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Supported palladium catalyst and preparation method and application thereof

A technology of supported palladium and catalyst, applied in the field of nanomaterials

Inactive Publication Date: 2015-01-28
SUZHOU INSTITUE OF WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the temperature of the liquid phase method is very high (above 160 ° C), which also limits the application of palladium nanocatalysts.
Moreover, the wet chemical method including the liquid phase synthesis method needs to introduce stabilizer macromolecules during the synthesis process, because the stabilizer macromolecules can be firmly adsorbed on the surface of the prepared nanoparticles to poison them, which seriously restricts its practical application. and improved catalytic performance

Method used

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  • Supported palladium catalyst and preparation method and application thereof
  • Supported palladium catalyst and preparation method and application thereof
  • Supported palladium catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] For the synthesis of palladium nanorods, 0.1 mmol of palladium acetylacetonate was dissolved in 10 mL of oleylamine, and 0.5 mmol of N,N-diethylaniline borane was injected, and the solution obviously changed from colorless to brown-black. The temperature of the solution was adjusted to 90° C. and reduced for 30 minutes. After the temperature dropped to room temperature, ethanol was added to settle the nanoparticles, and the nanoparticles were obtained by centrifugation. Then, the nanoparticles were washed successively with distilled water and ethanol, and dried to obtain brown-black powder (palladium nanocrystals). Take 8 mg of the powder and disperse it in 10 mL of n-hexane, add 72 mg of graphene, load at room temperature, and finally centrifuge and dry to obtain the supported palladium catalyst, in which the mass percentage of palladium is 10%.

Embodiment 2

[0052] For the synthesis of palladium nanorods, 0.1 mmol palladium acetylacetonate was dissolved in 10 mL oleylamine, and 0.8 mmol N,N-diethylaniline borane was injected into the above solution, and the solution obviously changed from colorless to brown black. The temperature of the solution was adjusted to 50° C. and reduced for 45 minutes to obtain nanocrystals. After the temperature dropped to room temperature, ethanol was added to settle the nanoparticles, and the nanoparticles were obtained by centrifugation. The nanoparticles were washed successively with distilled water and ethanol, and dried to obtain a brown-black powder (palladium nanocrystal). Take 8 mg of powder and disperse it in 10 mL of n-hexane, add 32 mg of graphene, load at room temperature, and finally centrifuge and dry to obtain the supported palladium catalyst, in which the mass percentage of palladium is 20%.

Embodiment 3

[0054] For the synthesis of palladium nanorods, 0.1 mmol of palladium acetylacetonate was dissolved in 10 mL of oleylamine, and 1 mmol of N,N-diethylaniline borane was injected into the solution, and the solution obviously changed from colorless to brown-black , reacted at room temperature for 1 hour. Then ethanol was added to make the nanoparticles settle down, and the nanoparticles were obtained by centrifugal separation. The nanoparticles were washed successively with distilled water and ethanol, and dried to obtain a brown-black powder (palladium nanocrystal), and its transmission electron microscope picture is as follows: figure 1 As shown, it can be seen from the figure that the prepared nanoparticles are nanorods with uniform size and good dispersion. figure 1 In (b), the lattice fringes of palladium can be clearly seen, and the lattice spacing is about 0.23 nm, which corresponds to the (111) crystal plane of palladium. Take 8 mg of powder and disperse it in 10 mL o...

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Abstract

The invention discloses a supported palladium catalyst and a preparation method and application thereof. The supported palladium catalyst disclosed by the invention comprises a graphene carrier and palladium nano-crystals or palladium nano-alloys supported on the carrier, wherein the palladium nano-crystals or palladium nano-alloys account for 10-50 mass percent. The preparation method comprises the following steps: (1) dissolving palladium salt in oleylamine to obtain a palladium salt solution, or dissolving cobalt salt or nickel salt and palladium salt in oleylamine to obtain a mixed solution; (2) adding a boron-nitrogen compound into the palladium salt solution or the mixed solution, and adding an organic settling agent, thereby obtaining the palladium nano-crystals or palladium nano-alloys; and (3) supporting the palladium nano-crystals or palladium nano-alloys on graphene, thereby obtaining the supported palladium catalyst. The supported palladium catalyst and the preparation method disclosed by the invention have the advantages that the preparation method is low in reaction temperature and is simple and convenient, and the shape and size of the palladium catalyst can be controlled. Moreover, the active ingredients of the supported palladium catalyst disclosed by the invention are uniform in size and high in dispersity, and the catalyst is high in activity and can be used for catalyzing formic acid oxidation.

Description

[0001] technical field [0002] The invention relates to a supported palladium catalyst and its preparation method and application, belonging to the field of nanometer materials. Background technique [0003] Nanomaterials have important application value in many fields such as electronics, optics, chemical industry, ceramics, biology and medicine due to their unique properties - small size effect, surface and interface effect, quantum size effect and macroscopic quantum orbital effect. It has attracted the attention of scientists from all over the world, and at the same time shows great application prospects. As an important part of nanomaterials, metal nanocatalysts have the characteristics of large specific surface area and high density of effective active centers, which are of great significance for improving the efficiency and selectivity of chemical reactions. Among the many metal nanocatalysts, palladium metal nanocatalysts occupy an important position, but palladium...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J23/89
Inventor 罗威杜成程功臻
Owner SUZHOU INSTITUE OF WUHAN UNIV
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