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Method for producing cerium-zirconium nanocomposite oxide fine particle with supercritical anti-solvent technology

A supercritical anti-solvent, nano-composite technology, used in zirconia, bulk chemical production, etc.

Inactive Publication Date: 2009-05-13
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no report on the method of preparing cerium-zirconium nanocomposite oxide particles by SAS method

Method used

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  • Method for producing cerium-zirconium nanocomposite oxide fine particle with supercritical anti-solvent technology
  • Method for producing cerium-zirconium nanocomposite oxide fine particle with supercritical anti-solvent technology
  • Method for producing cerium-zirconium nanocomposite oxide fine particle with supercritical anti-solvent technology

Examples

Experimental program
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Embodiment 1

[0031] Dissolve cerium acetate and zirconium nitrate in absolute ethanol, control the molar ratio of cerium / zirconium to 1:10, the total concentration of cerium nitrate and zirconium nitrate is 2wt%, and use a high-pressure pump to flow it through the nozzle at a flow rate of 3ml / min. Inject into the precipitation kettle, and at the same time, inject carbon dioxide into the precipitation kettle with a pump at a flow rate of 40ml / min. The temperature of the precipitation kettle is controlled at 320K, and the pressure of the precipitation kettle is controlled at 26MPa. Under these conditions, the anti-solvent process occurs, thereby preparing the precursor nanoparticles of cerium-zirconium composite oxide.

[0032] attached figure 1 The transmission electron microscope picture of the prepared cerium-zirconium composite oxide nano-precursor can be found that the average particle size range of the particle size is about 50-60nm. After firing the prepared composite oxide nano-prec...

Embodiment 2

[0034] Dissolve an appropriate amount of cerium acetylacetonate and zirconium acetylacetonate in methanol so that the molar ratio of cerium / zirconium is 3:1, the total concentration of cerium nitrate and zirconium nitrate is 3wt%, and use a plunger pump to pass through the nozzle at a flow rate of 2ml / min The solution is injected into the precipitation kettle, and at the same time, carbon dioxide is injected into the precipitation kettle with a pump at a flow rate of 30ml / min. The temperature of the precipitation kettle is controlled at 340K, and the pressure of the precipitation kettle is controlled at 40MPa. Then, a supercritical anti-solvent process occurs under the above conditions, thereby preparing a cerium-zirconium nanocomposite precursor. After the prepared nano-composite oxide precursor is calcined at 873K for 2 hours, cerium-zirconium nano-composite oxide particles can be prepared, and the particle size range is about 50-60nm. Its XRD spectrum is attached Figure 4...

Embodiment 3

[0036]The cerium acetylacetonate was dissolved in absolute ethanol, the solution concentration was 3%, the temperature of the precipitation tank was controlled at 313K, and the pressure was 35MPa, and the rest of the preparation process was the same as in Example 2. The cerium nano-precursor particles are prepared, and after being calcined at 773K for 2 hours, the average particle size of the cerium oxide oxide is 40-50nm.

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Abstract

The invention relates to a method for preparing nanoscale composite Ce-Zr oxide particles by supercritical antisolvent (SAS) technique. The method comprises the following steps: dissolving a Ce salt and a Zr salt in a solution; separating out the soluble salts of the Ce and Zr in a manner of uniformly-dispersed nanoparticles through the antisolvent effect of supercritical fluids to obtain the nanoscale precursor particles of the supercritical antisolvent; and baking the precursor to obtain the nanoscale composite Ce-Zr oxide particles. The SAS technique is a pure physical process so as to obviate the complex steps, such as washing and drying, of the conventional coprecipitation method, and has the advantages of mild operation condition, easily controlled process, small particle size, uniform size distribution, uniform distribution of each composite component, repeated use of CO2 and solvent, environmental protection, etc.

Description

technical field [0001] The invention relates to the technical field of preparing nanocomposite materials, in particular to a method for preparing cerium-zirconium nanocomposite oxide particles by supercritical antisolvent technology. Background technique [0002] The cerium-zirconium composite oxide with a solid solution structure composed of cerium and zirconium oxides is an important catalyst material. The cerium oxide has a unique ability to store and release oxygen. After cerium oxide and zirconia form a solid solution, It can effectively improve its specific surface area, oxygen storage performance and thermal stability. [0003] The properties of materials prepared by different preparation methods are quite different. The preparation methods of solid solution reported so far are: co-precipitation method, sol-gel method, ball milling method, surfactant template method, solution combustion method, chemical cutting file method, complexation method and so on. [0004] CN...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02
CPCY02P20/54
Inventor 姜浩锡李永辉余英哲张金彦张敏华
Owner TIANJIN UNIV
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