Preparation method and electrocatalytic nitrogen reduction applications of vanadium-doped ferrous sulfide

A ferrous sulfide and sulfidation reaction technology, applied in chemical instruments and methods, physical/chemical process catalysts, electrodes, etc., can solve problems such as poor selectivity

Active Publication Date: 2019-09-06
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Unfortunately, the d-orbital electrons of transition metals also favor the formation of met

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Step 1: Take a 50 mL hydrothermal autoclave for laboratory use, and the hydrothermal autoclave has a polytetrafluoroethylene liner. Take 10 mL of acetylacetone, 10 mL of glycerin, and 20 mL of absolute ethanol into a 50 mL polytetrafluoroethylene liner, and then add ferric ammonium sulfate (0.4788 g, 1.8 mmol), vanadyl acetylacetonate ( 0.0696 g, 0.2 mmol) was stirred overnight to fully dissolve and then transferred to a polytetrafluoroethylene liner. After sealing the hydrothermal autoclave, it was placed in an electric blast drying oven at 150 °C for 30 h. After natural cooling, centrifugal washing with absolute ethanol and vacuum drying to obtain iron vanadium precursor nanopowder.

[0019] Step 2: Take 40 mL of absolute ethanol in a polytetrafluoroethylene liner, add 50 mg of iron vanadium precursor and 1000 mg of thiourea in turn under magnetic stirring, and continue stirring for 2 h to obtain a vulcanization reaction solution. After sealing the hydrothermal reac...

Embodiment 2

[0029] Step 1: Take a 50 mL hydrothermal autoclave for laboratory use, and the hydrothermal autoclave has a polytetrafluoroethylene liner. Add 10 mL of ethylene glycol and 30 mL of isopropanol into a 50 mL polytetrafluoroethylene liner, and add ferric nitrate nonahydrate (0.3232 g, 0.8 mmol) and ammonium metavanadate (0.04680 g, 0.4 mmol) was stirred overnight and transferred to a polytetrafluoroethylene liner after fully dissolving. After sealing the hydrothermal autoclave, it was placed in an electric blast drying oven at 170 °C for 24 h. After natural cooling, centrifugal washing with absolute ethanol and vacuum drying to obtain iron vanadium precursor nanopowder.

[0030] Step 2: Take 40 mL of absolute ethanol in a polytetrafluoroethylene liner, add 50 mg of iron vanadium precursor and 750 mg of potassium thiocyanate in turn under magnetic stirring, and continue stirring for 2 h to obtain a vulcanization reaction solution. After sealing the hydrothermal reactor, place it...

Embodiment 3

[0040] Step 1: Take a 50 mL hydrothermal autoclave for laboratory use, and the hydrothermal autoclave has a polytetrafluoroethylene liner. Add 6 mL of glycerol and 34 mL of isopropanol into a 50 mL polytetrafluoroethylene liner, add ferric sulfate (0.7997 g, 2.0 mmol) and sodium vanadate (0.1103 g, 0.6 mmol) in turn under magnetic stirring and stir overnight Once fully dissolved, transfer it to a Teflon liner. After sealing the hydrothermal autoclave, it was placed in an electric blast drying oven at 190 °C for 15 h. After natural cooling, centrifugal washing with absolute ethanol and vacuum drying to obtain iron vanadium precursor nanopowder.

[0041] Step 2: Take 40 mL of absolute ethanol in a polytetrafluoroethylene liner, add 50 mg of iron vanadium precursor and 500 mg of thioacetamide in sequence under magnetic stirring, and continue stirring for 2 h to obtain a vulcanization reaction solution. After sealing the hydrothermal reactor, place it at 180 o C. Insulate in an...

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Abstract

In the prior art, ammonia (NH3) as the important raw material industry, agriculture and pharmacy plays an important role in human life and development, and the huge industrial ammonia production process and the release of a large amount of carbon dioxide greatly increase the greenhouse effect, such that the production of ammonia through electrocatalytic nitrogen reduction under mild conditions isthe research focus worldwide. Based on the problem in the prior art, the present invention provides a preparation method and electrocatalytic nitrogen reduction applications of vanadium-doped ferroussulfide nanometer powder, wherein the preparation method comprises: adding an iron source reagent and a vanadium source reagent to a special solvent to prepare a pre-reaction liquid, heating the pre-reaction liquid to obtain iron-vanadium precursor nanometer powder, and carrying out a vulcanization reaction on the iron-vanadium precursor nanometer powder to finally obtain the vanadium-doped ferrous sulfide nanometer powder. According to the present invention, the vanadium-doped ferrous sulfide nanometer powder has excellent activity in the field of production of ammonia through electrocatalytic nitrogen reduction (NRR), the yield of ammonia at -0.1 V (relative standard hydrogen electrode) is up to 106.3 [mu]g h<-1>mg<-1>cat, and the Faraday efficiency achieves 9.5%.

Description

technical field [0001] The invention relates to the field of preparation and application of inorganic nanopowder, in particular to a method for preparing vanadium-doped ferrous sulfide nanopowder based on a solvothermal method and its application in the field of electrocatalytic nitrogen reduction. Background technique [0002] With the progress of the times and the development of science and technology, the world today is increasingly dependent on energy. Considering the scarcity of fossil energy and the environmental pollution caused by its energy release process, it is necessary to explore novel, cheap, non-toxic, Recyclable new energy has become the focus of current research. Ammonia, as an important chemical raw material, plays an irreplaceable role in human progress, and it has attracted widespread attention as an efficient energy carrier. The current industrial method for preparing ammonia is the traditional Haber-Bosch method (more than 500 tons of ammonia are prepa...

Claims

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Application Information

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IPC IPC(8): B01J27/043C25B1/00C25B11/06
CPCB01J27/043B01J35/0033C25B1/00C25B11/075
Inventor 孙旭郭成英高令峰马晓晶赵明珠魏琴
Owner UNIV OF JINAN
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