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Preparation method and application of photocatalyst material with magnetic core-shell structure

A photocatalyst, core-shell technology, applied in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve pollution, low catalyst recycling efficiency, and energy consumption big problem

Active Publication Date: 2021-05-18
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most organic coupling reactions are completed by heating and using palladium as a catalyst, but it has the disadvantages of low catalyst recycling efficiency, serious pollution, and large energy consumption.

Method used

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  • Preparation method and application of photocatalyst material with magnetic core-shell structure
  • Preparation method and application of photocatalyst material with magnetic core-shell structure
  • Preparation method and application of photocatalyst material with magnetic core-shell structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1.0g of magnetic Fe 3 o 4 @SiO 2 The composite nanoparticles were suspended in 20 mL of anhydrous methanol solvent. After ultrasonication for 20 min, 0.1 g of organic ligand 1,10-phenanthroline-2,9-dicarboxylate potassium (phenCOOK) was added, and then the mixture was Reflux for 12 h, cool to room temperature, centrifuge to separate the precipitate, wash with anhydrous methanol three times, and dry in vacuum to obtain magnetic Fe containing phenCOO 3 o 4 @SiO 2 composite nanoparticles.

[0028] 1.0 g of magnetic Fe containing phenCOO 3 o 4 @SiO 2 Disperse the composite nanoparticles into 20mL of dry methanol, then slowly add 10mL of 0.01g / mL palladium acetate methanol solution dropwise, the mixture was refluxed under nitrogen atmosphere for 12h, cooled to room temperature, centrifuged to separate the precipitate, washed three times with anhydrous methanol , dried under vacuum to obtain magnetic Fe containing Pd-phenCOO 3 o 4 @SiO 2 Composite nanoparticles, ab...

Embodiment 2

[0030] 1.0g of magnetic Fe 3 o 4 @SiO 2 The composite nanoparticles were suspended in 30 mL of anhydrous ethanol solvent. After ultrasonication for 30 min, 0.1 g of organic ligand 1,10-phenanthroline-2,9-dicarboxylate potassium (phenCOOK) was added, and the mixture was heated under a nitrogen atmosphere. Reflux for 8h, cool to room temperature, centrifuge to separate the precipitate, wash with absolute ethanol three times, and dry in vacuum to obtain magnetic Fe containing phenCOO 3 o 4 @SiO 2 composite nanoparticles.

[0031] 1.0 g of magnetic Fe containing phenCOO 3 o 4 @SiO 2Disperse the composite nanoparticles into 30mL of dry ethanol, then slowly add 15mL of 0.01g / mL palladium dichloride ethanol solution dropwise, the mixture was refluxed under nitrogen atmosphere for 8h, cooled to room temperature, centrifuged to separate the precipitate, and washed with absolute ethanol After three times, vacuum drying yielded magnetic Fe containing Pd-phenCOO 3 o 4 @SiO 2 Co...

Embodiment 3

[0033] 1.0g of magnetic Fe 3 o 4 @SiO 2 The composite nanoparticles were suspended in 30 mL of anhydrous methanol solvent. After ultrasonication for 30 min, 0.1 g of organic ligand 1,10-phenanthroline-2,9-dicarboxylate potassium (phenCOOK) was added, and then the mixture was Reflux for 6 h, cool to room temperature, centrifuge to separate the precipitate, wash with anhydrous methanol three times, and dry in vacuum to obtain magnetic Fe containing phenCOO 3 o 4 @SiO 2 composite nanoparticles.

[0034] 1.0 g of magnetic Fe containing phenCOO 3 o 4 @SiO 2 Disperse the composite nanoparticles into 20mL of dry methanol, then slowly add 20mL of 0.01g / mL palladium nitrate methanol solution dropwise, the mixture was refluxed under nitrogen atmosphere for 6h, cooled to room temperature, centrifuged to separate the precipitate, washed three times with anhydrous methanol , dried under vacuum to obtain magnetic Fe containing Pd-phenCOO 3 o 4 @SiO 2 Composite nanoparticles, abbr...

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Abstract

The invention discloses a preparation method and application of a photocatalyst material with a magnetic core-shell structure. According to the invention, with magnetic Fe3O4@SiO2 composite nanoparticles, an organic ligand 1,10-phenanthroline-2,9-potassium dicarboxylate and palladium salt as raw materials, a photocatalyst material with a magnetic core-shell structure is prepared through a self-assembly reaction in a solution, and the material as an organic coupling reaction catalyst is high in catalytic efficiency, stable in structure and capable of being recycled for multiple times. The preparation process is safe and easy to operate, high in production efficiency, low in equipment investment and suitable for batch production.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic nanometer materials, and in particular relates to a preparation method and application of a photocatalyst material with a magnetic core-shell structure. Background technique [0002] The Suzuki reaction, also known as the Suzuki-Miyaura coupling reaction, is an organic coupling reaction in which aryl or alkenyl boronic acids or borates are cross-coupled with halogenated aromatic hydrocarbons or alkenes under the catalysis of palladium complexes. This reaction was first reported by Akira Suzuki in 1979. It is widely used in organic synthesis, has strong substrate adaptability and functional group tolerance, and is often used to synthesize derivatives of polyenes, styrene and biphenyl, thus widely It is an important organic synthesis reaction used in the synthesis of many natural products, drugs, and organic materials. At present, most organic coupling reactions are completed by he...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J31/28B01J35/00B01J35/08C07C1/32C07C15/14
CPCB01J31/2217B01J31/28C07C1/321B01J2231/4211B01J2531/824B01J35/33B01J35/51B01J35/39C07C15/14Y02P20/584
Inventor 李星孙嘉蔚
Owner NINGBO UNIV
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