Method for preparing metal single-atom catalyst

A catalyst and atomic technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve problems such as unknown heterogeneous phases, difficult artificial control, complicated MOFs crystal growth process, etc., to achieve high porosity rate, high specific surface effect

Pending Publication Date: 2019-07-05
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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Problems solved by technology

However, it is well known that the growth process of MOFs crystals is very complicated and difficult to control artificially.
Therefore, the main disadvantage of this metal single-at

Method used

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  • Method for preparing metal single-atom catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0029] The preparation method of Fe single-atom catalyst is as follows:

[0030] (1) Preparation of Zr-based metal-organic framework materials containing bipyridyl groups

[0031] 0.246g ZrCl 4 , 0.260g of 2,2′-bipyridyl-5,5′-dicarboxylic acid and 7mL of formic acid were added to 100mL of N,N′-dimethylformamide solvent, fully dissolved and then transferred to a liner containing polytetrafluoroethylene In a stainless steel reactor, react at 120°C for 24h. The reacted product was centrifuged and washed with acetone for 2-3 times, dried at 80°C for 2h, and then transferred to a vacuum drying oven at 160°C for 12h in vacuum. The white product obtained was Zr-based metal organic framework material, whose structure is a metal-organic framework material with UiO type, such as figure 1 As shown, its PXRD is consistent with the fitted PXRD.

[0032] (2) Preparation of Zr-based metal-organic framework materials loaded with ferric chloride

[0033] Add 0.02g of ferric chloride hexah...

Embodiment 2

[0043] In this example, the preparation method of the Co single-atom catalyst is basically the same as that in Example 1, except that the iron chloride hexahydrate in step (2) is replaced by cobalt chloride hexahydrate.

[0044] The spherical aberration electron microscope picture of the Co single-atom catalyst prepared above is as follows: Figure 5 As shown, it can be seen that Co single atoms are uniformly dispersed on the C substrate.

[0045] The synchrotron radiation EXAFS results of the Co single-atom catalyst prepared above are similar to Example 1, showing that there is no Co-Co bond in the Co single-atom catalyst, that is, there are no Co nanoparticles.

Embodiment 3

[0047] In the present embodiment, the preparation method of Ni single-atom catalyst is basically the same as the preparation method in Example 1 as follows, the difference is: replace the ferric chloride hexahydrate in step (2) with nickel chloride hexahydrate, solvent modification to acetonitrile.

[0048] The spherical aberration electron microscope picture of the Ni single-atom catalyst made above is as follows Figure 6 As shown, it can be seen that Ni single atoms are uniformly dispersed on the C substrate.

[0049] The synchrotron radiation EXAFS results of the Ni single-atom catalyst prepared above are similar to Example 1, showing that there is no Ni-Ni bond in the Co single-atom catalyst, that is, there are no Ni nanoparticles.

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Abstract

The invention provides a method for preparing a metal single-atom catalyst. The method comprises the following steps: a metal-organic framework material having a bipyridyl group is selected, a metal salt precursor is coordinated to the bipyridyl group by a post-treatment modification process, and the coordinated metal-organic framework material is carbonized and acid-etched in an inert atmosphereto obtain the metal single-atom catalyst. The method has the advantages of simplicity, easiness in implementation, universality, avoiding of formation of the impure phase, avoiding of the aggregationof metal atoms, and good application prospect.

Description

technical field [0001] The invention belongs to the technical field of chemical catalysis, and in particular relates to a preparation method of a metal single-atom catalyst. Background technique [0002] Metal single-atom catalysts exhibit extremely excellent catalytic activity and maximum atom usage efficiency due to their atomically dispersed metal active sites. Since academician Zhang Tao of Dalian Institute of Chemical Physics, Chinese Academy of Sciences proposed the concept of metal single-atom catalysis in 2011, after a few years of development, metal single-atom catalysts have rapidly become the research frontier and hotspot in the field of catalysis. The current strategies for preparing metal single-atom catalysts mainly include liquid phase impregnation, atomic layer deposition, metal hydroxide / polymer core-shell structure strategy and photoelectrochemical strategy. However, these methods are only suitable for the preparation of a certain metal single atom, and ha...

Claims

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Application Information

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IPC IPC(8): B01J27/24
CPCB01J27/24B01J35/0033
Inventor 林贻超陈亮
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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