WO2023082409A1 - Catalyseur à base de cuivre et électrode pour réduction catalytique électrochimique du dioxyde de carbone et pour stockage de l'énergie, procédé de préparation associé et son application - Google Patents

Catalyseur à base de cuivre et électrode pour réduction catalytique électrochimique du dioxyde de carbone et pour stockage de l'énergie, procédé de préparation associé et son application Download PDF

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WO2023082409A1
WO2023082409A1 PCT/CN2021/138135 CN2021138135W WO2023082409A1 WO 2023082409 A1 WO2023082409 A1 WO 2023082409A1 CN 2021138135 W CN2021138135 W CN 2021138135W WO 2023082409 A1 WO2023082409 A1 WO 2023082409A1
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copper
electrode
based catalyst
carbon dioxide
energy storage
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PCT/CN2021/138135
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Chinese (zh)
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夏霖
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深圳先进技术研究院
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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
    • 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
    • C25B11/095—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 at least one of the compounds being organic
    • 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
    • C25B3/00—Electrolytic production of organic compounds
    • C25B3/01—Products
    • C25B3/03—Acyclic or carbocyclic hydrocarbons
    • 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
    • C25B3/00—Electrolytic production of organic compounds
    • C25B3/01—Products
    • C25B3/07—Oxygen containing compounds
    • 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
    • C25B3/00—Electrolytic production of organic compounds
    • C25B3/20—Processes
    • C25B3/25—Reduction
    • C25B3/26—Reduction of carbon dioxide
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/38—Electroplating: Baths therefor from solutions of copper
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces

Definitions

  • the invention relates to the technical field of electric energy storage, in particular to a carbon dioxide reduction energy storage method driven by new energy electric energy.
  • Electrochemical catalytic processes are considered to be a reliable solution for the efficient integration of renewable resources such as wind and solar energy into the current carbon-neutral energy mix.
  • the scheme aims to use electrocatalysts combined with carbon dioxide, activated by electrical energy, to reduce carbon dioxide into fuels such as methanol, ethanol and methane, and store these fuels until they are reconverted during periods of high power consumption.
  • fuels such as methanol, ethanol and methane
  • Nickel-based catalysts are widely used in the reduction of carbon dioxide to methane due to their low cost and easy availability. However, even at low temperatures, nickel catalysts may be deactivated due to sintering of nickel particles, formation of mobile nickel carbonylenes, or formation of carbon deposits. In addition, active metals Rh, Co, Fe, etc. have also been reported as effective catalysts for carbon dioxide reduction to methane, but the high cost of these catalysts limits their industrial applications.
  • copper-based catalysts are cheaper and are the most effective catalysts for reducing carbon dioxide to hydrocarbons. They have advantages in improving the selectivity of carbon dioxide conversion products, and are also the most effective for carbon dioxide methanation and industrialized electric energy storage. means. By modifying the copper-based catalyst with chemical small molecules, not only the reaction rate can be increased, but also the formation of methane on the copper-based surface can be further promoted by suppressing the hydrogen evolution reaction.
  • the current research has encountered difficulties.
  • the key parameters of energy storage efficiency in the process of electrochemical reduction of carbon dioxide energy storage that is, the Faraday efficiency is insufficient, and the energy input loss is large; the second is the lack of energy storage products after reduction. Specificity, it is difficult to form a homogeneous product with high purity.
  • the traditional chemical small molecule is used to modify the copper electrode, although the conversion efficiency of carbon dioxide can be increased, the copper catalyst is prone to be desorbed from the electrode during use, and then removed with the liquid flow in the electrolytic cell, resulting in an effective Less catalyst and lower Faradaic efficiency.
  • the technical problem to be solved by the present invention is to provide a catalyst for electrochemical catalytic carbon dioxide reduction energy storage driven by new energy and electric energy, using a brand-new modification group to modify the copper-based catalyst as an electrochemical catalytic electrode to improve the catalytic efficiency of the existing copper-based catalyst And Faraday efficiency, reduce the loss of input energy, and realize the efficient storage of electric energy.
