Preparation method of loose zirconium hydroxide or zirconium oxide nano powder

A technology of nano-powder and zirconium hydroxide, which is applied in zirconia, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of increasing costs, achieve excellent performance, easy to filter and wash, and streamline the process flow

Inactive Publication Date: 2017-07-28
GUOBIAO BEIJING TESTING & CERTIFICATION CO LTD
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0008] Preparation of ZrO by Co-precipitation 2 Powder, the process is simple, and it is easy to realize industrial production. The ordinary co-precipitation method needs to be dried by azeotropic distillation, freeze drying, supercritical drying and other methods to obtain products with fine particle size and uniform distribution, which increases industrial production. cost

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  • Preparation method of loose zirconium hydroxide or zirconium oxide nano powder
  • Preparation method of loose zirconium hydroxide or zirconium oxide nano powder

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preparation example Construction

[0040] The preparation method of the zirconia-containing nano-loose powder of the present invention specifically comprises the following steps:

[0041]1) Precipitant A solution with a concentration of 0.05-4mol / L is prepared. The precipitant A solution contains dissolved carbonate, ammonium chloride, ammonium bicarbonate, calcium hydroxide, potassium hydroxide, sodium hydroxide, and One or more, while the precipitant A solution contains alcohols, wherein the alcohols have no more than 4 carbon atoms. The pH value of the precipitant A solution is adjusted to 3-13, the pH value is preferably in the range of 4-12, and the pH value is more preferably in the range of 5-11.

[0042] 2) Prepare a precipitant B solution with a concentration of 0.1-8mol / L, and the precipitant B solution contains one or more of dissolved sodium hydroxide, potassium hydroxide, calcium hydroxide, and ammonia water.

[0043] 3) In the solution containing zirconium salt, the concentration of zirconium ion...

Embodiment 1

[0048] Prepare a zirconium oxychloride and yttrium chloride mixed raw material solution with a concentration of 0.4mol / L. In this solution, the molar ratio of Zr ions to doped Y ions is 92:8. In the zirconium-containing raw material solution, ethanol and water The volume ratio of ammonium bicarbonate and ammonia water is 1:4; the mixed solution A of ammonium bicarbonate and ammonia water with a preparation concentration of 0.07mol / L (in the mixed solution, the mol ratio of ammonium bicarbonate and ammonia water is 1:1, and the volume ratio of ethanol and water is 1 :5), adjust the pH value to 7; the preparation concentration is the sodium hydroxide solution B of 3mol / L, and the pH value is 14. In the case of continuous stirring, first add the mixed raw material solution containing zirconium salt to the mixed solution A previously placed in the reactor at an initial flow rate of 0.01L / min; after adding for a period of time, the solution in the reactor changes from turbid to clea...

Embodiment 2

[0051] Prepare a zirconium oxychloride and yttrium chloride mixed raw material solution with a concentration of 0.8mol / L. In this solution, the molar ratio of Zr ions to doped Y ions is 92:8. In the zirconium-containing raw material solution, ethanol and water The volume ratio is 2:5; the preparation concentration is 0.1mol / L sodium carbonate and ammonia mixed solution A (in the mixed solution, the mol ratio of sodium carbonate and ammonia is 1:1), adjust the pH value to 8; the prepared concentration is 5mol / L sodium hydroxide solution B, the pH value is 14. Under the condition of continuous stirring, first add the mixed raw material solution containing zirconium salt to the mixed solution A previously placed in the reactor at an initial flow rate of 0.05L / min; after adding for a period of time, the solution in the reactor changes from turbid to clear, At the same time, solution B is added to the mixed solution of zirconium salt mixed raw material solution and mixed solution A...

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Abstract

The invention relates to a preparation method of a loose zirconium hydroxide or zirconium oxide nano powder, and belongs to the field of inorganic nano powder preparation. The preparation method comprises the steps of preparing a precipitant A solution and a precipitant B solution which have different pH (potential of hydrogen) values, adding a zirconium salt solution to the precipitant A solution at a certain flow rate, keeping the flow rate of the zirconium salt solution and simultaneously adding the precipitant B solution to the precipitant A solution at a certain flow rate after the solution becomes clarified from turbid, ageing, filtering, cleaning and drying to obtain the loose zirconium hydroxide nano powder, and then performing roasting and cooling to obtain the zirconium oxide nano powder. Zirconium hydroxide precursor slurry prepared by the method has no colloidality and is easy to filter; the dried zirconium hydroxide nano powder has no hard aggregation; the zirconium oxide powder generated after the roasting reaches a nanoscale; the particle size is 60-100nm; a pattern is regular; the distribution is narrow; the cleaning is easy; a ball milling process is not required; technological operation is simple and convenient; an equipment requirement is low; the preparation method is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a method for preparing loose zirconium hydroxide or zirconium oxide nanopowder, which belongs to the field of inorganic nanopowder preparation. Background technique [0002] Due to its excellent mechanical, thermal, electrical, and optical properties, zirconia has been widely used in high-temperature structural materials, high-temperature optical components, oxygen-sensitive components, and fuel cells. It is generally believed that ZrO 2 Crystals exist in three configurations: monoclinic, tetragonal, and cubic. In order to obtain a stable crystal structure type, generally in the preparation process, it is necessary to add a certain amount of phase stabilizer such as: yttrium oxide (Y 2 o 3 ), scandium oxide (Sc 2 o 3 ), cerium oxide (CeO 2 ), calcium oxide (CaO 2 ), magnesium oxide (MgO 2 )Wait. [0003] Nano zirconia powder has the characteristics of large specific surface area, high surface energy and low sintering t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02C01G25/00
CPCC01G25/02C01G25/00C01P2002/72C01P2004/03C01P2004/04C01P2004/32C01P2004/62C01P2004/80
Inventor 张婧蒋文全
Owner GUOBIAO BEIJING TESTING & CERTIFICATION CO LTD
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