Method for preparing rare-earth transition metal composite oxide porous hollow spheres

A composite oxide, transition metal technology, applied in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, cobalt oxide/cobalt hydroxide, etc., can solve the problem of limited types of MOF materials, high price, synthesis The problems of complex and limited process, to achieve the effect of low cost of raw materials, low cost of raw materials, and excellent catalytic performance

Inactive Publication Date: 2019-01-08
CHINA UNIV OF MINING & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the high price of organic ligands, the limited types of MOF materials suitable for rare earth metals, and the complexity of the synthesis process, this synthesis method has great limitations in industrial applications.

Method used

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  • Method for preparing rare-earth transition metal composite oxide porous hollow spheres
  • Method for preparing rare-earth transition metal composite oxide porous hollow spheres
  • Method for preparing rare-earth transition metal composite oxide porous hollow spheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039](1) According to the molar concentration of total metal ions of 12mmol / L, wherein the molar ratio of Cu:Ce is 3:17, respectively weigh 0.157g of copper nitrate trihydrate and 1.594g of cerium nitrate hexahydrate, fully dissolve in 360mL of isopropanol and Mixed solution of glycerol (glycerol: isopropanol volume ratio 1:3), transferred to a reaction kettle, reacted at 180°C for 16h, cooled naturally to room temperature, centrifuged, washed with ethanol, and dried in vacuum to obtain Copper cerium metal alkoxide solid pellets;

[0040] (2) Put the porcelain boat with the above-mentioned alkoxide precursor in a muffle furnace, heat treatment in the air atmosphere, set the heating rate to 3°C / min, program the temperature to 450°C, and keep it for 2h to synthesize copper-cerium composite metal oxide Hollow ball;

[0041] The transmission electron microscope TEM picture ( figure 1 ) shows that the composite oxide is a hollow spherical structure with a diameter of about 600nm...

Embodiment 2

[0045] (1) According to the molar concentration of total metal ions of 10mmol / L, wherein the molar ratio of Mn:Co:Ce is 1:1:4, respectively weigh 0.151g of manganese nitrate tetrahydrate, 0.175g of cobalt nitrate hexahydrate and cerium nitrate hexahydrate 1.042g, fully dissolved in 360mL of a mixed solution of isopropanol and glycerol (glycerol: isopropanol volume ratio 1:5), transferred to a reaction kettle, reacted at 180°C for 10h, cooled naturally to room temperature , centrifuged, washed with acetone, and vacuum-dried to obtain solid pellets of cerium cobalt manganese alkoxide.

[0046] (2) Put the porcelain boat with the above-mentioned alkoxide precursor in a muffle furnace, heat treatment in an air atmosphere, set the heating rate at 5°C / min, program the temperature to 300°C, and keep it for 4h to synthesize cerium-cobalt-manganese composite metal oxide hollow spheres.

[0047] The transmission electron microscope TEM picture ( image 3 a) shows that the composite ox...

Embodiment 3

[0050] (1) According to the molar concentration of total metal ions of 8mmol / L, wherein the molar ratio of Zn:Co:Ce is 2:2:3, weigh 0.244g of zinc nitrate hexahydrate, 0.239g of cobalt nitrate hexahydrate and 0.536g of cerium nitrate hexahydrate g, fully dissolved in 360 mL of a mixed solution of isopropanol and glycerol (glycerol: isopropanol volume ratio 1:7), transferred to a reaction kettle, reacted at 190°C for 6 hours, cooled naturally to room temperature, Centrifuge, wash with ethanol, and vacuum dry to obtain solid pellets of cerium-cobalt-zinc metal alkoxide.

[0051] (2) Put the porcelain boat with the above-mentioned alkoxide precursor in a muffle furnace, heat-treat in an air atmosphere, set the heating rate at 10°C / min, program the temperature to 500°C, and keep it for 1h to synthesize cerium-cobalt-zinc composite metal oxide hollow spheres.

[0052] The transmission electron microscope TEM picture ( Figure 5 ) shows that the composite oxide is a hollow spheric...

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Abstract

The invention discloses a method for preparing rare-earth transition metal composite oxide porous hollow spheres and belongs to the field of inorganic nanometer materials and heterogeneous catalysis.The method comprises the following steps: 1, dissolving a rare-earth metal source and a transition metal source in a polyol medium, and synthesizing a solid spherical alkoxide precursor with excellentdispersion by adopting a solvothermal method; and 2, performing heat treatment on the precursor under specific conditions, and synthesizing the rare-earth transition metal composite oxide porous hollow spheres based on an unbalanced heat treatment method. The method disclosed by the invention has the advantages that the raw material price is low, the hollow structure material is directly obtained, and the prepared rare-earth transition metal composite oxide porous hollow spheres have the advantages of being uniform in metal element dispersion, controllable in composition and size, capable ofrealizing porous distribution of the shell layer and controllable in thickness; and when the hollow spheres are applied to a catalytic reaction, the contact area between the substrate molecule and catalytic active sites can be greatly enlarged, the interface synergy among different components of the rare-earth transition metal oxides contributes to transmission of reactive oxygen species at the heterogenous interface and transfer of electrons, and the activity of the catalytic oxidation reaction is obviously improved.

Description

technical field [0001] The invention relates to the field of inorganic nanometer materials and heterogeneous catalysis, in particular to a method for preparing rare earth-transition metal composite oxide porous hollow spheres. Background technique [0002] Transition metal oxides and rare earth metal oxides have become the focus of catalyst research due to their advantages of low price, high reducibility and good thermal stability. As a typical structure, hollow nanospheres are widely used in catalysis, separation, Adsorption and other fields have been widely used. [0003] At present, the synthesis methods of hollow structures mainly include hard template method, soft template method and self-template method. Hollow structural materials of different types and shapes can be prepared by using the hard template method, but it is difficult to remove the template, which leads to the collapse and damage of the product structure to a certain extent. Although the template is eas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/04C01G3/02B01J23/83B01J23/889B82Y40/00B82Y30/00
CPCC01G3/02B01J23/002B01J23/83B01J23/8892B01J2523/00B82Y30/00B82Y40/00C01G51/04C01P2002/85C01P2004/03C01P2004/04C01P2004/34C01P2004/62C01P2004/64C01P2004/82B01J2523/27B01J2523/3712B01J2523/845B01J2523/72
Inventor 刘玲康建宏康国俊王瑞玉王全德刘滋武
Owner CHINA UNIV OF MINING & TECH
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