Hydrothermal synthesis method for IVB-group metal oxide

An IVB group, oxide technology, applied in the direction of titanium oxide/hydroxide, zirconia, etc., can solve the problems of low yield, air pollution, increased cost, etc., to achieve obvious effect, excellent performance, and reduce the introduction of impurities. Effect

Inactive Publication Date: 2009-12-30
邢长生
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Although it is possible to add organic matter to zirconium hydroxide to improve the agglomeration of the powder, the effect is minimal, and the introduct

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  • Hydrothermal synthesis method for IVB-group metal oxide
  • Hydrothermal synthesis method for IVB-group metal oxide
  • Hydrothermal synthesis method for IVB-group metal oxide

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[0025] A specific but non-limiting embodiment of the present invention is to use the hydrothermal synthesis method of the present invention to produce zirconia powder. The hydrothermal synthesis method of described zirconia comprises:

[0026] (1) adding the zirconium salt solution to the alkaline precipitating agent to obtain zirconium hydroxide precipitation;

[0027] (2) washing the precipitate to remove other impurities;

[0028] (3) After adding water to the zirconium hydroxide precipitate to prepare a suspension, carry out a hydrothermal reaction to obtain a zirconium oxide suspension;

[0029] (4) Post-processing the zirconia suspension to obtain zirconia powder.

[0030] Specifically, in the above-mentioned step (1), the concentration of the zirconium salt solution is generally 0.02-0.2 mol / L (based on zirconium dioxide), preferably 0.2 mol / L. As the zirconium salt, zirconium oxychloride, zirconium nitrate or zirconium chloride can be used, and zirconium oxychloride...

Embodiment 1

[0040] Preparation of zirconia powder

[0041] Weigh 75.0kg of industrial-grade zirconium oxychloride (zirconia content is 36%), add it to 1 cubic meter of ultrapure water, stir into a transparent solution to obtain a zirconium oxychloride solution, and slowly add the solution to 2.5m 2 In the urea solution with pH = 9-10, white flocculent precipitate was obtained, and the reaction ended when pH = 8. Wash the precipitate with Class II electronic industrial water until there is no Cl in the precipitate - exist. Centrifuge the precipitate, then transfer the precipitate to a hydrothermal reactor, add 0.5m3 Heat ultrapure water to 150°C and keep it for 16 hours. When the temperature is lowered to below 100°C, wash the precipitate with II-grade electronic industrial water until no impurity ions exist in the precipitate. After spraying granulation and jet crushing, the zirconia powder can be obtained. figure 1 TEM photo of the obtained powder.

[0042] The zirconia powder is bidi...

Embodiment 2

[0044] Preparation of zirconia powder (with mineralizer added)

[0045] Weigh 75.0kg of industrial-grade zirconium oxychloride (the content of zirconia is 36%), add it to 1 cubic meter of ultrapure water, and stir it into a transparent solution to obtain a zirconium oxychloride solution, which is slowly added to 2.5m 2 In the urea solution with pH = 9-10, white flocculent precipitate was obtained, and the reaction ended when pH = 8. Wash the precipitate with Class II electronic industrial water until there is no Cl in the precipitate - exist. Centrifuge the precipitate, then transfer the precipitate to a hydrothermal reactor, add 0.5m 3 Add 500g of magnesium hydroxide to ultrapure water, heat it to 150°C and keep it for 16 hours. When the temperature drops below 100°C, wash the precipitate with II-grade electronic industrial water until there are no impurity ions in the precipitate. Spray granulation and jet crushing. Zirconia powder was obtained. figure 2 TEM photo of th...

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Abstract

The invention provides a hydrothermal synthesis method for IVB-group metal oxide. The IVB-group metal oxide is the oxide of titanium, zirconium or hafnium. The method comprises: adding IVB-group metal salt solution to alkaline precipitant and obtaining hydroxide precipitate; washing and precipitating to remove other impurities; adding water to the hydroxide precipitate to prepare suspension liquid and then performing hydrothermal reaction to obtain metal-oxide suspension liquid; and performing post-treatment to the metal-oxide suspension liquid to obtain metal oxide powder. The hydrothermal synthesis method can form zirconia powder through reaction at low temperature, thereby overcoming the disadvantage of using a co-precipitation method to product zirconia, avoiding powder agglomeration caused by high-temperature calcinations, ensuring the extremely excellent performance of the obtained zirconia powder and having the advantages of uniform particle size, good dispersity, strong maneuverability and the like. According to the hydrothermal synthesis method, zirconia composite material can also be produced by further adding stabilizers, such as yttrium-oxide compound zirconia, magnesium-oxide compound zirconia, cerium-oxide compound zirconia, calcium-oxide compound zirconia and the like.

Description

technical field [0001] The invention relates to a hydrothermal synthesis method of titanium, zirconium and hafnium oxides of group IVB metals, in particular to a hydrothermal synthesis method of zirconia, which belongs to the technical field of material preparation technology. Background technique [0002] Oxides of Group IVB metals titanium, zirconium or hafnium are widely used in industrial fields. Titanium oxide powder is widely used in various structural surface coatings, paper coatings and fillers, plastics and elastomers, ceramics, glass, catalysts, etc. Hafnium oxide is an excellent fast ion conductor material, which has very important applications in electronic materials, fuel cells and other fields. Zirconia powder is widely used in structural ceramics, electronic ceramics, bioceramics, advanced refractory materials, optical communication devices, artificial gemstones, oxygen sensors, solid oxygen fuel cells, grinding and polishing and other industries. Among them...

Claims

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Application Information

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IPC IPC(8): C01G23/04C01G25/02C01G27/02
Inventor 邢长生
Owner 邢长生
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