Metal monatomic catalyst and preparation method thereof

A catalyst and atomic technology, applied in the field of metal single-atom catalysts and their preparation, can solve problems such as the inability to achieve high single-atom loading, many synthesis steps, and complex synthesis processes, and achieve high active site density and metal utilization. The process is simple and the effect of improving catalytic performance

Active Publication Date: 2020-07-10
SOUTH UNIVERSITY OF SCIENCE AND TECHNOLOGY OF CHINA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods all synthesize the carrier first, then load the metal, and finally perform post-processing. The synthesis steps are many, the synthesis process is complicated, and it is impossible to achieve high single-atom loading.

Method used

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  • Metal monatomic catalyst and preparation method thereof
  • Metal monatomic catalyst and preparation method thereof
  • Metal monatomic catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A metal single-atom catalyst, its specific preparation method:

[0039] Under inert gas conditions, the polyacetylenic compound hexaethynylbenzene (22 mg, 0.1 mmol) was added to a Schlenk bottle filled with 20 mL of n-hexane, and at -80 ° C, solid sodium methoxide (32.4 mg, 0.6 mmol) was added, At this temperature, add ferric chloride (32.4 mg, 0.2 mmol) in n-hexane, stir for 2 h, heat and stir in an oil bath at 80°C for 6 h to obtain a black mixture; cool the mixture to room temperature, and centrifuge to remove the supernatant solution, add 30mL deionized water, ultrasonically disperse, and centrifuge again, repeat the above operations once with ethanol and acetone respectively, to obtain a gray-black solid, which is dried and ground to obtain 33.2 mg of the black target product, which is the metal mono An atomic catalyst, specifically a graphyne material supporting single-atom metal iron. The loading of iron was measured to be 16.4wt% by inductively coupled plasma o...

Embodiment 2

[0041] A metal single-atom catalyst, its specific preparation method comprises:

[0042]Under inert gas conditions, polyacetylenic compound hexaethynylbenzene (22 mg, 0.1 mmol) was added to a Schlenk bottle filled with 20 mL of tetrahydrofuran, and at -80 ° C, solid sodium ethoxide (40.8 mg, 0.6 mmol) was added to the At this temperature, add a tetrahydrofuran solution of cobalt dichloride (39.0mg, 0.3mmol), stir the reaction for 2h, heat and stir in an oil bath at 70°C for 12h, and obtain a black suspension; cool the suspension to room temperature, and centrifuge to remove the supernatant solution, add 30mL deionized water, ultrasonically disperse, and centrifuge again, repeat the above operations once with ethanol and acetone respectively, to obtain a gray-black solid, which is dried and ground to obtain 39.7 mg of the target product. The black target product is a metal single atom The catalyst is specifically a graphyne material supporting monoatomic metal cobalt. The load...

Embodiment 3

[0044] A metal single-atom catalyst, its specific preparation method comprises:

[0045] Under the condition of inert gas, the polyacetylenic compound 1,3,5-triethynylbenzene (15 mg, 0.1 mmol) was added to a Schlenk bottle containing 20 mL of chloroform, and at -80 ° C, potassium tert-butoxide was added (33.6mg, 0.3mmol), at this temperature, add cuprous chloride (29.7mg, 0.3mmol) in chloroform, stir for 2h, heat and stir in an oil bath at 60°C for 24h, to obtain a dark reddish-brown mixture; Cool the mixture to room temperature, centrifuge to remove the supernatant, add 30mL of deionized water, ultrasonically disperse, centrifuge again, repeat the above operations once with ethanol and acetone, respectively, to obtain a dark reddish brown solid, dry and grind to obtain the target product 34.0 mg, the black target product is a metal single-atom catalyst, specifically a graphyne material supporting single-atom metal copper. The loading of copper was measured to be 40.3wt% by i...

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Abstract

The invention discloses a metal monatomic catalyst and a preparation method thereof. The preparation method comprises the following steps: under the protection of inert atmosphere, dissolving a polyacetylene compound in an aprotic solvent; adding organic strong base and a metal salt precursor under the condition of -40 DEG C or below, performing heating and stirring for reaction, and then carryingout solid-liquid separation to obtain a precipitate; and washing, drying and grinding the precipitate to obtain a target product. The preparation method of the metal monatomic catalyst is simple, short in synthesis period and high in universality, and the obtained metal monatomic catalyst is good in thermal stability and high in metal monatomic loading capacity.

Description

technical field [0001] The invention relates to the technical field of catalyst preparation, in particular to a metal single-atom catalyst and a preparation method thereof. Background technique [0002] Due to their special electronic structure and geometric structure, single-atom catalysts can maximize metal utilization and exhibit excellent performance in a series of important catalytic reactions such as small molecule activation conversion, organic catalysis, and electrocatalysis. Therefore, it has become a broad consensus to increase the loading of metal single atoms, thereby improving the catalytic efficiency. Graphyne’s unique nanoscale pores, two-dimensional layered conjugated framework structure, and semiconductor properties make it an excellent carrier, and the preparation of high-load metal single-atom dispersed graphyne carbon material catalysts has become a hot direction. . [0003] However, when the metal particles are reduced to the single-atom level, the spe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/42B01J23/44B01J23/46B01J23/50B01J23/52B01J23/72B01J23/745B01J23/75B01J23/36B01J23/28B01J23/14
CPCB01J23/745B01J23/75B01J23/72B01J23/462B01J23/464B01J23/44B01J23/28B01J23/50B01J23/36B01J23/466B01J23/468B01J23/42B01J23/52B01J23/14
Inventor 段乐乐荣卫锋邹海远刘科
Owner SOUTH UNIVERSITY OF SCIENCE AND TECHNOLOGY OF CHINA
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