Sulfur defect-rich sulfurized ferrophosphorus nanosheet as well as preparation method and application thereof

A technology for ferric phosphorus sulfide and nanosheets, which is applied in the preparation/separation of ammonia, chemical instruments and methods, phosphorus compounds of phosphorus sulfur/selenium/tellurium, etc., can solve the problems of low yield, complicated preparation process, etc. High performance, good reproducibility and considerable yield

Inactive Publication Date: 2020-08-28
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Aiming at the disadvantages of complex preparation process and low yield in the glass method of ferrophosphorus sulfide in the prior art, the present invention provides a phosphorus sulfide with high efficiency, controllable cost, high catalytic activity, suitable for large-scale production, and rich in sulfur defects. Preparation method of iron nanosheets

Method used

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  • Sulfur defect-rich sulfurized ferrophosphorus nanosheet as well as preparation method and application thereof
  • Sulfur defect-rich sulfurized ferrophosphorus nanosheet as well as preparation method and application thereof
  • Sulfur defect-rich sulfurized ferrophosphorus nanosheet as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0039] 1. Preparation of bulk ferrophosphorus sulfide

[0040] (1) Mix iron powder, phosphorus powder and sulfur powder according to the molar ratio of 1:1:3. After fully mixing and grinding, seal the mixed powder in a vacuum quartz glass tube;

[0041] (2) Heat the above-mentioned quartz glass tube with sealed mixed powder in a tube furnace at a temperature of 650°C for 120 hours at a heating rate of 5°C / min, and cool it down to room temperature naturally after heating to obtain massive phosphorous sulfide iron crystals.

[0042] 2. Electrochemical stripping

[0043] Fix the massive iron phosphorus sulfide on the copper sheet as the working electrode, use platinum wire as the counter electrode, and use N-methylpyrrolidone solution containing 5 mg / mL tetrabutylammonium bromide as the electrolyte to make the massive phosphorus sulfide Immerse the iron and platinum sheets into the electrolyte; continuously apply a negative voltage of -6V to the working electrode for 10 hours t...

Embodiment 2

[0061] 1. Preparation of bulk ferrophosphorus sulfide

[0062] (1) Mix iron powder, phosphorus powder and sulfur powder according to the molar ratio of 1:1:3. After fully mixing and grinding, seal the mixed powder in a vacuum quartz glass tube;

[0063] (2) Heat the above-mentioned quartz glass tube with sealed mixed powder in a tube furnace at a temperature of 650°C for 120 hours at a heating rate of 5°C / min, and cool it down to room temperature naturally after heating to obtain massive phosphorous sulfide iron crystals.

[0064] 2. Electrochemical stripping

[0065] Fix the massive iron phosphorus sulfide on the copper sheet as the working electrode, use platinum wire as the counter electrode, and use N-methylpyrrolidone solution containing 5 mg / mL tetrabutylammonium bromide as the electrolyte to make the massive phosphorus sulfide Immerse the iron and platinum sheets into the electrolyte; continuously apply a negative voltage of -4V to the working electrode for 10 hours t...

Embodiment 3

[0081] 1. Preparation of bulk ferrophosphorus sulfide

[0082] (1) Mix iron powder, phosphorus powder and sulfur powder according to the molar ratio of 1:1:3. After fully mixing and grinding, seal the mixed powder in a vacuum quartz glass tube;

[0083] (2) Heat the above-mentioned quartz glass tube with sealed mixed powder in a tube furnace at a temperature of 650°C for 120 hours at a heating rate of 5°C / min, and cool it down to room temperature naturally after heating to obtain massive phosphorous sulfide iron crystals.

[0084] 2. Electrochemical stripping

[0085] Fix the massive iron phosphorus sulfide on the copper sheet as the working electrode, use platinum wire as the counter electrode, and use N-methylpyrrolidone solution containing 5 mg / mL tetrabutylammonium bromide as the electrolyte to make the massive phosphorus sulfide Immerse the iron and platinum sheets into the electrolyte; continuously apply a negative voltage of -8V to the working electrode for 10 hours t...

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Abstract

The invention relates to the technical field of catalysts. The invention discloses a sulfur defect-rich sulfurized ferrophosphorus nanosheet as well as a preparation method and application thereof. The preparation method includes following steps: stripping the blocky phosphorus sulfide into phosphorus sulfide nanosheets by adopting an electrochemical stripping method; respectively carrying out low-speed centrifugal separation and high-speed centrifugal separation; washing and drying the product, and calcining the product to obtain a phosphorus sulfide nanosheet rich in sulfur defects. According to the invention, the nanosheet has good electrochemical performance and stability, when the nanosheet is applied to electrochemical nitrogen fixation ammonia synthesis, the maximum ammonia synthesis rate can reach 6.27 [mu]g*h<-1>mg<-1>cat; the preparation method has the advantages of being simple, efficient, low in cost, high in controllability, good in reproducibility and suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to iron phosphorus sulfide nanosheets rich in sulfur defects and a preparation method and application thereof. Background technique [0002] Ammonia is an important raw material for the manufacture of fertilizers, polymers, dyes and explosives. It is not only one of the most produced and widely used chemicals in the world, but also considered as a potential carrier of green energy and a potential transportation fuel, which can Response to the future global energy crisis. At present, the industry mainly uses the Haber method to carry out large-scale reaction of nitrogen and hydrogen to synthesize ammonia under high temperature and high pressure conditions, which consumes a lot of energy and emits a lot of CO 2 Greenhouse gases. In recent years, electrochemical ammonia synthesis technology has been considered as an important means to solve these problems. Compared with the traditi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/00C01B25/14C01C1/04
CPCC01B25/14C01C1/0411C01G49/009C01P2002/72C01P2002/86C01P2004/03C01P2004/04C01P2004/20C01P2006/40
Inventor 侯阳王晗杨彬雷乐成
Owner ZHEJIANG UNIV
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