Preparation of nano spherical sulfur-doped iron oxide and application in electrocatalytic nitrogen reduction

A sulfur-doped, iron oxide nanotechnology, applied in physical/chemical process catalysts, electrodes, electrolysis processes, etc., can solve problems such as inhibition

Inactive Publication Date: 2020-04-28
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, Sun Xuping's research group reported that density functional calculation (DFT) and experimental results have confirmed that molybdenum disulfide can be used as an excellent electrocatalytic nitrogen reduction catalyst for 0.1 M Na 2 SO 4 In the electrolyte, however, the high HER activi...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Step 1: Take a 50 mL hydrothermal reaction kettle for laboratory use. The hydrothermal reaction kettle has a stainless steel shell and a polytetrafluoroethylene liner. Take 40 mL of 0.5 mol / L ammonia water and add it to a 50 mL polytetrafluoroethylene liner, add p-aminobenzoic acid (0.0549 g, 0.4 mmol) under magnetic stirring, and continue stirring until a colorless and transparent solution is formed. Then, thiourea (0.5 g, 6.569 mmol) and ferric nitrate nonahydrate (0.2412 g, 1.0 mmol) were added in sequence, and stirred until fully dissolved, then the hydrothermal autoclave was sealed and placed in an oven at 160 °C for 13 h. After natural cooling, wash with deionized water and absolute ethanol for several times, and finally place at 60 o In vacuum drying, black sulfur-doped iron oxide nanopowders were obtained after 12 h.

[0019] The second step: the application of sulfur-doped iron oxide nanopowder electrocatalytic ammonia production

[0020] 1. Weigh 5 mg of su...

Embodiment 2

[0030] Step 1: Take a 50 mL hydrothermal reaction kettle for laboratory use. The hydrothermal reaction kettle has a stainless steel shell and a polytetrafluoroethylene liner. Take 40 mL of 0.5 mol / L ammonia water and add it to a 50 mL polytetrafluoroethylene liner, add p-aminobenzoic acid (0.0549 g, 0.4 mmol) under magnetic stirring, and continue stirring until a colorless and transparent solution is formed. Then, add sodium sulfide (0.4995 g, 6.400 mmol) and ferric nitrate nonahydrate (0.2412 g, 1.0 mmol) in sequence, stir until they are fully dissolved, then seal the hydrothermal autoclave, and place it in an oven at 180 °C for reaction 12 h. After natural cooling, they were washed several times by centrifugation with deionized water and absolute ethanol, and finally, placed in a vacuum oven at 60 °C for 12 h to obtain black sulfur-doped iron oxide nanopowders.

[0031] The second step: the application of sulfur-doped iron oxide nanopowder electrocatalytic ammonia productio...

Embodiment 3

[0041] Step 1: Take a 50 mL hydrothermal reaction kettle for laboratory use. The hydrothermal reaction kettle has a stainless steel shell and a polytetrafluoroethylene liner. Add 40 mL of 0.5 mol / L ammonia water into a 50 mL polytetrafluoroethylene liner, add p-aminobenzoic acid (0.0480 g, 0.35 mmol) under magnetic stirring and continue stirring until a colorless and transparent solution is formed, then add sodium sulfide ( 0.4995 g, 6.400 mmol), ferric trioxide hexahydrate (0.136 g, 1.0 mmol), continue until fully dissolved, seal the hydrothermal autoclave, and place it in an oven at 200 °C for 15 h. After natural cooling, they were washed several times by centrifugation with deionized water and absolute ethanol, and finally, placed in a vacuum oven at 60 °C for 12 h to obtain black sulfur-doped iron oxide nanopowders.

[0042] The second step: the application of sulfur-doped iron oxide nanopowder electrocatalytic ammonia production

[0043] 1. Weigh 5 mg of sulfur-doped iro...

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Abstract

The invention provides a preparation method of nano spherical sulfur-doped iron oxide nano-powder and application of the nano spherical sulfur-doped iron oxide nano-powder in electrocatalytic nitrogenreduction. The method comprises the following steps: firstly, adding a sulfur source and an iron source into a high-temperature and high-pressure reaction kettle to prepare pre-reaction liquid; heating the pre-reaction liquid to react for a certain time; cooling, washing, drying in vacuum, and collecting to obtain the nano spherical sulfur-doped iron oxide nano powder. The sulfur-doped iron oxideshows excellent catalytic activity in the field of electrocatalytic nitrogen reduction (NRR), the ammonia yield under -0.2 V (relative to a standard hydrogen electrode) is as high as 30.6 [mu]g.h <-1>.mg<cat.><-1>, and meanwhile, the Faraday efficiency reaches 1.3%.

Description

technical field [0001] The invention relates to the field of preparation of inorganic nano-powder and the application field of electrocatalytic nitrogen reduction, in particular to a method for preparing nano-spherical sulfur-doped iron oxide nano-powder based on a hydrothermal method and its application in the field of electrocatalytic nitrogen reduction. Background technique [0002] Ammonia, as an efficient and non-polluting energy carrier and the main raw material of chemical fertilizers, its output greatly affects the development of society and the progress of human beings. With the rapid growth of the world's population today, the demand for chemical fertilizers is increasing worldwide. In addition, the limitation of fossil fuels as the main energy supply and the pollution of the environment make the further development of human beings face major problems. Therefore, the development of clean, efficient, and recyclable new energy sources and energy storage materials ha...

Claims

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Application Information

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IPC IPC(8): B01J27/043B01J35/08C25B1/00C25B11/06
CPCB01J27/043B01J35/08C25B1/00C25B11/091
Inventor 孙旭赵明珠高令峰郭成英马晓晶
Owner UNIV OF JINAN
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