WO2023284064A1 - Procédé de préparation d'un catalyseur fe@cumoo4nwa/cu et application - Google Patents

Procédé de préparation d'un catalyseur fe@cumoo4nwa/cu et application Download PDF

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WO2023284064A1
WO2023284064A1 PCT/CN2021/113396 CN2021113396W WO2023284064A1 WO 2023284064 A1 WO2023284064 A1 WO 2023284064A1 CN 2021113396 W CN2021113396 W CN 2021113396W WO 2023284064 A1 WO2023284064 A1 WO 2023284064A1
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nwa
cumoo
catalyst
water
concentration
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PCT/CN2021/113396
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English (en)
Chinese (zh)
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薛晓东
冷艳秋
庄云飞
姜云鹏
李超
刘国祥
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山东省环境保护科学研究设计院有限公司
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Publication of WO2023284064A1 publication Critical patent/WO2023284064A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/054—Electrodes comprising electrocatalysts supported on a carrier
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
    • C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
    • C25B11/061—Metal or alloy
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/133—Renewable energy sources, e.g. sunlight

Definitions

  • the invention belongs to the technical field of inorganic nano-array catalysts, and in particular relates to a preparation method and application of a Fe@CuMoO 4 NWA/Cu catalyst.
  • Hydrogen energy that is, hydrogen, has become the most ideal secondary energy source to replace fossil energy because of its high calorific value per unit mass and its non-polluting products.
  • Electrocatalytic water splitting for hydrogen production is the use of electrical energy as the driving force for water splitting to produce hydrogen, which has received more and more attention.
  • electric energy is no longer only relying on the burning of fossil fuels, but can be directly generated in a variety of ways, and the stable electric energy obtained by using renewable energy (solar energy, wind energy, tidal energy, etc.) has no pollution to the environment. Since the overpotential of hydrogen production by electrolysis of water is very high, electrocatalysts are used to reduce the problem of excessive power consumption during the electrolysis process.
  • the present invention provides a method for preparing Fe@CuMoO nanowire arrays by redoxing Cu(OH) 2 nanowire arrays at room temperature on foamed copper, followed by hydrothermal ion exchange, and its electrocatalytic water splitting for hydrogen production Applications.
  • one of the purposes of the present invention is to propose a method for preparing Fe@CuMoO 4 NWA/Cu catalyst, comprising the following steps:
  • the molybdenum source reagent and the iron source reagent are dissolved in water to obtain a mixed solution, then Cu(OH) 2 NWA/Cu is added to the mixed solution, and the Fe@CuMoO 4 NWA/Cu catalyst is obtained by hydrothermal reaction.
  • the oxidant is ammonium persulfate or hydrogen peroxide
  • the molybdenum source reagent is one or more of sodium molybdate, ammonium molybdate tetrahydrate or lithium molybdate
  • the iron source reagent is iron sulfate , one or more of ferrous sulfate, ferric chloride, ferric nitrate or ferric oxide.
  • the immersion in the foamed copper is specifically: the immersion time of the foamed copper at room temperature is 0.5-30 minutes, and then cleaned several times.
  • the hydrothermal method is carried out at a temperature of 100-160° C. for 4-72 hours, and the obtained product is washed several times after the reaction.
  • the concentration of sodium hydroxide is 0.1-2 mol/L; the concentration of the ammonium persulfate dissolved in water is 0.1-2 mol/L; the peroxide
  • the mass concentration of hydrogen dissolved in water is 0.1-30%.
  • the molybdenum source reagent has a concentration of 0.1-2.0 mol/L
  • the iron source reagent has a concentration of 0.1-2.0 mol/L.
  • the second purpose of the present invention is to propose an application of Fe@CuMoO 4 NWA/Cu catalyst in electrocatalytic water splitting for hydrogen production.
  • the electrocatalytic water splitting hydrogen production is specifically as follows: using a three-electrode system, testing with an electrochemical workstation, using Fe@CuMoO 4 NWA/Cu as a working electrode, using a carbon rod as a counter electrode, and using Ag/AgCl or The Hg/HgO electrode is used as the reference electrode, and sodium hydroxide solution or sodium sulfate solution is used as the electrolyte to carry out the electrocatalytic hydrogen production reaction.
