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Preparation method of Mo or Fe doped Zn1-xIn2S4 catalyst for photocatalytic nitrogen fixation and ammonia synthesis

A zn1-xin2s4, photocatalytic technology, applied in the direction of ammonia preparation/separation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of low efficiency of nitrogen fixation and synthesis of ammonia, interference with the accuracy of photocatalytic nitrogen fixation and synthesis of ammonia yield, etc. , to achieve the effects of simple preparation method and process flow, improved efficiency and good application prospects

Pending Publication Date: 2021-01-26
YANCHENG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (2) The main problem of the carbon nitride-based photocatalytic nitrogen fixation catalyst is that the nitrogen in the carbon nitride catalyst will generally precipitate during the photocatalytic nitrogen fixation reaction, which will greatly interfere with the accuracy of the photocatalytic nitrogen fixation synthetic ammonia yield detection
[0007] (3) The efficiency of photocatalyst nitrogen fixation and ammonia synthesis currently developed is still low, generally tens of µmol·g -1 h -1 , is far from the goal of actual industrial production. Therefore, it is necessary to develop a new photocatalytic nitrogen fixation catalyst system to improve the efficiency of photocatalytic nitrogen fixation and synthesis of ammonia.

Method used

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  • Preparation method of Mo or Fe doped Zn1-xIn2S4 catalyst for photocatalytic nitrogen fixation and ammonia synthesis
  • Preparation method of Mo or Fe doped Zn1-xIn2S4 catalyst for photocatalytic nitrogen fixation and ammonia synthesis
  • Preparation method of Mo or Fe doped Zn1-xIn2S4 catalyst for photocatalytic nitrogen fixation and ammonia synthesis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1 Pure ZnIn 2 S 4 Preparation of Photocatalytic Nitrogen Fixation Catalyst

[0032] Under magnetic stirring conditions, 0.0744g (ie 0.25mmol) of zinc nitrate hexahydrate (Zn(NO 3 ) 2 ·6H 2 O), 0.1504g (0.5mmol) of indium nitrate (In(NO 3 ) 3 ), 0.2420g (ie 2mmol) of L-cysteine ​​were dissolved in 30mL of deionized water, and after magnetic stirring for 10 minutes, the mixed solution was transferred to a hydrothermal reaction kettle, and put into the blast drying together with the hydrothermal reaction kettle In the box, hydrothermal reaction at 180°C for 18 hours, after cooling to room temperature, a yellow-green precipitate was obtained, and the yellow-green precipitate was washed with deionized water and ethanol by centrifugation, repeated washing 3 times, and dried in a blast drying oven at 60°C All night, get pure ZnIn 2 S 4 Photocatalytic nitrogen fixation catalyst.

Embodiment 2

[0033] Example 2 Zn containing Zn vacancies 1-x In 2 S 4 Preparation of Photocatalytic Nitrogen Fixation Catalyst

[0034] Under magnetic stirring conditions, 0.0595g (ie 0.2mmol) of zinc nitrate hexahydrate (Zn(NO 3 ) 2 ·6H 2 O), 0.1504g (0.5mmol) of indium nitrate (In(NO 3 ) 3 ), 0.2420g (ie 2mmol) of L-cysteine ​​were dissolved in 30mL of deionized water, and after magnetic stirring for 10 minutes, the mixed solution was transferred to a hydrothermal reaction kettle, and put into the blast drying together with the hydrothermal reaction kettle In the box, 200 °C hydrothermal reaction for 18 hours, after cooling to room temperature, a yellow-green precipitate was obtained, and the yellow-green precipitate was washed with deionized water and ethanol by centrifugation, repeated washing 3 times, and dried in a blast drying oven at 60 °C Over night, get Zn with Zn vacancies 1-x In 2 S 4 Photocatalytic nitrogen fixation catalyst.

Embodiment 3

[0035] Example 3 1% Fe 3+ Doped with Zn 1-x In 2 S 4 Preparation of Photocatalytic Nitrogen Fixation Catalyst

[0036] Under magnetic stirring conditions, 0.0595g (ie 0.2mmol) of zinc nitrate hexahydrate (Zn(NO 3 ) 2 ·6H 2 O), 0.1504g (0.5mmol) of indium nitrate (In(NO 3 ) 3 ), 0.2420g (ie 2mmol) of L-cysteine ​​were dissolved in 30mL deionized water, and then 0.0021g (ie 0.005mmol) of iron nitrate nonahydrate (Fe(NO 3 ) 3 9H 2 O), after magnetic stirring for 10 minutes, transfer the mixed solution to a hydrothermal reaction kettle, put it into a blast drying oven together with the hydrothermal reaction kettle, and conduct a hydrothermal reaction at 200°C for 18 hours. After cooling to room temperature, a yellow For the green precipitate, wash the yellow-green precipitate by centrifugation with deionized water and ethanol in turn. After repeated washing for 3 times, dry it overnight at 60°C in a blast drying oven to obtain 1% Fe 3+ Doped with Zn 1-x In 2 S 4 Phot...

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Abstract

The invention discloses a preparation method of a Mo or Fe doped Zn1-xIn2S4 catalyst for photocatalytic nitrogen fixation and ammonia synthesis. The method comprises the following steps: dissolving zinc nitrate hexahydrate, indium nitrate and L-cysteine into deionized water under a magnetic stirring condition, adding an inorganic salt containing molybdenum or iron, conducting magnetic stirring, transferring a mixed solution into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a blast drying oven together, and conducting drying to obtain a precursor; and carrying out hydrothermal reaction for 15-24 hours, conducting cooling to room temperature to obtain a yellow-green precipitate, washing the yellow-green precipitate with deionized water and ethanol in sequence, repeatedly carrying out centrifugal washing for 3-5 times, and conducting drying in a blast drying oven at the temperature of 60-100 DEG C for the whole night to obtain the Mo or Fe doped Zn1-xIn2S4photocatalytic nitrogen fixation catalyst. The Mo or Fe doped Zn1-xIn2S4 photocatalytic nitrogen fixation catalyst provided by the invention is high in nitrogen fixation efficiency and simple in preparation method, and has a good application prospect.

Description

technical field [0001] The invention relates to the field of photocatalysts, in particular to a Mo or Fe doped Zn for photocatalytic nitrogen fixation and synthesis of ammonia 1-x In 2 S 4 Catalyst preparation method. Background technique [0002] Ammonia is not only a widely used chemical raw material, but also serves as an important energy carrier. Ammonia synthesis by the Haber process is considered to be one of the greatest inventions of the 20th century and has made great contributions to the development of human society. At the same time, the ammonia synthesis process needs to consume 1%-2% of the world's total energy every year. Therefore, the development of green and clean ammonia synthesis methods has always been a hot topic in industry and academia worldwide. With the vigorous development of artificial photosynthetic solar fuel research, the use of solar photocatalysis to synthesize ammonia under mild conditions has attracted more and more researchers' inter...

Claims

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Application Information

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IPC IPC(8): B01J27/051C01C1/04C01C1/02
CPCB01J27/0515C01C1/026B01J35/39Y02P20/52
Inventor 董鹏玉罗虎关荣锋管瑞峰宋骏陆聪房维朱雷
Owner YANCHENG INST OF TECH
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