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Monoatomic iron-sulfur-nitrogen co-doped carbon airgel electrocatalyst, preparation method and application

A carbon aerogel and electrocatalyst technology, applied in the field of electrocatalysis, can solve the problems of unclear catalytic active sites and low ammonia production rate, and achieve the effects of improving the catalytic reaction rate, low preparation cost and large interface area.

Active Publication Date: 2021-08-17
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] However, the catalyst in this invention still has a low rate of ammonia production, and the Faradaic efficiency is only 4.31%.
At the same time, the catalytic active sites of this type of M-SNC catalysts for electrochemical nitrogen reduction are still unclear. In the field of electrocatalysis, especially in the emerging field of electrochemical nitrogen reduction, it is still a challenge to reveal the active sites of M-SNC materials.

Method used

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  • Monoatomic iron-sulfur-nitrogen co-doped carbon airgel electrocatalyst, preparation method and application
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  • Monoatomic iron-sulfur-nitrogen co-doped carbon airgel electrocatalyst, preparation method and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Preparation process of monoatomic iron-sulfur-nitrogen co-doped carbon airgel electrocatalyst:

[0038] (1) Dissolve 4g of urea in 200mL of deionized water, heat the solution to 80°C and stir for 1 hour; add 4g of carrageenan and 0.5g of ferric nitrate nonahydrate, keep stirring at 80°C until the carrageenan and ferric nitrate are completely dissolved , to obtain a mixed solution;

[0039](2) The mixed solution obtained in step (1) is naturally cooled to room temperature, and freeze-dried to form an iron-urea-carrageenan mixture aerogel; the freeze-drying time is 24h;

[0040] (3) Calcinate the airgel obtained in step (2) at 900°C for 2h under a nitrogen atmosphere, put the obtained sample in 2M hydrochloric acid solution and etch for 24h, then wash it with deionized water until neutral, and vacuum at 80°C After drying, the carbon airgel electrocatalyst was obtained, which was designated as Fe-S-N-900.

[0041] Such as figure 1 As shown, the prepared Fe-S-N-900 catal...

Embodiment 2～4

[0043] According to the preparation process of Example 1, the calcination temperature in step (3) was changed to 800 ° C, 1000 ° C and 1100 ° C, respectively, to obtain carbon airgel electrocatalysts, respectively expressed as Fe-S-N-800, Fe-S-N-1000 and Fe-S-N-1100.

[0044] Iron atoms (0.54wt%, 0.84wt%, 0.74wt%, 0.48wt%) of the prepared catalyst (Fe-S-N-800, Fe-S-N-900, Fe-S-N-1000, Fe-S-N-1000), S (2.5wt%, 4.04wt%, 4.9wt%, 5.59wt%) and N (9.36wt%, 3.93wt%, 2.38wt%, 2.23wt%), the specific surface area is (197m 2 g -1 ,547m 2 g -1 , 379m 2 g -1 , 249m 2 g -1 ), pore volume (0.04cm 3 g -1 ,0.1cm 3 g -1 , 0.08cm 3 g -1 , 0.05cm 3 g -1 ) pore size (8.7nm, 7.7nm, 7.5nm, 4.3nm).

Embodiment 5

[0046] Preparation process of monoatomic iron-sulfur-nitrogen co-doped carbon airgel electrocatalyst:

[0047] (1) Dissolve 4g of urea in 200mL of deionized water, heat the solution to 80°C and stir for 1 hour; add 4g of carrageenan, keep stirring at 80°C until the carrageenan and ferric nitrate are completely dissolved to obtain a mixed solution;

[0048] (2) The mixed solution obtained in step (1) is naturally cooled to room temperature, and freeze-dried to form an iron-urea-carrageenan mixture aerogel; the freeze-drying time is 24h;

[0049] (3) Calcinate the airgel obtained in step (2) at 900°C for 2h under a nitrogen atmosphere, put the obtained sample in 2M hydrochloric acid solution and etch for 24h, then wash it with deionized water until neutral, and vacuum at 80°C After drying, the carbon airgel electrocatalyst was obtained, which was designated as S-N-900.

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Abstract

The invention relates to the technical field of electrocatalysis, and discloses a monoatomic iron-sulfur-nitrogen co-doped carbon aerogel electrocatalyst and its preparation method and application. In the carbon aerogel electrocatalyst, iron is dispersed in the form of a single atom In the carbon airgel co-doped with sulfur and nitrogen, the content of iron atoms in the electrocatalyst is 0.1-1wt%, the content of sulfur atoms is 2-6wt%, and the content of nitrogen atoms is 2-10wt%; the carbon aerogel electrocatalyst The specific surface area is 150~500m 2 g ‑1 , pore volume 0.01~0.1cm 3 g ‑1 , the pore size is 2-10nm; after dissolving urea, add carrageenan and ferric nitrate to dissolve completely; the airgel formed by the freeze-drying of the obtained mixed solution is calcined and acid-treated to obtain the electrocatalyst of the present invention, which can be used to catalyze Nitrogen is reduced to ammonia and a zinc-nitrogen battery has high catalytic activity, and the preparation method has the advantages of being simple, easy to operate and low in cost.

Description

technical field [0001] The invention relates to the technical field of electrocatalysis, in particular to a monoatomic iron-sulfur-nitrogen co-doped carbon airgel electrocatalyst, preparation method and application. Background technique [0002] Ammonia has become one of the most important chemicals in modern chemical production due to its wide application in fertilizer production and its great potential as a hydrogen energy carrier. At present, the production of ammonia is mainly through the Haber-Bosch process, but this process needs to be carried out under high temperature and pressure, resulting in a large amount of energy consumption and significant environmental pollution problems. Therefore, there is an urgent need for a low-energy, sustainable method to produce ammonia. [0003] Compared with the Haber-Bosch method, the electrocatalytic nitrogen reduction ammonia production can theoretically be carried out at normal temperature and pressure, and the source of raw wa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24B01J35/10B01J37/08H01M4/90H01M12/06C25B11/091C25B11/054C25B1/27
CPCB01J27/24B01J37/082H01M4/90H01M12/06C25B1/00B01J35/23B01J35/33B01J35/633B01J35/647B01J35/615
Inventor 侯阳李燕杨彬雷乐成
Owner ZHEJIANG UNIV
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