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A preparation method of cerium-based oxygen storage material doped with magnesium and aluminum mesoporous hollow microspheres

A technology of hollow microspheres and oxygen storage materials, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, inorganic chemistry, etc., can solve the problem of oxygen storage capacity and specific surface area reduction, loss of porous structure, Poor thermal stability and other problems, to achieve the effect of improving oxygen storage capacity, increasing specific surface area, and simple preparation steps

Active Publication Date: 2018-01-12
CHONGQING TONGHUI GAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The composition of the first generation cerium-based oxygen storage materials is pure CeO 2 , its main feature is that the oxygen storage performance depends on the specific surface area, the thermal stability is poor, and the specific surface area decreases rapidly after aging above 850 ° C, thus losing the oxygen storage performance; the composition of the second-generation cerium-based oxygen storage material is CeO 2 -ZrO 2 , which is characterized by the fact that both the surface and the bulk phase of the oxygen storage material can store oxygen, so the oxygen storage performance not only depends on the specific surface area of ​​the material, but the thermal stability of the texture is poor at high temperature, and the specific surface area decreases rapidly, thus affecting the oxygen storage / release performance The third generation of cerium-based oxygen storage materials is still in the development stage, and the research focus is mainly on low-valent ions such as Y 3+ , La 3+ 、Al 3+ Equally doped CeO 2 -ZrO 2 Solid solution, the purpose is to increase oxygen ion defects in the bulk phase to improve the structure, texture and oxygen storage performance of CeO2-ZrO2 solid solution
But above 1123K, CeO 2 Easy to sinter and lose the porous structure, thereby reducing the oxygen storage capacity and specific surface area

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0017] First, weigh 150g of sodium silicate, put it into a container, and add 550mL of water into the container at the same time, control the temperature at 37°C, stir at 300r / min for 1h, and add it dropwise at a rate of 2 drops / s while stirring. 20mL mass fraction is 30% hydrochloric acid solution, after the stirring is completed, move the container with the mixed solution into an ultrasonic disperser, carry out ultrasonic dispersion treatment for 2h, and obtain a dispersion liquid; then add 15mL mass concentration of 1.5mol / L magnesium nitrate solution and 15mL aluminum nitrate solution with a mass concentration of 1.2mol / L, after stirring and mixing at 260r / min, 10mL acetone was added dropwise to it, and ultrasonic dispersion treatment was carried out for 1h, and then 10g After mixing cerium acetylacetonate, shake it in a shaker for 2 hours; after shaking it, add 10 mL of ammonia water with a mass fraction of 17% to the shaker at a rate of 2 drops / s, adjust the pH to 9.0, an...

example 2

[0019]First weigh 175g of sodium silicate, put it into a container, and add 600mL of water into the container at the same time, control the temperature at 38°C, stir at 300r / min for 2h, and add it dropwise at a rate of 3 drops / s while stirring. 23mL mass fraction is 30% hydrochloric acid solution, after the stirring is completed, move the container with the mixed solution into an ultrasonic disperser, carry out ultrasonic dispersion treatment for 3h, and obtain a dispersion liquid; then add 20mL mass concentration of 1.5mol / L magnesium nitrate solution and 18mL aluminum nitrate solution with a mass concentration of 1.2mol / L were stirred and mixed evenly at 260r / min, then 11mL acetone was added dropwise to it, and ultrasonic dispersion was performed for 2 hours, and then 13g After mixing cerium acetylacetonate, shake it in a shaker for 3 hours; after shaking it, add 13 mL of ammonia water with a mass fraction of 17% to the shaker at a rate of 3 drops / s, adjust the pH to 9.5, and...

example 3

[0021] First weigh 200g of sodium silicate, put it into a container, and add 650mL of water into the container at the same time, control the temperature at 39°C, stir at 300r / min for 2h, and add it dropwise at a rate of 3 drops / s while stirring. 25mL mass fraction is 30% hydrochloric acid solution, after stirring is completed, the container that mixed solution is housed is moved in the ultrasonic disperser, carry out ultrasonic dispersion treatment 3h, obtain dispersion liquid; Then add 25mL mass concentration to the dispersion liquid obtained above respectively 1.5mol / L magnesium nitrate solution and 20mL aluminum nitrate solution with a mass concentration of 1.2mol / L, after stirring and mixing at 260r / min, 12mL of acetone was added dropwise to it, and ultrasonic dispersion treatment was performed for 2 hours, and then 15g of After mixing cerium acetylacetonate, shake it in a shaker for 3 hours; after shaking it, add 15 mL of ammonia water with a mass fraction of 17% to the sh...

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Abstract

The invention discloses a preparation method of a magnesium and aluminum doped mesoporous hollow sphere ceria-based oxygen storage material and belongs to the technical field of oxygen storage material preparation. The method includes: weighing sodium silicate and water, dropwise adding hydrochloric acid solution, performing ultrasonic dispersion to obtain dispersion liquid, adding magnesium nitrate solution, aluminium nitrate solution, acetone and acetylacetone cerium, enabling the matters to be loaded to the surface of orthosilicic acid sediment under the action of ammonia water titration, performing calcination under nitrogen atmosphere after dehydration, washing with ethyl alcohol, sodium hydroxide solution and deionized water, and filtering to obtain filter residue prior to activation to prepare the magnesium and aluminum doped mesoporous hollow sphere ceria-based oxygen storage material. The preparation method has the advantages that the preparation steps are simple, specific surface area is increased effectively, and oxygen storage capacity is increased by 22-26%; the obtained produce is of a spatial stereostructure, and under the condition of over 1123K, sintering is avoided, and the oxygen storage capacity and the specific surface area are unchanged.

Description

technical field [0001] The invention relates to a preparation method of a cerium-based oxygen storage material doped with magnesium and aluminum mesoporous hollow microspheres, and belongs to the technical field of preparation of oxygen storage materials. Background technique [0002] Oxygen storage materials, powders, have different colors depending on the elements contained, mainly yellow, brown, etc.; binary or multi-component composite oxides composed of rare earth elements, alkaline earth metal elements or transition metal elements mainly composed of cerium oxide . The composition of the first-generation cerium-based oxygen storage materials is pure CeO 2 , its main feature is that the oxygen storage performance depends on the specific surface area, the thermal stability is poor, and the specific surface area decreases rapidly after aging above 850 ° C, thus losing the oxygen storage performance; the composition of the second-generation cerium-based oxygen storage mate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00B01J23/10B01J35/10
CPCB01J23/10B01J35/1014B01J35/1038C01F17/32C01P2006/12C01P2006/14
Inventor 黄加斗
Owner CHONGQING TONGHUI GAS
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