Preparation method and application of ultra-smallpalladium base alloy material

A technology based on alloys and ultra-small palladium, applied in the field of nanomaterials, can solve the problems that the soft landing method cannot be applied to large-scale production, and the contact between the substrate and the active site of the catalyst is difficult, so as to facilitate the application of catalytic research and facilitate industrial production , the effect of simple method

Inactive Publication Date: 2019-11-05
UNIV OF SCI & TECH OF CHINA
View PDF4 Cites 13 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these synthetic methods and means can effectively limit the particle size growth, there are many disadvantages, such as the difficulty in contacting the substrate with the active site of the catalyst during the catalytic process when using a protective agent, and the soft landing method is still in the laboratory stage and cannot be applied. in mass production

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method and application of ultra-smallpalladium base alloy material
  • Preparation method and application of ultra-smallpalladium base alloy material
  • Preparation method and application of ultra-smallpalladium base alloy material

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0038] The invention provides a method for preparing an ultra-small palladium-based alloy material, comprising: mixing a nitrogen-doped porous carbon material, a palladium salt and a metal salt in a solvent, and obtaining the mixture after removing the solvent; Calcined in the atmosphere to obtain ultra-small palladium-based alloy materials.

[0039] This application has prepared a palladium-based ultra-small alloy catalyst by means of impregnation and heat treatment. The alloy cluster restricts the growth of particles through the coordination of metal atoms and nitrogen atoms on the support, and at the same time improves the stability of the catalyst. In addition, the abundant pores on the support Structure also plays a key role in inhibiting particle sintering.

[0040] The present invention has no special limitation on the sources of all raw materials, which can be commercially available.

[0041] Wherein, the content of nitrogen element in the nitrogen-doped porous carbon...

Embodiment 1

[0057] Mix 2.50g of cyclohexanone octawater and 1.44g of urea, grind it thoroughly, add 15.0g of zinc chloride, grind it fully, move it to a quartz boat, and raise the temperature to 90~ at a rate of 5°C / min under nitrogen protection Form a eutectic flux at 100°C, keep it warm for 1-2 hours, then raise the temperature to 600°C at a heating rate of 2.5°C / min and keep it warm for 3 hours, use 1M HCl solution to stir at 80°C for 6 hours, filter with suction, and dry to get nitrogen-doped porous carbon material. The mass fraction of nitrogen in the obtained nitrogen-doped porous carbon material reaches more than 10%.

[0058] figure 1 It is the nitrogen adsorption-desorption curve and pore size distribution diagram of the nitrogen-doped porous carbon material obtained in Example 1 of the present invention. BET specific surface area reaches >900m 2 / g, containing a large number of micropores and mesopores.

Embodiment 2

[0060] Mix 50.0 mg of nitrogen-doped porous carbon material obtained in Example 1 above with palladium chloride solution containing 1.25 mg of Pd, then add lead nitrate solution so that the atomic ratio of Pd and Pb is 1:2, and finally add water to dilute to make The total volume of the mixed solution was kept at 40 ml. The mixed solution obtained above was sonicated for 1 hour, and then stirred at room temperature for 12 hours, so that the precursor and the carbon carrier were fully mixed; Medium reduction, the heating rate is 5°C / min, the temperature is raised to 500°C, and the temperature is kept for 2h. Then cool down to room temperature naturally, and the ultra-small palladium-based alloy material can be obtained.

[0061] Utilize the high-angle annular dark field image-scanning transmission electron microscope to analyze the ultra-small palladium-based alloy material obtained in embodiment 2, obtain its HAADF-STEM electron microscope photo and its energy dispersive spec...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
specific surface areaaaaaaaaaaa
sizeaaaaaaaaaa
specific surface areaaaaaaaaaaa
Login to view more

Abstract

The invention provides a preparation method of an ultra-small palladium base alloy material. The preparation method comprises the steps that a porous nitrogen-doped carbon carrier, a palladium salt and a metal salt are mixed in a solvent, and a mixture is obtained after removing the solvent; and the mixture is calcined in a reduction atmosphere to obtain an ultra-small palladium base alloy material. According to the preparation method of the ultra-small palladium base alloy material, compared with the prior art, by the fact that the metal-nitrogen coordination bond is formed between metal andthe heteroatomic nitrogen on the carbon carrier and the channel limiting effect of the abundant channel structure in the carrier, growth of particles is inhabited, metal particles can be evenly supported on the surface of the porous nitrogen-doped carbon carrier, not only effective utilization of palladium atoms is increased, but also the cost of a catalyst can be reduced, catalytic research is favorable to be applied, at the same time, the method is simple and universal, and industrial production is easy.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and in particular relates to a preparation method and application of an ultrasmall palladium-based alloy material. Background technique [0002] Supported palladium-based catalysts have been widely used in many important fields such as hydrogenation / dehydrogenation, electrochemical oxidation, CO oxidation, and Suzuki coupling reaction. The geometric structure, electronic effect, and coordination environment of Pd particles can be flexibly adjusted by introducing a second metal, which further flexibly adjusts the activity and selectivity of the catalyst. At the same time, the introduction of another metal can greatly reduce the use of Pd, thereby reducing the cost of catalyst preparation. However, the catalytic performance of most catalysts depends on the size and geometric structure of Pd particles, and Pd-based catalysts are easy to agglomerate during preparation and use, and it is ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J31/18C07C5/09C07C15/46
CPCB01J27/24B01J31/1805B01J2231/645C07C5/09C07C15/46
Inventor 梁海伟王磊
Owner UNIV OF SCI & TECH OF CHINA
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap