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Preparation method of covalent organic framework material derivative carbon skeleton loaded metallic monatomic composite material

A covalent organic framework and metal-loaded technology, which is applied in chemical instruments and methods, catalyst activation/preparation, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem that metal active components are easy to aggregate into nanoparticles, The types of single-atom metals cover a narrow range of problems, such as single atoms are easy to fall off from the carrier, and the reaction process conditions are easy to control, the synthesis time is short, and the cost is low.

Pending Publication Date: 2019-10-25
HEFEI UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to overcome the deficiencies of the prior art, the present invention provides a method for preparing a covalent organic framework material-derived carbon skeleton-supported metal single-atom composite material. Aggregation into nanoparticles, single atoms are easy to fall off from the carrier, poor catalytic stability, secondary pollution caused by the leaching of a large number of ions during the reaction process, and technical problems such as narrow coverage of single-atom metal types, complicated operation, and inability to scale production

Method used

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  • Preparation method of covalent organic framework material derivative carbon skeleton loaded metallic monatomic composite material
  • Preparation method of covalent organic framework material derivative carbon skeleton loaded metallic monatomic composite material
  • Preparation method of covalent organic framework material derivative carbon skeleton loaded metallic monatomic composite material

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Effect test

Embodiment 1

[0027] Preparation of Fe@COFs-2-700 Fe@COFs-2-700, a covalent organic framework material-derived carbon skeleton-loaded single-atom iron composite:

[0028] Step 1: Weigh 32mg of p-phenylenediamine (0.3mmol) and 95mg of 2,4,6-triformylphloroglucinol (0.45mmol), place them in a mortar and grind them evenly, then add 2 drops of 1,3,5-Trimethylbenzene, dioxane and acetic acid in a volume ratio of 1:1:0.01 mixed solution, continue to grind evenly; the obtained product is centrifuged and cleaned 3 times with dichloromethane as a solvent (centrifuge speed is 2500r / min, each centrifugation time is set to 8min), then collected by methanol, and then dried in an oven at 60°C. The dried powder was placed in a tube furnace, heated to 180°C at a rate of 2°C / min under a nitrogen atmosphere with a flow rate of 0.1mL / min, and kept at a constant temperature for 24 hours; after the reaction was completed, it was cooled in a nitrogen atmosphere to At room temperature, the dark red target produ...

Embodiment 2

[0035] Preparation of Fe@COFs-1-700 Fe@COFs-1-700, a covalent organic framework material-derived carbon skeleton-loaded single-atom iron composite:

[0036] The preparation method of this embodiment is the same as that of Embodiment 1, the only difference is that 80 mg of anhydrous ferric chloride is weighed in step 2.

[0037] It has been demonstrated that in this example, monoatomic iron is uniformly dispersed in the carbon skeleton derived from the high-temperature carbonization of the covalent organic framework material, and the composite material has high dispersion of catalytic active sites and high catalytic stability.

Embodiment 3

[0039] Preparation of Fe@COFs-0.5-700 Fe@COFs-0.5-700, a covalent organic framework material-derived carbon skeleton-loaded single-atom iron composite:

[0040] The preparation method of this embodiment is the same as that of embodiment 1, the only difference is that step 2 weighs 40 mg of anhydrous ferric chloride.

[0041] It has been demonstrated that the monoatomic iron in this example is highly dispersed and stably embedded in the carbon skeleton derived from the covalent organic framework material.

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Abstract

The invention discloses a preparation method of a covalent organic framework material derivative carbon skeleton loaded metallic monatomic composite material. The preparation method comprises the following steps that firstly, a covalent organic framework material is synthesized through a room-temperature solid phase method, then the covalent organic framework material and a transition metal salt are mixed, stirred and dried, and a precursor is obtained; and finally, the precursor is calcinated through an in-situ pyrolysis method under protection of inert gas, and thus a target product is obtained. According to the preparation method, the monatomic catalytic material with high catalytic activity site dispersion and high catalytic stability is successfully constructed, the coverage of the metal types is wide, the cost is low, the operation steps are simple, reaction process conditions are easy to adjust and control, expensive equipment, special raw materials and complex processes are notneeded, and large-scale production can be achieved.

Description

technical field [0001] The invention belongs to the technical field of single-atom catalysis, and in particular relates to a preparation method of a covalent organic framework material-derived carbon skeleton-loaded metal single-atom composite material. Background technique [0002] Due to their high catalytic activity and selectivity, single-atom catalysts exhibit maximum atom utilization and effectively reduce catalyst costs, and are widely used in the fields of electrochemistry and chemical catalysis. However, in the process of preparation and catalytic reaction, due to the high surface energy of single-atom metals, they are easy to agglomerate and couple to form large clusters and lose their catalytic activity. Therefore, to prepare single-atom catalysts, the first thing to consider is to load isolated single atoms on the support to avoid agglomeration of metal atoms. Theoretically, two measures can be taken to increase the surface area of ​​the carrier and enhance the ...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J23/50B01J23/745B01J23/755B01J23/89B01J35/10B01J37/08
CPCB01J23/745B01J23/755B01J23/50B01J23/44B01J23/8906B01J37/086B01J37/084B01J35/61
Inventor 姚运金尹红玉张阳洋胡熠胡欢欢余茂静高梦雪
Owner HEFEI UNIV OF TECH
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