Preparation method of metal monatomic catalyst

A catalyst and metal technology, which is applied in the field of preparation of metal single-atom catalysts, can solve problems such as difficulty in controlling the dispersion of metals, and achieve the effects of wide coverage of metal types, high atomic dispersion, and many types of metals

Active Publication Date: 2019-04-09
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 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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  • Preparation method of metal monatomic catalyst
  • Preparation method of metal monatomic catalyst

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Embodiment 1

[0031] Embodiment 1: the preparation of Ag single-atom catalyst

[0032] 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;

[0033] 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;

[0034] 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%.

[0035]...

Embodiment 2

[0039] Embodiment 2: the preparation of Cu single-atom catalyst

[0040] 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;

[0041] 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;

[0042] 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

[0046] Embodiment 3: the preparation of Co single-atom catalyst

[0047] 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;

[0048] 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;

[0049] 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%.

[0050] The c...

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Abstract

The invention discloses a preparation method of a metal monatomic catalyst. The preparation method comprises the following steps: (1) adding a functionalized carbon-based material into an organic solvent A, then dropwise adding an organic lithium reagent into the organic solvent in an inert atmosphere and carrying out a reaction in the inert atmosphere after dropwise addition to obtain an intermediate product, wherein the functionalized carbon-based material is a hydroxyl or / and aminated carbon-based material; (2) dispersing the intermediate product and a metal chloride in an organic solvent Bin the inert atmosphere to react to obtain a mixture of the metal monatomic catalyst and lithium chloride and (3) purifying the mixture in the step (2) to obtain the metal monatomic catalyst. The metal monatomic catalyst prepared by the method is relatively controllable in metal atom dispersity and active sites on the surface of a carrier and suitable for synthesizing various metal monatomic catalysts commonly and can be used in the synthetic catalytic fields of energy sources, catalysis, medicines, biology and the like.

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. technical background [0002] 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 can maxim...

Claims

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Application Information

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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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