Preparation method of defect-foamed graphene-supported transition metal single-atom catalyst

A technology of foamed graphene and transition metals, applied in the direction of electrolysis process, electrolysis components, electrodes, etc., can solve the problems of large fossil fuel consumption, greenhouse gas emission, etc., achieve the effect of increasing quantity, improving catalytic activity, and broadening the field of preparation

Active Publication Date: 2022-04-22
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this process involves high temperature and pressure, consumes a lot of fossil fuels, and emits a lot of greenhouse gases

Method used

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  • Preparation method of defect-foamed graphene-supported transition metal single-atom catalyst
  • Preparation method of defect-foamed graphene-supported transition metal single-atom catalyst
  • Preparation method of defect-foamed graphene-supported transition metal single-atom catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take 1 gram of the dried graphene oxide sample, soak it in nitric acid solution for 4 hours, and centrifuge and wash it to neutral with deionized water. figure 1 It can be seen that the defective graphene oxide is relatively thin, and there are obvious defects in the morphology.

[0032] Take 100 mg of dried defective graphene oxide and dissolve it in 100 mL of thiourea aqueous solution for ultrasonic dispersion, stir for 6 h, re-disperse in aqueous solution after centrifugation, add 1 ml of 19 mmol / L ferrous sulfate solution for ultrasonic dispersion. The filtered sample was redispersed in the solution and treated with 700W microwave for 1min, the sample turned from yellow to grayish black. The microwaved sample was acid-washed in 3 mol / L HCL solution for 8 hours to remove the particles and impurities inside, and then washed to neutrality. The neutralized sample was prepared into a 40 mL solution, placed in a reaction kettle at 180°C for 6 hours, and freeze-dried for ...

Embodiment 2

[0038] Take 1 gram of the dried graphene oxide sample, soak it in nitric acid solution for 2 hours, and wash it by centrifugation with deionized water until it becomes neutral.

[0039] Take 100 mg of dried defective graphene oxide and dissolve it in 100 mL of urea aqueous solution for ultrasonic dispersion, stir for 6 h, re-disperse in aqueous solution after centrifugation, and add 3 ml of 15 mmol / L molybdenum chloride solution for ultrasonic dispersion. The filtered sample was redispersed in the solution and treated with 500W microwave for 3min, the sample turned from yellow to grayish black. The sample after microwave was acid-washed in 3 mol / L HCL solution for one day to remove the particles and impurities inside, and then washed to neutrality. The neutralized sample was prepared into a 40 mL solution, placed in a reaction kettle at 180°C for 12 hours, and freeze-dried for 24 hours.

[0040] The freeze-dried samples were placed in a tube furnace with argon at 800°C for tw...

Embodiment 3

[0043] The preparation method is the same as in Example 2, only the transition metal salt is nickel sulfate, and the performance diagram is shown in the attached Figure 7 , it can be seen from the figure that at -0.3V (VS.RHE), the synthesis efficiency is the highest and the ammonia synthesis yield is 21μgh -1 mgcat -1 , with a Faraday efficiency of 10%.

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Abstract

The invention discloses a method for preparing a transition metal single-atom catalyst supported on defective foamed graphene, which is applied to nitrogen reduction to synthesize ammonia. After treatment with hydrochloric acid solution, it is washed until it is neutrally dispersed in aqueous solution. The surface of the microwave-treated sample has oxygen-containing functional groups, and the product is obtained after hydrothermal treatment and freeze-drying. The above-mentioned product is reduced by heat treatment at high temperature and the transition metal atoms are rearranged to ensure the formation of transition metal single atoms, and a defect foamed graphene-supported transition metal single atom catalyst is prepared. Advantage 1 of the preparation method of the present invention is that defects are used to increase active sites and the number of transition metal single atoms is increased; advantage 2 is that the surface area of ​​the catalyst is increased by using the three-dimensional network to improve catalytic activity. The catalyst obtained by the method has high catalytic activity, durability and good stability.

Description

technical field [0001] The invention relates to the field of electrocatalytic synthesis of ammonia at room temperature, specifically relates to anchoring transition metal atoms by preparing defective graphene oxide, and assembling the sample into a three-dimensional foam network structure through hydrothermal reaction, further reducing the defective foam graphene through high temperature annealing, improving the Thermal stability of transition metal single atoms. Background technique [0002] Ammonia is an important raw material for the production of nitric acid, fertilizers and explosives. Before the invention of artificial nitrogen fixation technology, NH 3 It is difficult to meet the demand of rapid population growth. The birth of the Haber-Bosch method has significantly increased the world's population and industrialization. However, this process involves high temperature and pressure, consumes a lot of fossil fuels, and emits a lot of greenhouse gases. Therefore, it ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B1/27C25B11/075C25B11/065C25B11/054
CPCC25B1/00
Inventor 陈少娜卜梦珂代忠旭
Owner CHINA THREE GORGES UNIV
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