  • the present invention oxidizes copper into positive divalent Cu 2+ through the reasonable ratio of ammonium persulfate (NH 4 ) 2 S 2 O 8 and sodium hydroxide Na(OH), and the generated Cu 2+ immediately reacts with sodium hydroxide Na
  • the (OH) reaction generates nanowire arrays, thereby exposing more catalytically active sites, which is beneficial to the subsequent electrocatalytic process.
  • Adopting the technical solution of the present invention the synthesis of the Cu(OH) 2 NWA/Cu precursor is carried out at room temperature.
  • the precursor synthesized by this method Compared with the traditional high-temperature and high-pressure environment, the precursor synthesized by this method has the characteristics of low energy consumption and superior performance, and the improved The precursor material synthesized by this method has good stability and can better provide a good chemical reaction site for the next step of catalyst preparation.
  • Copper foam is a new multifunctional material with a large number of connected or disconnected pores evenly distributed in the copper matrix.
  • the present invention provides a method for preparing Fe-doped CuMoO 4 nanowire arrays Fe@CuMoO 4 NWA/Cu by hydrothermal ion exchange after preparing Cu(OH) 2 nanowire arrays on foamed copper at room temperature, exemplarily , see the following examples.
  • a preparation method of Fe@CuMoO 4 NWA/Cu catalyst exemplarily, 50mL deionized water is added in the clean beaker, ammonium persulfate is added (exemplarily, the concentration of ammonium persulfate after adding is 0.1mol /L) and sodium hydroxide (the concentration of sodium hydroxide after adding is 0.1mol/L), stirred for 30min to form a clear and transparent solution, after foam copper was pretreated by ultrasonic cleaning in hydrochloric acid solution, immersed in the clear and transparent solution, at room temperature After soaking for 5 minutes, after the reaction, the obtained product was rinsed with ultrapure water and ethanol for 3 to 5 times respectively to obtain a Cu(OH) 2 nanowire array Cu(OH) 2 NWA/Cu grown on foamed copper;
  • the polarization curve test is carried out in a three-electrode system.
  • the electrolyte is sodium sulfate solution.
  • the polarization curve test voltage range is -1.8 ⁇ 0V, the highest potential is 0V, and the lowest potential is -1.8 V, the start potential is 0V, the end potential is -1.8V, the scan rate is 0.005V/s, the sampling interval is 0.001V, the rest time is 2s, when the current density is 10mA/ cm2 , the required overpotential is 90mV (The lower the overpotential, the better the performance).
  • the application of the Fe@CuMoO 4 NWA/Cu catalyst prepared based on the above method in electrocatalytic hydrogen production is exemplarily tested by an electrochemical workstation, with Fe@CuMoO 4 NWA/Cu as the working electrode and carbon rod as the For the counter electrode, the Ag/AgCl or Hg/HgO electrode is used as the reference electrode, and the long-term electrocatalytic water splitting hydrogen production rate is tested in the three-electrode system.
  • the production rate is 1mol/h
  • the electrolyte is sodium sulfate solution.
  • the potential was set at 90 mV (relative to reversible hydrogen potential, vs. RHE) and the run time was 1 hour.
  • a preparation method of Fe@CuMoO 4 NWA/Cu catalyst Exemplarily, 50mL deionized water is added to a cleaned beaker, and ammonium persulfate is added (exemplarily, the concentration of ammonium persulfate after adding is 2mol/ L) and sodium hydroxide (concentration 2mol/L of sodium hydroxide after adding), stir 30min to form clear and transparent solution, the foam copper of pretreatment is immersed in the above-mentioned solution, soak 10min at room temperature, after reaction finishes, will obtain The product was washed with ultrapure water and ethanol for 3 to 5 times respectively to obtain Cu(OH) 2 nanowire array Cu(OH) 2 NWA/Cu grown on foamed copper;
  • the hydrothermal reaction kettle has a stainless steel shell and a polytetrafluoroethylene lining, and puts Cu(OH) 2 NWA/Cu, 0.5g iron sulfate (concentration: 2.0mol/L), and 35mL ultrapure water. After sealing the hydrothermal autoclave, it was placed in an oven at 100 °C for 48 hours. After natural cooling, it was washed with deionized water and absolute ethanol, and dried in vacuum to obtain Fe@CuMoO 4 NWA/Cu.
  • the polarization curve test is carried out in a three-electrode system.
  • the electrolyte is sodium sulfate solution.
  • the polarization curve test voltage range is -1.8 ⁇ 0V, the highest potential is 0V, and the lowest potential is -1.8 V, the start potential is 0V, the end potential is -1.8V, the scan rate is 0.005V/s, the sampling interval is 0.001V, the rest time is 2s, when the current density is 10mA/ cm2 , the required overpotential is 86mV .
