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A kind of preparation method of metal single atom catalyst

A catalyst and metal technology, applied in the field of preparation of metal single-atom catalysts, can solve problems such as difficulty in controlling metal dispersion, achieve metal atom dispersion and controllable active sites, high metal atom loading concentration, simple and practical preparation method Effect

Active Publication Date: 2021-06-11
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In view of the above-mentioned deficiencies in the prior art, the purpose of the present invention is to provide a method for preparing a metal single-atom catalyst, which solves the problem that the existing method is difficult to control the metal dispersion

Method used

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  • A kind of preparation method of metal single atom catalyst
  • A kind of preparation method of metal single atom catalyst

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Experimental program
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Effect test

Embodiment 1

[0032] Embodiment 1: the preparation of Ag single-atom catalyst

[0033] Step 1, 1 g of aminated g-C 3 N 4 Add it to 20ml of anhydrous ether, add 0.25ml of 1.6M methyllithium ether solution dropwise to it under nitrogen atmosphere, stir while adding, keep the temperature of the system at -78°C during the dropwise addition, and place in nitrogen atmosphere after the dropwise addition Stir and react at 25°C for 8 hours, then filter, and the filter cake is washed and dried with anhydrous ether to obtain an intermediate product;

[0034] Step 2, disperse the obtained intermediate product and 65 mg AgCl in 20 ml of anhydrous ether under a nitrogen atmosphere, and stir and react at 25° C. for 8 hours to obtain a mixture of Ag single-atom catalyst and lithium chloride;

[0035] In step 3, the mixture described in step 2 is fully dissolved in water and then filtered, and the filter cake is dried at 50° C. to obtain the Ag single-atom catalyst with a loading capacity of 4%.

[0036] ...

Embodiment 2

[0040] Embodiment 2: the preparation of Cu single-atom catalyst

[0041] Step 1, add 1g of hydroxylated fullerene to 20ml of anhydrous n-hexane, add 0.5ml of 2.5M n-butyl lithium ether solution dropwise to it under nitrogen atmosphere, stir while adding, and maintain the system during the dropping process The temperature is -78°C. After the dropwise addition, stir and reflux at 60°C under a nitrogen atmosphere for 6 hours, then filter, and the filter cake is washed and dried with anhydrous n-hexane to obtain an intermediate product;

[0042] Step 2, disperse the obtained intermediate product and 124 mg CuCl in 20 ml of anhydrous n-hexane under a nitrogen atmosphere, and stir and reflux at 60 ° C for 6 h to obtain a mixture of Cu single-atom catalyst and lithium chloride;

[0043] In step 3, the mixture described in step 2 is fully dissolved in water and then filtered, and the filter cake is dried at 100° C. to obtain the Cu single-atom catalyst with a loading capacity of 7%. ...

Embodiment 3

[0047] Embodiment 3: the preparation of Co single-atom catalyst

[0048] Step 1, add 1g of graphene oxide to 20ml of anhydrous furan, add 0.34ml of 16% tert-butyl lithium pentane solution dropwise to it under nitrogen atmosphere, stir while adding, and maintain the system temperature at -78°C during the dropping process °C, after the dropwise addition, stir and reflux at 80 °C for 4 hours under a nitrogen atmosphere, then filter, and the filter cake is washed and dried with anhydrous furan to obtain an intermediate product;

[0049] Step 2, the intermediate product obtained with 66mg CoCl 2 Disperse in 20ml of anhydrous furan under a nitrogen atmosphere, stir and reflux at 80°C for 4h to obtain a mixture of Co single-atom catalyst and lithium chloride;

[0050] In step 3, the mixture described in step 2 is fully dissolved in water and then filtered, and the filter cake is dried at 150° C. to obtain the Co single-atom catalyst, wherein the loading amount is 2%.

[0051] The c...

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Abstract

The invention discloses a method for preparing a metal single-atom catalyst, which comprises the following steps: (1) adding a functionalized carbon-based material into an organic solvent A, and then adding an organolithium reagent dropwise therein under an inert atmosphere, adding dropwise After completion, react under an inert atmosphere to obtain an intermediate product, and the functionalized carbon-based material is a hydroxyl or / and aminated carbon-based material; Dispersing in an organic solvent B for reaction to obtain a mixture of the metal single-atom catalyst and lithium chloride; (3) purifying the mixture described in step (2) to obtain the metal single-atom catalyst. The metal single-atom catalyst prepared by the method of the present invention has relatively controllable metal atom dispersion and active sites on the surface of the carrier, is generally applicable to the synthesis of various metal single-atom catalysts, and can be used in the fields of synthetic catalysis such as energy, catalysis, medicine and biology. .

Description

technical field [0001] The invention belongs to the field of catalyst preparation, and in particular relates to a method for preparing a metal single-atom catalyst supported by a hydroxyl / aminated carbon-based material. [0002] technical background [0003] The development of more efficient catalysts has always been the focus of materials and chemistry. The most widely used in industry is the supported metal catalyst with high catalytic activity. The root of its high catalytic activity lies in the size of the supported metal atom particles. For this reason, researchers continue to try smaller-sized particles. In recent years, it has been found that sub-nanometer clusters have higher catalytic activity than nano-clusters. The ideal state of a catalyst with a substrate-supported metal structure is that the metal atoms are independently distributed on the substrate one by one to achieve the highest degree of dispersion, which is a single-atom catalyst. Single-atom catalysts c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/72B01J23/75B01J23/755B01J27/24C01B3/04C01B32/40C01B32/50C07C1/12C07C9/04C07C209/18C07C211/44
CPCB01J23/72B01J23/75B01J23/755B01J27/24C01B3/042C01B2203/0277C01B2203/1041C07C1/12C07C209/18C01B32/40C01B32/50C07C9/04C07C211/44Y02E60/36
Inventor 杜立永丁玉强王科炎
Owner JIANGNAN UNIV
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