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Process for preparing water-soluble ceria nanocrystalline

A cerium dioxide, water-soluble technology, applied in the field of preparation of water-soluble CeO2 nanocrystals

Inactive Publication Date: 2009-12-02
CHANGCHUN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no water-soluble CeO 2 Related reports on the preparation of nanocrystals

Method used

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  • Process for preparing water-soluble ceria nanocrystalline
  • Process for preparing water-soluble ceria nanocrystalline
  • Process for preparing water-soluble ceria nanocrystalline

Examples

Experimental program
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Embodiment 1

[0018] Embodiment 1: take by weighing the Ce(acac) of 2mmol 3 ·H 2 O, add in the two-neck round bottom flask of 100ml, then add the 2-pyrrolidone of 20ml. Insert a thermometer into one neck of the bottle and a water-cooled reflux condenser into the other neck. The mixture was heated to 75°C, Ce(acac) 3 Dissolve in 2-pyrrolidone to obtain 0.1mol / L 2-pyrrolidone solution of cerium acetylacetonate, heat the solution to 240°C and reflux for 60min, remove the heating mantle, and cool to room temperature to obtain water-soluble CeO 2 Transparent brown sol of nanoparticles. Add 200ml of methanol to the solution, there is water-soluble CeO 2 The precipitation of nanoparticles is separated out, and the precipitation is centrifuged, and the precipitation is washed 5 times with acetone (each consumption 50ml), and the precipitation is washed with N 2 Flow drying for 4h, to obtain light yellow water-soluble CeO 2 Nanoparticles. If a certain amount of deionized water or 2-pyrrolidon...

Embodiment 2

[0019] Embodiment 2: take by weighing the Ce (acac) of 4mmol 3 ·H 2 O, add in the two-neck round bottom flask of 100ml, then add the 2-pyrrolidone of 20ml. Insert a thermometer into one neck of the bottle and a water-cooled reflux condenser into the other neck. The mixture was heated to 85°C, Ce(acac) 3 Dissolve in 2-pyrrolidone to obtain 0.2mol / L 2-pyrrolidone solution of cerium acetylacetonate, heat the solution to 225°C and reflux for 120min, remove the heating mantle and cool to room temperature to obtain water-soluble CeO 2 Transparent brown sol of nanoparticles. Add 300ml of methanol to the solution, there is water-soluble CeO 2 The nanoparticles were precipitated, and the precipitate was centrifuged, washed with acetone (80ml each time) for 5 times, and dried at 50°C for 10h to obtain light yellow water-soluble CeO 2 Nanoparticles. The prepared water-soluble CeO 2 The diameter of the nanoparticles is about 10 nm, and the particles are spherical.

Embodiment 3

[0020] Embodiment 3: take by weighing the Ce(acac) of 3mmol 3 ·H 2 O, add in the two-neck round bottom flask of 100ml, then add the 2-pyrrolidone of 20ml. Insert a thermometer into one neck of the bottle and a water-cooled reflux condenser into the other neck. The mixture was heated to 80°C, Ce(acac) 3 Dissolve in 2-pyrrolidone to obtain 0.15mol / L 2-pyrrolidone solution of cerium acetylacetonate, heat the solution to 230°C and reflux for 100min, remove the heating mantle, and cool to room temperature to obtain water-soluble CeO 2 Transparent brown sol of nanoparticles. Add 300ml of methanol to the sol, there is water-soluble CeO 2 The nanoparticles were precipitated, and the precipitate was centrifuged, washed with acetone (80ml each time) for 5 times, and dried at 60°C for 5h to obtain light yellow water-soluble CeO 2 Nanoparticles. The prepared water-soluble CeO 2 The diameter of the nanoparticles is about 8 nm, and the particles are spherical.

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Abstract

A method for preparing water-soluble ceria nanocrystals belongs to the technical field of nanomaterials. Existing CeO2 nanoparticles include non-surface-modified and oil-soluble CeO2 nanoparticles. The present invention adopts reflux hydrolysis method. The steps are: 1. Synthesis of water-soluble CeO2 nanoparticles dispersed in the solution. A reflux hydrolysis method is adopted, the cerium source is cerium acetylacetonate, and 2-pyrrolidone is used as a solvent and a surface modifier. The technical parameters are: reflux hydrolysis temperature: 225-240°C, reflux time: 60-120min. 2. Separation of water-soluble CeO2 nanoparticles from the solution. The solution containing the water-soluble CeO2 nanoparticles was cooled to room temperature, precipitated with methanol, centrifuged, washed with acetone, and dried. The technical parameters are: the amount of methanol used is 200-300ml, the amount of acetone used is 50-80ml, and dried with N2 flow for 4h or at 50-60°C for 5-10h. The final prepared water-soluble CeO2 nanoparticles have an average particle diameter of about 5nm-10nm and are spherical.

Description

technical field [0001] The invention relates to the field of nanomaterial research, in particular to water-soluble CeO 2 Methods of preparing nanocrystals. Background technique [0002] nano-CeO 2 Particles have a wide range of applications. For example, they can be used as three-way purification catalysts for automobile exhaust. They have the advantages of high activity, low price, and long life. They replace most precious metals and are used in thousands of tons per year. nano-CeO 2 Can be used in electronic ceramics and solid electrolytes. nano-CeO 2 The particles can be decorated on gold electrodes, which are good accelerators for the electrochemical reaction of cytochrome c. nano-CeO 2 The powder has a strong absorption of ultraviolet rays, and can be used to prepare ultraviolet-absorbing materials, such as absorbing 185nm short-wave ultraviolet rays in fluorescent tubes to improve the life of the lamp tubes, and also used in sunscreen cosmetics, sunscreen fibers,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00
Inventor 董相廷王进贤刘桂霞李正宇于文生
Owner CHANGCHUN UNIV OF SCI & TECH
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