  • the long-term electrocatalytic water splitting hydrogen yield was tested in a three-electrode system.
  • the electrolyte was sodium sulfate solution, and the potential was set to 86mV (relative to the reversible hydrogen potential, vs. RHE) run time is 1 hour.
  • the application of the Fe@CuMoO 4 NWA/Cu catalyst prepared based on the above method in electrocatalytic hydrogen production is exemplarily tested by an electrochemical workstation, with Fe@CuMoO 4 NWA/Cu as the working electrode and carbon rod as the For the counter electrode, the Ag/AgCl or Hg/HgO electrode is used as the reference electrode, and the long-term electrocatalytic water splitting hydrogen production rate is tested in the three-electrode system.
  • the production rate is 0.8mol/h.
  • the electrolyte is sodium sulfate solution.
  • the potential was set at 85 mV (relative to the reversible hydrogen potential, vs. RHE) and the run time was 1 hour.
  • the electrolytic cell for electrocatalytic hydrogen production is connected with the barometer sensor, the real-time pressure data in the pressure gauge is output on the computer, and the amount of the gas is calculated by the Clapeyron equation, and then the catalyst is calculated.
  • the faradaic efficiency of hydrogen production in electrocatalytic water splitting is 99.3%.
  • the polarization curve test is carried out in a three-electrode system.
  • the electrolyte is sodium sulfate solution.
  • the polarization curve test voltage range is -1.8 ⁇ 0V, the highest potential is 0V, and the lowest potential is -1.8 V, the start potential is 0V, the end potential is -1.8V, the scan rate is 0.005V/s, the sampling interval is 0.001V, the rest time is 2s, when the current density is 10mA/ cm2 , the required overpotential is 70mV .
  • the application of the Fe@CuMoO 4 NWA/Cu catalyst prepared based on the above method in electrocatalytic hydrogen production is exemplarily tested by an electrochemical workstation, with Fe@CuMoO 4 NWA/Cu as the working electrode and carbon rod as the For the counter electrode, the Ag/AgCl or Hg/HgO electrode is used as the reference electrode, and the long-term electrocatalytic water splitting hydrogen production rate is tested in the three-electrode system, and the electrolyte is sodium sulfate solution.
  • the potential was set at 70 mV (relative to the reversible hydrogen potential, vs. RHE) and the run time was 1 hour.
  • the polarization curve test is carried out in a three-electrode system.
  • the electrolyte is sodium sulfate solution.
  • the polarization curve test voltage range is -1.8 ⁇ 0V, the highest potential is 0V, and the lowest potential is -1.8 V, the start potential is 0V, the end potential is -1.8V, the scan rate is 0.005V/s, the sampling interval is 0.001V, the rest time is 2s, when the current density is 10mA/ cm2 , the required overpotential is 70mV .
  • the application of the Fe@CuMoO 4 NWA/Cu catalyst prepared based on the above method in electrocatalytic hydrogen production is exemplarily tested by an electrochemical workstation, with Fe@CuMoO 4 NWA/Cu as the working electrode and carbon rod as the For the counter electrode, the Ag/AgCl or Hg/HgO electrode is used as the reference electrode, and the long-term electrocatalytic water splitting hydrogen production rate is tested in the three-electrode system.
  • the electrolyte is a sodium sulfate solution, and the potential is set to 70mV (relative to the reversible Hydrogen potential, vs. RHE) run time was 1 hour.
  • the polarization curve test is carried out in a three-electrode system.
  • the electrolyte is sodium sulfate solution.
  • the polarization curve test voltage range is -1.8 ⁇ 0V, the highest potential is 0V, and the lowest potential is -1.8 V, the start potential is 0V, the end potential is -1.8V, the scan rate is 0.005V/s, the sampling interval is 0.001V, the rest time is 2s, when the current density is 10mA/ cm2 , the required overpotential is 85mV .
  • the copper foam has good conductivity, which is helpful for electron transport during the catalytic process, and the Fe@CuMoO 4 nanowire array structure exposes a higher active area, which helps to improve the catalytic efficiency.
  • the application of the Fe@CuMoO 4 NWA/Cu catalyst prepared based on the above method in electrocatalytic hydrogen production is exemplarily tested by an electrochemical workstation, with Fe@CuMoO 4 NWA/Cu as the working electrode and carbon rod as the
  • the Ag/AgCl or Hg/HgO electrode is used as the reference electrode, and the long-term electrocatalytic water splitting hydrogen production rate is tested in the three-electrode system, and the electrolyte is sodium sulfate solution.
  • the potential was set at 70 mV (relative to reversible hydrogen potential, vs. RHE) and the run time was 1.5 hours.

