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: 2008-11-19
CHANGCHUN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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
Comparison scheme
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Embodiment 1

[0014] Example 1: Weigh 2mmol Ce(acac) 3 ·H 2 O, add a 100ml two-necked round bottom flask, then add 20ml of 2-pyrrolidone. Insert the thermometer into one bottleneck, and insert the water-cooled reflux condenser into the other bottleneck. Heat the mixture to 75℃, Ce(acac) 3 Dissolve in 2-pyrrolidone to obtain a 0.1 mol / L 2-pyrrolidone solution of cerium acetylacetonate, heat the solution to 240°C and reflux for 60 minutes, 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, which has water-soluble CeO 2 Nanoparticles precipitate out, centrifuge the precipitate, wash the precipitate 5 times with acetone (50ml each time), and dry it with N2 flow for 4 hours to obtain light yellow water-soluble CeO 2 Nanoparticles. If a certain amount of deionized water or 2-pyrrolidone is added to the solid particles, a transparent colloidal solution can be obtained. figure 1 Is water-s...

Embodiment 2

[0015] Example 2: Weigh 4mmol Ce(acac) 3 ·H 2 O, add a 100ml two-necked round bottom flask, then add 20ml of 2-pyrrolidone. Insert the thermometer into one bottleneck, and insert the water-cooled reflux condenser into the other bottleneck. Heat the mixture to 85°C, Ce(acac) 3 Dissolve in 2-pyrrolidone to obtain a 0.2mol / L 2-pyrrolidone solution of cerium acetylacetonate, heat the solution to 225°C and reflux for 120 minutes, 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 this solution, with water-soluble CeO 2 Nano particles precipitate out, centrifuge the precipitate, wash the precipitate 5 times with acetone (80ml each time), and dry it at 50°C for 10 hours to obtain light yellow water-soluble CeO 2 Nanoparticles. Prepared water-soluble CeO 2 The diameter of the nanoparticles is about 10 nm, and the particles are spherical.

Embodiment 3

[0016] Example 3: Weigh 3mmol Ce(acac) 3 ·H 2 O, add a 100ml two-necked round bottom flask, then add 20ml of 2-pyrrolidone. Insert the thermometer into one bottleneck, and insert the water-cooled reflux condenser into the other bottleneck. Heat the mixture to 80°C, Ce(acac) 3 Dissolve in 2-pyrrolidone to obtain a 0.15 mol / L 2-pyrrolidone solution of cerium acetylacetonate. Heat the solution to 230°C and reflux for 100 minutes. 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, which has water-soluble CeO 2 Nano particles precipitate out, centrifuge the precipitate, wash the precipitate 5 times with acetone (80ml each time), and dry it at 60°C for 5 hours to obtain light yellow water-soluble CeO 2 Nanoparticles. Prepared water-soluble CeO 2 The diameter of the nanoparticles is about 8nm, and the particles are spherical.

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Abstract

The invention provides a method for preparing a water-soluble ceria nano-crystal, belonging to the nano material technical field. The prior CeO2 nano particles include oil-soluble CeO2 nano particles without surface finishing. A back flow hydrolization method is adopted in the invention. The method of the invention comprises the following steps that: 1. the water-soluble nano particles dispersed in a solution are synthesized; and the back flow hydrolization method is adopted, wherein the cerium source is acetylacetone cerium, and the solvent and the surface finishing agent are 2-pyrrolidone; technical parameters are as follows: the temperature of the back flow hydrolization is between 225 and 240 DEG C, and the time of the back flow is between 60 and 120min; 2. the water-soluble nano particles are separated from the solution; the solution containing the water-soluble nano particles is cooled down to the room temperature and undergoes the steps of deposition by methanol, centrifugal separation, washing by acetone and drying; technical parameters are as follows: the use level of the methanol is between 200 and 300ml, the use level of the acetone is between 50 and 80ml, and the solution is dried by N2 flow for 4h or at a temperature of between 50 and 60 DEG C for 5 to 10h. The water-soluble ceria nano particles finally obtained are ball-shaped and the average particle diameter of which is approximately 5 to 10nm.

Description

Technical field [0001] The present invention relates to the field of nanomaterial research, in particular to water-soluble CeO 2 Preparation method of 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 of the precious metals and consume thousands of tons per year. Nano CeO 2 Can be used for electronic ceramics and solid electrolytes. Nano CeO 2 The particles can be modified on the gold electrode, which is a good promoter of the electrochemical reaction of cytochrome C. Nano CeO 2 The powder has 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 increase the life of the tube, and also used in sunscreen cosmetics, sunscreen fibers, automot...

Claims

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Application Information

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Patent Type & Authority Applications(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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