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A palladium-containing single-atom monolithic catalyst and its preparation method and application

A monolithic catalyst and catalyst technology, applied in chemical instruments and methods, preparation of organic compounds, physical/chemical process catalysts, etc., can solve the problems of low hydrogenation efficiency and poor selectivity, and achieve the dispersion of metal active sites , good selectivity and good cycle stability

Active Publication Date: 2020-12-08
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to overcome the disadvantages of low efficiency and poor selectivity in the selective hydrogenation of aromatic alkynes in the prior art, the present invention provides a palladium-containing single-atom monolithic catalyst

Method used

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  • A palladium-containing single-atom monolithic catalyst and its preparation method and application
  • A palladium-containing single-atom monolithic catalyst and its preparation method and application
  • A palladium-containing single-atom monolithic catalyst and its preparation method and application

Examples

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Effect test

preparation example 1

[0058] Soak a 2cm×2cm×2.5cm melamine-formaldehyde sponge in 30mL of 67mg / L palladium acetylacetonate-methanol solution. Shake on a shaker at low speed for 6 hours. The resulting adsorbed palladium ion sponge was rinsed three times with methanol, and vacuum-dried at 70°C for 24 hours. The obtained dried palladium salt loaded sponge was heat-treated at 800° C. for 0.5 h under nitrogen atmosphere. Through inductively coupled plasma emission spectrometry test, the palladium loading amount in the obtained catalyst is 0.023wt%.

[0059] Gained solid is taken out, and the black solid that obtains is exactly final monatomic palladium-containing catalyst, figure 1 This is the high-angle annular dark-field scanning transmission electron microscope image of the obtained catalyst. The bright spot in the figure is the synthesized single-atom Pd, indicating that the Pd metal atoms are in a monodisperse state on the carbon-nitrogen support, without the formation of clusters or nanoparticle...

preparation example 2

[0063] Other steps and conditions are the same as those in the preparation example, except that the obtained dried palladium salt-loaded sponge is heat-treated at 650° C. for 0.5 h under a nitrogen atmosphere to prepare a palladium-loaded single-atom catalyst. Figure 7 It is an image of the catalyst under a high-resolution scanning electron microscope. It can be seen that the shape of the melamine-formaldehyde sponge is maintained after heat treatment, and a good supporting structure and strength are maintained. The supported amount of palladium in the obtained catalyst was 0.021wt%.

preparation example 3

[0065] The other steps and conditions are the same as those in the preparation example, except that the obtained dried palladium salt-loaded sponge is heat-treated at 900° C. for 0.5 h in a nitrogen atmosphere to prepare a palladium-loaded single-atom catalyst. Figure 8 It is an image of the catalyst under a high-resolution scanning electron microscope. It can be seen that there are some fractures in its structure. Compared with the carbon sponge in the optimal temperature region, the diameter of the carbon-nitrogen frame becomes smaller, and the frame nodes are also damaged, and the structural strength is slightly weaker. . The loading amount of palladium in the obtained catalyst was 0.025wt%.

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Abstract

The invention provides a palladium-containing single-atom monolithic catalyst and its preparation method and use. Nitrogen-containing carbon sponges are used to load catalytically active components, and then heat-treated at a certain temperature to directly obtain a monolithic catalyst with a specific solid morphology. In addition, the present invention also provides a method for the selective hydrogenation of aromatic alkynes to obtain aromatic olefin compounds catalyzed by the single-atom palladium-containing catalyst, and the use of the single-atom palladium-containing catalyst. The obtained catalyst not only has high activity and good selectivity for the hydrogenation of alkynes to prepare olefins, but also the active components of the catalyst are directly combined with the nitrogen-carbon carrier during the heat treatment process to form an integrated structure of single-atom catalyst and carrier composite, ensuring the single-atom Catalyst stability.

Description

technical field [0001] The invention relates to the field of catalysts, in particular to an integral single-atom catalyst, which can be used for the selective hydrogen addition of aromatic alkynes. Background technique [0002] In recent years, single-atom catalysts have become a hot spot in the research of catalytic chemistry, and the heterogeneity of homogeneous reactions is a unique property of single-atom catalysts. However, the traditional single-atom catalyst carrier is mostly powder, and the molding process is more complicated; the integral catalyst is characterized by its good mass transfer efficiency, small amplification effect and simple operation, which is conducive to separation. To explore the synthesis method of the integral single-atom catalyst , more beneficial to the use of industrial catalysis. [0003] Styrene is the raw material for the production of PS, ABS resin and styrene-butadiene rubber. At present, industrial production of styrene is mainly recove...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24C07C201/12C07C205/06C07C5/09C07C15/46C07C41/20C07C43/215C07C17/354C07C25/24C07C25/22C07D213/127C07D213/06
CPCB01J27/24C07C201/12C07C5/09C07C41/20C07C17/354C07D213/127C07D213/06B01J35/394C07C205/06C07C15/46C07C43/215C07C25/24C07C25/22
Inventor 李亚栋张泽栋王定胜冀淑方
Owner TSINGHUA UNIV
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