Mesoporous cerium dioxide hollow spheres or mesoporous cerium dioxide/carbon composite material hollow spheres and preparation method thereof

A technology of carbon composite material and cerium oxide, which is applied in the direction of rare earth metal oxide/hydroxide, metal/metal oxide/metal hydroxide catalyst, chemical instrument and method, etc., can solve complex operation, polluted environment, Long reaction time and other problems, to solve the effect of complex raw materials, large specific surface area and short reaction time

Inactive Publication Date: 2017-05-10
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, Ma Jingjing and others used hexamethylenetetramine, citric acid, water, and cerium nitrate as raw materials to prepare double-layer CeO 2 Hollow microspheres; such as Gao Lian et al prepared CeO with oleic acid, cerium nitrate, toluene, water, etc. 2 Hollow nano-cube; ordinary hydrothermal reaction process needs to add surfactants, alkaline substances or organic solvents, which pollutes the environment, takes a long time to react, and is complicated to operate
[0006] At present, there is no direct synthesis of nano-CeO with different sizes, different wall thicknesses, and good dispersion in the absence of alkaline substances and surfactants. 2 Related reports on hollow spherical powder

Method used

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  • Mesoporous cerium dioxide hollow spheres or mesoporous cerium dioxide/carbon composite material hollow spheres and preparation method thereof
  • Mesoporous cerium dioxide hollow spheres or mesoporous cerium dioxide/carbon composite material hollow spheres and preparation method thereof
  • Mesoporous cerium dioxide hollow spheres or mesoporous cerium dioxide/carbon composite material hollow spheres and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0037] 1) Using cerium nitrate hexahydrate and citric acid monohydrate as raw materials, according to the ratio of the amount of substances of 1:0.1, make an aqueous solution with a concentration of 0.5mol / L, and stir magnetically for 3 hours at room temperature, and fully mix;

[0038] 2) Put the mixed solution into a microwave reaction bottle, react at 200°C for 2 minutes, after the reaction is completed, cool down to room temperature, perform suction filtration, wash with distilled water for 3 times, and then put the washed sample in a drying oven at 80°C for 8 hours , to obtain a hollow spherical ceria precursor;

[0039] 3) Place the dried hollow spherical ceria precursor in a tube furnace. Under an air atmosphere, start from room temperature and raise the temperature to 280°C at a rate of 2°C / min. The furnace was cooled to room temperature to obtain mesoporous ceria hollow sphere powder.

[0040] The CeO prepared by microwave hydrothermal in this example 2 The appearan...

Embodiment 2

[0042] 1) Using cerium nitrate hexahydrate and citric acid monohydrate as raw materials, according to the ratio of the amount of substances of 1:0.5, make an aqueous solution with a concentration of 0.1mol / L, stir magnetically for 4 hours at room temperature, and fully mix;

[0043] 2) Put the mixed solution into a microwave reaction bottle, react at 170°C for 2min, after the reaction is completed, cool down to room temperature, perform suction filtration, wash with distilled water for 3 times, and then put the washed sample in a drying oven at 80°C for 20h , to obtain a hollow spherical ceria precursor;

[0044] 3) Place the dried hollow spherical ceria precursor in a tube furnace, raise the temperature up to 300°C at a rate of 0.5°C / min in an air atmosphere, keep it warm for 1 hour, and cool it down to room temperature with the furnace after the heat preservation is over. The mesoporous ceria hollow sphere powder is obtained.

[0045] The CeO prepared by microwave hydrother...

Embodiment 3

[0047] 1) Using cerium nitrate hexahydrate and citric acid monohydrate as raw materials, according to the ratio of the amount of substances of 1:0.7, make an aqueous solution with a concentration of 0.1mol / L, and stir magnetically for 2 hours at room temperature, and fully mix;

[0048] 2) Put the mixed solution into a microwave reaction bottle, react at 150°C for 2 minutes, after the reaction is completed, cool down to room temperature, perform suction filtration, wash with distilled water for 3 times, and then put the washed sample in a drying oven at 80°C for 12 hours , to obtain a hollow spherical ceria precursor;

[0049] 3) Place the dried hollow spherical ceria precursor in a tube furnace, raise the temperature up to 600°C at a rate of 2°C / min in an Ar atmosphere, keep it for 1 hour, and cool it down to room temperature with the furnace after the hold. Obtain mesoporous ceria / carbon composite hollow spheres.

[0050] The CeO prepared by microwave hydrothermal in this e...

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Abstract

The invention discloses mesoporous cerium dioxide hollow spheres or mesoporous cerium dioxide / carbon composite material hollow spheres and a preparation method thereof. The preparation method comprises the following steps: 1) dissolving one cerium salt and one organic acid into distilled water according to a certain ratio of amount of the substances, so as to prepare a mixed solution; 2) putting the mixed solution in a microwave hydrothermograph for reaction for a period of time at certain temperature; after finishing the reaction, performing suction filtration and washing; drying at 80 DEG C to obtain a hollow sphere type cerium dioxide precursor; 3) carrying out heat treatment on the dried precursor in an atmosphere at certain temperature and keeping heat for a period of time to obtain mesoporous cerium dioxide hollow sphere or cerium dioxide / carbon hollow sphere powder. The mesoporous cerium dioxide ( / carbon) hollow sphere powder prepared by the method has the characteristics of controllable phase composition, controllable sphere diameter and controllable wall thickness. Meanwhile, the method has the advantages of low cost, simple preparation process, high efficiency and easiness in control.

Description

[0001] 【Technical field】 [0002] The invention belongs to the technical field of new materials, and in particular relates to a mesoporous ceria hollow sphere or a mesoporous ceria / carbon composite hollow sphere and a preparation method thereof. [0003] 【Background technique】 [0004] CeO 2 It is a cheap rare earth material, which has good structural stability and catalytic performance, and strong oxidation-reduction performance. [0005] Currently, cerium oxide hollow spheres (CeO 2 ) There are two commonly used methods: one is the template method. For example, Zhang Xiyu and others prepared CeO with yeast, ceric sulfate, sodium hydroxide, ethanol, acid orange and other reagents. 2 Hollow microspheres; Li Yadong et al. made polysaccharide microspheres from glucose, using this as a template and cerium nitrate as a reagent, and obtained CeO by calcination. 2 Nano hollow spheres; Jiang Xueliang and others used styrene, methyl methacrylate, polyvinyl pyrrolidone, water, metha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/10B01J35/08C01F17/00
CPCB01J23/10B01J35/08C01P2004/34C01P2004/03C01P2002/82C01P2006/14C01P2004/62C01P2006/17C01F17/206
Inventor 杜显锋马明波徐友龙王红洁
Owner XI AN JIAOTONG UNIV
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