  • the present invention provides a copper-based catalyst for electrochemically catalytic carbon dioxide reduction energy storage driven by new energy electric energy.
  • the copper-based catalyst is composed of copper nanoparticles and a modified polymer, and the modified polymer is proton conductive Polymers with side chains and electronically conductive backbones.
  • the electronically conductive main chain has more than one conjugated group, and the conjugated group may be an alkenyl group or an aromatic conjugated group.
  • the proton conductive side chain is preferably a side chain containing a sulfonic acid group or a side chain containing a phosphoric acid group.
  • the polymer is further polystyrene sulfonic acid (PSS), polybutadiene sulfonic acid, polyaniline with camphor sulfonic acid as a dopant.
  • PSS polystyrene sulfonic acid
  • polybutadiene sulfonic acid polybutadiene sulfonic acid
  • polyaniline with camphor sulfonic acid as a dopant.
  • the present invention also provides an electrochemical catalytic carbon dioxide reduction energy storage electrode driven by new energy, which includes: an electrode substrate and the above-mentioned copper-based catalyst, and the copper-based catalyst can be prepared as a coating and coated on the electrode substrate .
  • the thickness of the coating formed by the copper-based catalyst is 2 ⁇ m-25 ⁇ m, more preferably 8 ⁇ m-20 ⁇ m.
  • the present invention also provides a method for preparing an electrochemical electrode using the above-mentioned copper-based catalyst, which includes: preparing the electrochemical catalytic electrode by using an in-situ co-deposition method or a coating method.
  • the in-situ co-deposition method further specifically includes: the first step, the preparation of an electroplating solution, the electroplating solution includes a CuSO 4 solution, the above-mentioned modified polymer, Na 2 SO 4 and H 2 SO 4 , and the above-mentioned components are prepared according to proportions mixed together;
  • the electrode base material is put into the above-mentioned electroplating solution, and electroplating is performed by an electroplating method.
  • the concentration of the modifying polymer is preferably 1 ⁇ M-200 ⁇ M.
  • the present invention also provides the application of the above reduction energy storage electrode in realizing carbon dioxide reduction energy storage.
  • the invention adopts a brand-new modification group to modify the copper-based catalyst as an electrochemical catalytic electrode, uses new energy to drive electrochemical catalytic carbon dioxide reduction energy storage, improves the catalytic efficiency and Faraday efficiency of the existing copper-based catalyst, reduces the loss of input energy, and realizes electric energy efficient storage.
  • the copper-based catalyst is modified by a polymer modification group with a special structure, and the hydrophilicity and hydrophobicity of the polymer side chain affect the protonation process of the CO2 reduction reaction and the diffusion process of CO2 on the electrode surface, both It will further regulate the efficiency of the reaction and the product.
  • the chemical properties of the polymer polymer side chains provided by the present invention regulate the reduction of CO2 on the Cu surface, since the polymers used contain proton-conducting side chains, such as those containing sulfonic acid groups or containing phosphoric acid groups
  • the side chain can effectively increase the concentration of CO radicals on the surface of the Cu electrode and the surface pH value in the reaction system. While regulating the catalytic activity, it also significantly regulates the formation of products, making the entire reaction easy to form methane.
  • the electronically conductive main chain of the polymer provided by the present invention has more than one conjugated group, and the conjugated group can be an alkenyl group, an aromatic conjugated group, etc., which can significantly reduce the electrode interface impedance and improve the conversion into methane Faraday efficiency and catalytic current density (catalytic efficiency).
  • the present invention provides a copper-based catalyst for electrochemically catalytic carbon dioxide reduction energy storage driven by new energy.
  • the copper-based catalyst is obtained by electroplating copper nanoparticles and modified polymers.
  • the modified polymer The polymer is a polymer with a proton-conducting side chain and an electron-conducting main chain.
