Multi-shell-layer hollow-core-shell cubic structure type M1.8M'1.2O4@CeO2 composite material and preparation method thereof

An M1.8M, cubic structure technology, applied in chemical instruments and methods, catalyst activation/preparation, metal/metal oxide/metal hydroxide catalysts, etc. It can solve the problems of mass transfer and diffusion of chemical reaction molecules, and limit the practical application in the field of catalysis, so as to achieve the effect of simple and controllable synthesis method, improved diffusion speed and uniform size.

Active Publication Date: 2019-02-22
CHINA UNIV OF MINING & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when surfactant-based micelles, reverse micelles, and microemulsion droplets are used as soft templates, in order to minimize the surface energy, they usually tend to form spherical structures, so they are not suitable for non-spherical nanostructures (especially polyhedral structure) formation
Even the preparation of non-spherical nanostructures using the hard template method still has certain difficulties, such as how to coat a uniform shell on the surface of the template with a large curvature change
Because non-spherical templates may have different crystal faces, and different crystal face...

Method used

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  • Multi-shell-layer hollow-core-shell cubic structure type M1.8M'1.2O4@CeO2 composite material and preparation method thereof
  • Multi-shell-layer hollow-core-shell cubic structure type M1.8M'1.2O4@CeO2 composite material and preparation method thereof
  • Multi-shell-layer hollow-core-shell cubic structure type M1.8M'1.2O4@CeO2 composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A kind of Mn with multi-shell hollow core-shell cubic structure 1.8 co 1.2 o 4 / CeO 2 The preparation method of composite materials, the technological process is as follows figure 1 shown, including the following steps:

[0035] (1) Synthesis of Prussian blue-like MnCo-PBAs cubic structure:

[0036] Weigh 0.245g (1mmol) of manganese acetate tetrahydrate and 1.5g of polyvinylpyrrolidone, dissolve them in 90mL ethanol-water mixed solution (ethanol:water=2:1, V / V) to form solution A; weigh K 3 [Co(CN) 6 ] 0.166 g (0.5 mmol) was dissolved in 60 mL deionized water to form solution B, and solution B was added dropwise to solution A under magnetic stirring, and after continuous stirring for 30 min, aged at room temperature for 24 h; centrifuged, washed, and dried to obtain the scale Uniform Mn 3 [Co(CN) 6 ] 2 (MnCo-PBA) cubic structure material;

[0037] (2) Mn 1.8 co 1.2 o 4 Synthesis of a single-shell hollow cubic structure:

[0038] Put the porcelain boat with...

Embodiment 2

[0045] Prussian blue-like MnCo-PBAs cubic structure, Mn 1.8 co 1.2 o 4 Egg yolk-eggshell hollow cubic structure and CeO 2 The synthesis steps of the assembly of the shell are the same as in Example 1. The difference is that in Mn 1.8 co 1.2 o 4 During the synthesis process of the egg yolk-eggshell hollow cube structure, the heating rate of the muffle furnace was set at 10°C / min, the reaction temperature was 300°C, and the holding time was 4h; 2 During the shell assembly process, 0.5 g of cerium nitrate was added, and the reaction was refluxed at 80° C. for 2.5 h.

[0046] The transmission electron microscope TEM picture ( Figure 4 ) shows that Mn 1.8 co 1.2 o 4 @CeO 2 The composite oxide has an egg yolk-eggshell hollow cubic structure, the outside is a hollow cubic box, and the center is a solid cube. The average size of the egg yolk-eggshell hollow cubic structure is 500-600 nm, and the surface is uniformly covered with nanocrystalline particles. CeO 2 Shell, Ce...

Embodiment 3

[0049] Prussian blue-like MnCo-PBAs cubic structure, Mn 1.8 co 1.2 o 4 Double-shelled hollow cubic structure and CeO 2 The synthesis steps of the assembly of the shell are the same as in Example 1. The difference is that in Mn 1.8 co 1.2 o 4 During the synthesis process of the double-shell hollow cubic structure, the heating rate was set at 25°C / min, the reaction temperature was 600°C, and the holding time was 0.5h; 2 During shell assembly, 0.75 g of cerium nitrate and 1.5 g of urea were added, ultrasonicated for 40 min, and refluxed at 80°C for 3 h.

[0050] The transmission electron microscope TEM picture ( Figure 6 ) shows that Mn 1.8 co 1.2 o 4 @CeO 2 The composite oxide is a double-shell hollow cubic structure with a size of 500-600nm, and the surface is coated with CeO composed of nanocrystalline grains. 2 Shell, CeO 2 The shell thickness is 30-50nm.

[0051] Catalytic performance is the same as embodiment 1, and test result shows, the temperature (T 100 ...

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Abstract

The invention discloses a multi-shell-layer hollow-core-shell cubic structure type M1.8M'1.2O4@CeO2 composite material and a preparation method thereof. The preparation method comprises the steps of firstly synthesizing a uniformly dispersed Prussian blue-similar metal organic framework material MM'-PBAs cubic structure, roasting MM'-PBAs at a high temperature under a specific condition so as to obtain a multi-shell-layer transition metal multiple oxide M1.8M'1.2O4 hollow cubic box based on an unbalanced thermal treatment method, and assembling a thickness-controllable CeO2 shell layer formedby nanometer crystals to the surface of M1.8M'1.2O4, so as to obtain the M1.8M'1.2O4@CeO2 core-shell cubic box. The process is simple, mild in condition and high in yield, a multi-shell-layer hollow structure material is directly obtained without use of a template or additional cavitation; the prepared material has a hollow structure and is large in specific surface area, meanwhile, the internal space can be effectively utilized by virtue of the multi-layer hollow structure, the contact area between substrate molecules and the material is increased, and more active sites are exposed, so that the catalytic oxidation performance is excellent.

Description

technical field [0001] The invention belongs to the field of inorganic nanomaterials and heterogeneous catalysis, and relates to a rare earth-transition metal composite oxide, in particular to a multi-shell hollow core-shell cubic structure M 1.8 M' 1.2 o 4 @CeO 2 Composite materials and methods for their preparation. Background technique [0002] The application of metal oxide materials in the fields of catalysis, sensing, and energy storage is directly related to the structure of the material. As a typical structure, the nano- or micro-scale multi-shell hollow structure has the characteristics of low density, large specific surface area, hollow structure, and multi-shell composed of nanoparticles, so it is widely used in fields related to surface properties. . [0003] At present, there are few reports on the preparation of metal oxides with multi-shell non-spherical hollow structures, especially rare earth-transition metal composite oxides. According to the existing...

Claims

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Application Information

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IPC IPC(8): B01J23/889B01J35/10
CPCB01J23/002B01J23/8892B01J35/0073B01J35/1004B01J37/0018B01J2523/00B01J2523/3712B01J2523/72B01J2523/845B01J2523/847
Inventor 刘玲康建宏王瑞玉王全德刘滋武康国俊陈浮
Owner CHINA UNIV OF MINING & TECH
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