Preparation method and solar nitrogen fixation application of indium sulfide photocatalyst with sulfur vacancies

A photocatalyst and indium sulfide technology, applied in the field of photocatalytic materials, can solve the problems of low utilization rate of visible light, fast recombination of photogenerated electron holes, etc., and achieve the effects of reducing environmental pollution, high quantum efficiency and broad application prospects.

Inactive Publication Date: 2019-08-09
DALIAN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still some shortcomings in the current photocatalytic nitrogen fixation technology, such as: the photocatalyst has low utilization rate o

Method used

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  • Preparation method and solar nitrogen fixation application of indium sulfide photocatalyst with sulfur vacancies
  • Preparation method and solar nitrogen fixation application of indium sulfide photocatalyst with sulfur vacancies
  • Preparation method and solar nitrogen fixation application of indium sulfide photocatalyst with sulfur vacancies

Examples

Experimental program
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Embodiment 1

[0054] Add 0.408g of indium nitrate hydrate and 0.2g of terephthalic acid into 12mL of N,N-dimethylformamide (DMF) solution, stir thoroughly for 30min until the solution is clear, then put it into a 1-2MPa autoclave, and heat it at 100℃ Constant temperature hydrothermal reaction 48h. The product was cooled to room temperature for centrifugation and washed 6 times with N,N-dimethylformamide (DMF) and ethanol solution respectively. After vacuum drying at 60°C, the powder was collected to obtain MIL-68(In). Add 0.01g MIL-68(In) and 0.6g thiourea to 80mL ethanol solution, stir thoroughly for 30min until the solution becomes clear, then put it into a 1-2MPa autoclave, and conduct a constant temperature hydrothermal reaction at 180°C for 3h. The product was cooled to room temperature, centrifuged and washed 6 times with water and ethanol solution respectively, and dried at 60°C to collect the powder to obtain In 2 S 3 . will get In 2 S 3 The powder is calcined under a nitrogen ...

Embodiment 2

[0062] Add 0.408g of indium nitrate hydrate and 0.2g of terephthalic acid into 12mL of N,N-dimethylformamide (DMF) solution, stir thoroughly for 30min until the solution is clear, then put it into a 1-2MPa autoclave, and heat it at 100℃ Constant temperature hydrothermal reaction 48h. The product was cooled to room temperature for centrifugation and washed 6 times with N,N-dimethylformamide (DMF) and ethanol solution respectively. After vacuum drying at 60°C, the powder was collected to obtain MIL-68(In). Add 0.01g MIL-68(In) and 0.6g thiourea to 80mL ethanol solution, stir thoroughly for 30min until the solution becomes clear, then put it into a 1-2MPa autoclave, and conduct a constant temperature hydrothermal reaction at 180°C for 3h. The product was cooled to room temperature, centrifuged and washed 6 times with water and ethanol solution respectively, and dried at 60°C to collect the powder to obtain In 2 S 3 . will get In 2 S 3 The powder is calcined under a nitrogen ...

Embodiment 3

[0064] Add 0.408g of indium nitrate hydrate and 0.2g of terephthalic acid into 12mL of N,N-dimethylformamide (DMF) solution, stir thoroughly for 30min until the solution is clear, then put it into a 1-2MPa autoclave, and heat it at 100℃ Constant temperature hydrothermal reaction 48h. The product was cooled to room temperature for centrifugation and washed 6 times with N,N-dimethylformamide (DMF) and ethanol solution respectively. After vacuum drying at 60°C, the powder was collected to obtain MIL-68(In). Add 0.01g MIL-68(In) and 0.6g thiourea to 80mL ethanol solution, stir thoroughly for 30min until the solution becomes clear, then put it into a 1-2MPa autoclave, and conduct a constant temperature hydrothermal reaction at 180°C for 3h. The product was cooled to room temperature, centrifuged and washed 6 times with water and ethanol solution respectively, and dried at 60°C to collect the powder to obtain the final product In 2 S 3 .

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Abstract

The invention discloses an indium sulfide photocatalyst with sulfur vacancies. The indium sulfide photocatalyst has a molecular formula of In2S3, abd is used for high-efficiency solar nitrogen fixation. A preparation method of the catalyst comprises the following steps: 1, taking an organic liquid as a solvent; 2, adding an organic substance and an indium salt compound to the organic solvent; 3, filling a reaction kettle with the obtained solution, and performing a constant temperature reaction; 4, cooling the obtained solution to room temperature, centrifuging the cooled solution, respectively washing the obtained reaction product with the organic solvent and an ethanol solution, drying the washed reaction product, and collecting the obtained powder to obtain MIL-68(In); 5, adding an organic sulfide to an organic alcohol solvent, and performing mixing and sufficient stirring; 6, adding MIL-68 (In), and performing mixing and sufficient stirring; 7, filling the reaction kettle with theobtained mixture, and carrying out a constant temperature reaction; 8, cooling the obtained solution to room temperature, centrifuging the cooled solution, washing the obtained solid with water and the ethanol solution respectively, drying the washed solid, and collecting the obtained powder to obtain indium sulfide; and 9, annealing the indium sulfide in a nitrogen atmosphere to produce sulfur vacancies. The catalyst obtained by the method of the invention has the advantages of environmental protection, harmlessness, realization of batch production, and efficient solar nitrogen fixation performance.

Description

technical field [0001] The invention relates to the technical field of photocatalytic materials, more specifically, to the preparation of an indium sulfide photocatalyst containing sulfur vacancies and the application of solar nitrogen fixation. Background technique [0002] Ammonia (NH 3 ) as an extremely important chemical for the synthesis of chemicals and fertilizers has been widely used in industry and agriculture. All along, the traditional NH 3 The manufacturing method is the Haber ammonia production process, which usually uses an iron-based catalyst to combine the largest single component in the earth's atmosphere-nitrogen and hydrogen (H 2 ) together to produce ammonia. However, this method consumes a lot of energy, therefore, it is necessary to use a low energy consumption and clean and safe method to reduce energy consumption. [0003] Solar photocatalytic nitrogen fixation technology has attracted much attention because of its mild reaction conditions, high e...

Claims

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Application Information

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IPC IPC(8): B01J27/04C01C1/04C05C3/00
CPCB01J27/04B01J35/004C01C1/04C05C3/00Y02P20/52
Inventor 董晓丽何志漪王宇郑楠马红超张秀芳
Owner DALIAN POLYTECHNIC UNIVERSITY
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