Transition metal single-atom catalyst as well as preparation method and application thereof

A transition metal and transition metal salt technology, applied in the field of micro-nano material preparation, can solve problems such as inability to improve, complex synthesis methods, intensified thermal motion, etc., and achieve the effects of reducing surface pollution, avoiding metal agglomeration, and reducing costs.

Inactive Publication Date: 2019-06-21
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the method of impregnation and calcination of metal ions and supports still has problems such as complex synthesis methods and inability to prepare on a large scale.
And with MOFs or C 3 N 4 Such as the carrier needs to be calcined at a very high temperature to be carbonized, and the thermal movement of atoms is intensified at high temperature, w

Method used

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  • Transition metal single-atom catalyst as well as preparation method and application thereof
  • Transition metal single-atom catalyst as well as preparation method and application thereof
  • Transition metal single-atom catalyst as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0044] A method for preparing a nickel single-atom catalyst, comprising the steps of:

[0045] 1) Weigh 0.2mmol nickel acetate and 0.6mmol o-phenanthroline into a test tube, add 2mL ethanol, stir magnetically until completely dissolved to obtain a clear and transparent solution;

[0046] 2) After the reaction is completed, weigh 69.6mg of carbon black and add it to the above solution of Ketjenblack EC-300J type, mix evenly, heat in a water bath at 60°C for 4h, and then dry it in an oven at 80°C for 12h to obtain a crude product;

[0047] 3) The crude product obtained above was heated in an argon atmosphere at 10°C·min -1 The heating rate is raised to 580°C, and kept at this temperature for 2 hours. After the completion, the temperature is naturally lowered to room temperature, and the Ni single-atom catalyst is obtained, which is recorded as Ni-SAC. The Ni-SAC can be detected by the ICP-AES method. The supported amount of Ni atoms was 6.0 wt%.

[0048] figure 1 The middle c...

Embodiment 2-4

[0054] Repeat embodiment 1, its difference is only to change nickel acetate into nickel chloride, nickel nitrate, nickel sulfate. The Ni single-atom catalyst obtained is not significantly different from the single-atom catalyst obtained in Example 1, and by ICP-AES method, it can be detected that the Ni atom loading in the Ni-SAC is 6 wt%.

[0055] Figure 5 It is the XRD pattern of the Ni single-atom catalyst synthesized by embodiment 2-4, as can be seen from the figure, the Ni single-atom catalyst that adopts nickel chloride, nickel nitrate, nickel sulfate all only appears the peak of carbon black, and The peak of Ni or its compound did not appear. This also shows that the species of anions in transition metal salts have no significant effect on the formation of single-atom catalysts.

Embodiment 5

[0057] Repeat Example 1, its difference is only to change Ketjenblack EC-300J type carbon black into Vulcan XC-72 type carbon black, the catalyzer that obtains is single-atom catalyst, and by ICP-AES method, can detect in this Ni-SAC , the loading of Ni atoms was 4.5wt%.

[0058] Figure 6 Shown are the Ni single-atom XRD patterns synthesized in Example 1 and Example 5. In the figure, the Ni single atoms synthesized by two types of carbon black only have the peak of carbon black, and no peak of metal element or compound appears. This indicates that the type of carbon black has no significant effect on the formation of single-atom catalysts.

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Abstract

The invention provides a transition metal single-atom catalyst. In the catalyst, transition metal single atoms are taken as active ingredients, carbon black is taken as a carrier, the loading capacityof the transition metal single atoms is 0.5-6wt%, and the highest loading capacity of the transition metal single atoms is higher than that of the prior art by 2-3 times. Various low-price transitionmetal single-atom catalysts with high dispersibility and high loading capacity are formed by inducing a limit range and by taking phenanthroline with strong complexation effect as a ligand and takingthe carbon black with high conductivity and high surface activity as the carrier. A preparation method of the transition metal single-atom catalyst has universality and can be used for preparing various low-price transition metal single-atom catalysts; according to the method, a Cr single-atom catalyst, an Nb single-atom catalyst, an Rh single-atom catalyst, a Cd single-atom catalyst, an Os single-atom catalyst and an Ir single-atom catalyst are prepared for the first time. Additionally, the preparation method has the advantages of being low in cost and simple in process and achieving large-scale production. Next, the catalyst has higher selectivity and Faraday efficiency in application of preparation of carbon monoxide by reducing carbon dioxide through electro-catalysis.

Description

technical field [0001] The invention relates to the technical field of preparation of micro-nano materials. More specifically, it relates to a universal transition metal single-atom catalyst and its preparation method and application. Background technique [0002] Homogeneous catalysts and heterogeneous catalysts have been widely used in the chemical industry as two types of catalysts, and they have their own characteristics and advantages. Homogeneous catalysts have the advantages of uniform active sites, high atom utilization, and easy adjustment of active sites, but they have poor stability and are difficult to separate from reactants. Heterogeneous catalysts have high stability and are easy to separate from the reactants, but their atom utilization is low, and only the atoms on the surface can contact the reactants to participate in the catalytic reaction. How to combine the advantages of the two types of catalysts is a hot spot and difficult problem in catalytic resea...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J23/26B01J23/75B01J23/72B01J23/42B01J23/44B01J23/34B01J23/28B01J23/20B01J23/06B01J23/46B01J23/89C25B1/00C25B11/06C25B11/08
Inventor 张铁锐杨洪舟尚露
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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