, simplicity in industrial production and the like.

Description

Technical field [0001] The invention belongs to the field of fine chemicals, and specifically relates to a method for preparing nano zirconia powder. Background technique [0002] Zirconia is white heavy amorphous powder or monoclinic crystal, odorless and tasteless. There are three crystal types of zirconia, monoclinic at low temperature, density 5.65g / cm 3 ; Form tetragonal crystal system above 1100℃, density 6.10g / cm 3 ; Form cubic crystal system above 2370℃, density is 6.27g / cm 3 . Zirconium dioxide is the only metal oxide with acidic, basic, oxidizing and reducing properties. Its chemical stability is very high. It is only soluble in hydrofluoric acid in various acids. Zirconium dioxide has high melting point and boiling point, high hardness, is an insulator at room temperature, and has excellent properties such as electrical conductivity at high temperature. Zirconia materials have excellent physical and chemical properties such as high hardness, high strength, high tough...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02B82Y30/00B82Y40/00
Inventor 吕小军宋自洪任柏芬
Owner DONGGUAN DIDA NANO MATERIALS CO LTD