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Preparation method and application of a hollow core-shell structure metal-organic framework material

An organic framework and shell structure technology, applied in the field of materials, can solve the problems of long time, complicated preparation process, and harsh template removal processing conditions, and achieve the effect of simple preparation process, stable precious metal nanoparticles, and synergistically enhancing high-efficiency catalysis.

Active Publication Date: 2021-08-24
ANHUI AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Recently, researchers in the world have used the hard template method to prepare hollow core-shell structure metal-organic framework materials, but the preparation process of this method is complicated, time-consuming and the conditions for template removal are harsh.
Therefore, it is still a great challenge to develop a facile and effective method to synthesize functional materials based on metal-organic framework hollow core-shell structures.

Method used

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  • Preparation method and application of a hollow core-shell structure metal-organic framework material
  • Preparation method and application of a hollow core-shell structure metal-organic framework material
  • Preparation method and application of a hollow core-shell structure metal-organic framework material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Example 1: One-step preparation of hollow core-shell functional materials (Au@Zn / Ni-MOF-2 nanocubes)

[0048] Weigh 25 mg of zinc nitrate hexahydrate, 37 mg of nickel acetylacetonate, 12 mg of terephthalic acid and 1.36 g of PVP and dissolve in 25.6 mL of DMF-DMAC-EtOH (volume ratio=5:5:6). After fully dissolved, add 400 μL HAuCl with stirring 4 4H 2 O (0.02g mL -1 ), the resulting mixture was transferred to a 50 mL autoclave, and reacted at 150 °C for 4 h. Cool to room temperature, centrifuge at 10,000 rpm for 5 minutes to collect the product, wash with ethanol, and dry overnight at 70° C. under vacuum.

[0049] pass figure 2 The morphology and microstructure of the hollow core-shell structured Au@Zn / Ni-MOF-2 can be clearly revealed, which has a well-defined cubic structure with a size of about 500 nm, a very rough surface, and consists of a large number of nanosheets. It can be clearly seen that there is a hollow structure in each core-shell nanocube structure, ...

Embodiment 2

[0058] Example 2: One-step preparation of a hollow core-shell functional material (AgPd@Zn / Ni-MOF-2 nanocube)

[0059] Weigh 25 mg of zinc nitrate hexahydrate, 37 mg of nickel acetylacetonate, 12 mg of terephthalic acid, 1.36 g of PVP, and 1.44 mg of silver nitrate and dissolve in 25.6 mL of DMF-DMAC-EtOH (volume ratio=5:5:6). After fully dissolved, add 75 μL PdCl under stirring 2 solution, the resulting mixture was transferred to a 50 mL stainless steel autoclave, and reacted at 150 °C for 4 h. Cool to room temperature, centrifuge at 10,000 rpm for 5 minutes to collect the product, wash with ethanol, and dry overnight at 70° C. under vacuum.

[0060] pass Figure 7 The morphology and microstructure of the hollow core-shell structure AgPd@Zn / Ni-MOF-2 can be clearly revealed, with a clear cubic structure and each cavity with a size of 500nm, and it is obvious that the cavity contains AgPd alloy nanoparticles.

Embodiment 3

[0061] Example 3: Application of Hollow Core-Shell Structured Functional Materials in Catalytic Alcohol Oxidation Reaction

[0062] In the alcohol catalytic oxidation reaction, the catalytic oxidation of benzyl alcohol to benzaldehyde was first selected to test the efficiency of the hollow core-shell structure catalyst synthesized in implementation 1. Into a 50 mL round bottom flask was added 15 mg of the material synthesized in Example 1 dissolved in 6 mL of toluene solution, followed by the addition of 0.2 mmol of benzyl alcohol. The reaction mixture was stirred at 95°C for the required time. After the reaction, the catalyst particles in the solution were recovered by centrifugation. Conversion and selectivity were determined by GC and characterized by GC-MS.

[0063] For the recyclability test, the catalyst was recovered from the solution by centrifugation, washed with ethanol, dried at 70 °C, and then subjected to the next cycle of catalysis under the same reaction condi...

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Abstract

The invention discloses a preparation method and application of a metal-organic framework material with a hollow core-shell structure, and belongs to the field of material technology. The present invention provides a simple, efficient, template-free one-step synthesis method to prepare hollow core-shell structure metal-organic framework nanomaterials, wherein the noble metal element or noble metal alloy is the core, and the porous hollow metal-organic framework is the shell. The principle of the invention is based on the rare self-transformation process of the crystal structure at the molecular level from a solid core-shell structure to a hollow core-shell structure performance. The material of the present invention combines the strong catalytic activity of traditional noble metal nanoparticles with novel The unique advantages of porous hollow metal-organic frameworks can achieve synergistic enhancement. The noble metal nanoparticles and porous hollow metal-organic framework core-shell functional material of the present invention can be used as a catalyst with super-catalytic activity and applied to highly selective heterogeneous catalytic reactions and hydrogen production reactions.

Description

technical field [0001] The invention relates to a preparation method and application of a metal-organic framework material with a hollow core-shell structure, and belongs to the field of material technology. Background technique [0002] Metal-organic frameworks (MOFs) are an attractive class of porous crystalline materials with tunable pore structures and well-defined physicochemical properties. Due to the diversity of multidentate organic ligands and the richness of inorganic metal ions or clusters as coordination nodes, the microstructure of metal-organic frameworks can be designed and constructed according to the target performance needs. These unique superior properties make them promising for a wide range of industrial applications, such as sensing, adsorption and separation, drug delivery, and catalysis, etc. In recent years, hollow metal-organic framework functional materials with complex nanostructures have attracted extensive research interest among researchers. C...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00B01J31/22B01J35/10B01J37/10C07C45/29C07C47/54C01B3/04
CPCB01J31/1691B01J31/2239B01J35/008B01J35/1009B01J35/1014B01J35/1019B01J35/1023B01J35/1028B01J37/10B01J2531/26B01J2531/847C01B3/042C07C45/29C08G83/008C07C47/54Y02E60/36
Inventor 柯飞秦念巧潘安袁军朱婧张春艳
Owner ANHUI AGRICULTURAL UNIVERSITY
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