Abstract

Un procédé de préparation d'un réseau de nanofils de CuMoO4 dopés au fer sur un catalyseur de mousse de cuivre (Fe@CuMoO4NWA/Cu), ainsi qu'une application. Le procédé comprend les étapes suivantes consistant : à dissoudre un oxydant et de l'hydroxyde de sodium dans de l'eau, puis à immerger la mousse de cuivre dans ce dernier pour obtenir un réseau de nanofils de Cu(OH)2 formés sur de la mousse de cuivre (Cu(OH)2NWA/Cu); et à dissoudre un réactif source de molybdène et un réactif source de fer dans de l'eau pour obtenir une solution mixte, puis à ajouter le Cu(OH)2NWA/Cu dans la solution mixte, et à utiliser un procédé hydrothermique de réaction pour obtenir un catalyseur Fe@CuMoO4NWA/Cu. La synthèse du précurseur Cu(OH)2NWA/Cu est effectuée à température ambiante; par rapport à un environnement classique à haute température et haute pression, le précurseur synthétisé par ce procédé présente des caractéristiques telles qu'une faible consommation d'énergie et d'excellentes propriétés; et le matériau précurseur synthétisé par ce procédé présente une bonne stabilité, et peut constituer un meilleur lieu de réaction chimique pour l'étape suivante de préparation de catalyseur.
PCT/CN2021/113396 2021-07-16 2021-08-19 Procédé de préparation d'un catalyseur fe@cumoo4nwa/cu et application WO2023284064A1 (fr)

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CN202110807984.4 2021-07-16

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Cited By (1)

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CN116393138A (zh) * 2023-04-20 2023-07-07 河南师范大学 一种用于硝酸根还原转氨的铜镍锡纳米金属玻璃催化剂的制备方法

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Publication number Priority date Publication date Assignee Title
CN116393138A (zh) * 2023-04-20 2023-07-07 河南师范大学 一种用于硝酸根还原转氨的铜镍锡纳米金属玻璃催化剂的制备方法
CN116393138B (zh) * 2023-04-20 2024-04-05 河南师范大学 一种用于硝酸根还原转氨的铜镍锡纳米金属玻璃催化剂的制备方法

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