Montmorillonite-loaded nano Pd/Cu catalyst and in-situ one-pot preparation and application thereof

A montmorillonite and catalyst technology, applied in the field of catalysts, can solve problems such as difficulties, and achieve the effects of less catalyst consumption, green reaction system, and simple preparation and post-processing steps

Inactive Publication Date: 2014-06-25
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although various studies have shown that bimetallic nanoparticles with controllable size, shape and composition have greater advantages in terms of catalytic activity, the preparation of nanoparticles with the above various characteristics, especially Pd-based bimetallic nanoparticles, is a challenge for researchers. still challenging
The commonly used hydrothermal me...

Method used

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  • Montmorillonite-loaded nano Pd/Cu catalyst and in-situ one-pot preparation and application thereof
  • Montmorillonite-loaded nano Pd/Cu catalyst and in-situ one-pot preparation and application thereof
  • Montmorillonite-loaded nano Pd/Cu catalyst and in-situ one-pot preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 1.0g of calcium-based montmorillonite, 0.0170g (0.07mmol) of palladium acetate, 0.0136g (0.07mmol) of copper nitrate, and 9.6g (12mL) of absolute ethanol into a 30mL hydrothermal kettle, stir well and ultrasonically for 1 hour, seal the water Heat the kettle, heat to 170°C for 16 hours, then naturally cool to room temperature, wash with absolute ethanol, centrifuge, and vacuum-dry the obtained solid at room temperature to obtain a montmorillonite-supported nano-Pd / Cu catalyst.

[0016] Gained catalysts were characterized by environmental scanning electron microscopy, transmission electron microscopy, and X-ray powder diffraction. The results are shown in Figure 1~4 . It can be seen from the figure that the Pd / Cu bimetallic was successfully supported on the montmorillonite, and nanoparticles were formed, and the layered structure of the montmorillonite remained intact.

Embodiment 2

[0018] Add 1.0g of calcium-based montmorillonite, 0.0233g (0.1mmol) of palladium acetate, 0.0192g (0.1mmol) of copper nitrate, and 11.3g (15mL) of absolute ethanol into a 30mL hydrothermal kettle, stir well and ultrasonically for 2 hours, seal the water Heat the kettle, heat to 150°C for 24 hours, then naturally cool to room temperature, wash with absolute ethanol, centrifuge, and vacuum-dry the obtained solid at room temperature to obtain a montmorillonite-supported nano-Pd / Cu catalyst.

Embodiment 3

[0020] The application of the montmorillonite-loaded nano-Pd / Cu catalyst prepared in Example 1 in the Sonogashira cross-coupling reaction of catalyzed iodoarenes and terminal alkynes, the specific method is as follows:

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Abstract

The invention discloses a montmorillonite-loaded nano Pd/Cu catalyst and in-situ one-pot preparation and application thereof. The catalyst is prepared by taking montmorillonite as a carrier by taking absolute ethyl alcohol as a solvent and a reducing agent, and by adopting an in-situ one-pot method in one step under solvothermal conditions. The preparation and after-treatment of the catalyst are simple in steps, any surfactant is not needed to be added, the reaction system is green and environment-friendly, the problem that bimetallic nanoparticles are difficultly obtained in a solvent system is solved, and the shape, size and metal ratio of the catalyst are effectively controlled. The prepared catalyst can be used for efficiently catalyzing a Sonogashira cross-coupling reaction of aryl iodides and aryl terminal alkyne or alkyl terminal alkyne under a mild condition, the amount of the catalyst is small, the yield of the target product is high, and the catalyst can be applied to construction of Csp-Csp2 bond structures.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to an in-situ preparation method of montmorillonite-loaded nanoparticles, and relates to the application of the catalyst obtained by the method in catalyzing Sonogashira cross-coupling reactions. Background technique [0002] Bimetallic nanoparticles have attracted great interest for their wide applications in catalysis, electricity, magnetism, and optics. Among them, Pd-containing bimetallic nanoparticles have attracted extensive attention in catalyzing organic reactions due to their excellent catalytic properties. Since the 1990s, various Pd-containing bimetallic nanoparticles have emerged and been applied in many fields of catalytic reactions. However, although various studies have shown that bimetallic nanoparticles with controllable size, shape and composition have greater advantages in terms of catalytic activity, the preparation of nanoparticles with the above ...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07B37/04C07C15/54C07C2/88C07C43/215C07C41/30C07C22/08C07C17/266C07C205/06C07C201/12
Inventor 高子伟徐伟于波孙元龙张莹王振华陈禧杨金斗张伟强
Owner SHAANXI NORMAL UNIV
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