Preparation method and application of metal-organic framework material with hollow core-shell structure
An organic framework and shell structure technology, applied in the field of materials, can solve the problems of harsh template removal treatment conditions, long time-consuming, complicated preparation process, etc., and achieve the effect of easy and fast delivery, simple preparation process, and stable noble metal nanoparticles
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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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