  • the electronically conductive main chain has more than one conjugated group, and the conjugated group may be an alkenyl group or an aromatic conjugated group, more preferably a butadienyl group.
  • the proton conductive side chain is preferably a side chain containing a sulfonic acid group or a side chain containing a phosphoric acid group.
  • the polymer is further preferably polystyrenesulfonic acid (PSS), polybutadienesulfonic acid, polybutadienesulfonate, polyaniline with camphorsulfonic acid as a dopant.
  • PSS polystyrenesulfonic acid
  • polybutadienesulfonic acid polybutadienesulfonate
  • polyaniline with camphorsulfonic acid as a dopant.
  • the copper-based catalyst can be prepared as a coating and coated on the electrode substrate to prepare an electrochemical catalytic electrode.
  • the electrode substrate can be selected from carbon material electrodes, carbon material composite electrodes, noble metal electrodes, stainless steel electrodes, copper electrodes, iron electrodes, etc. .
  • the carbon material electrode can further be a graphite electrode, a carbon fiber electrode, a graphene electrode, a carbon nanotube electrode, a diamond electrode, and the like.
  • the noble metal electrode may further be selected from gold, silver, platinum and the like.
  • the coating thickness is preferably 2 ⁇ m-25 ⁇ m, more preferably 8 ⁇ m-20 ⁇ m.
  • the copper-based catalyst can also directly modify the above-mentioned polymer on the copper electrode to prepare an electrochemical catalytic electrode.
  • the present invention adopts an in-situ co-deposition method or a coating method to prepare an electrochemical catalytic electrode, and the in-situ co-deposition method is more preferred. Further preferably, the in-situ co-electrodeposition method can be used to deposit the polymer on the copper electrode, which can keep the polymer molecules on the surface of the electrode and avoid the problem of desorption from the copper electrode.
  • the present invention also provides a preparation method for the above-mentioned electrochemical catalytic electrode, which adopts an in-situ co-deposition method, specifically comprising:
  • the first step is the preparation of the electroplating solution
  • the electroplating solution includes CuSO 4 solution, the above-mentioned modified polymer, Na 2 SO 4 , H 2 SO 4 , and the above-mentioned components are mixed together in proportion;
  • the electrode base material is put into the above-mentioned electroplating solution, and electroplating is performed by an electroplating method.
  • the concentration of the CuSO 4 solution is preferably 1mM-10mM, more preferably 1mM-5mM.
  • the concentration of the modifying polymer is preferably 1 ⁇ M-200 ⁇ M, more preferably 10 ⁇ M-100 ⁇ M, even more preferably 10 ⁇ M-20 ⁇ M.
  • the concentration of the Na 2 SO 4 solution is preferably 0.01M-0.2M, more preferably 0.05M-0.1M.
  • the concentration of the H 2 SO 4 solution is preferably 0.1M-1M, more preferably 0.3M-0.5M.
  • the current density in the second step is preferably (-0.5mA/cm 2 )-(-10mA/cm 2 ), more preferably (-2mA/cm 2 )-(-6mA/cm 2 ).
  • the present invention also provides a new energy-driven electrochemical catalytic carbon dioxide reduction energy storage system, which includes: the above-mentioned electrochemical catalytic electrode as a cathode, an electrolyte, and an anode.
  • the anode can be an inert metal electrode or a carbon electrode.
  • the electrolyte solution can be KHCO 3 , NaHCO 3 , etc., and the concentration is between 0.05M-2M, more preferably between 0.05M-1M.
  • the present invention also provides a new energy-driven electrochemical catalytic carbon dioxide reduction energy storage method, which includes:
  • the first step is to pass the carbon dioxide gas source into the system electrolyte until saturated
  • the second step is to use new energy to provide electricity to the above-mentioned carbon dioxide reduction energy storage system for electrochemical catalytic reaction;
  • the third step is to export and store the generated methane fuel for subsequent energy use.
  • the pH value of the electrolyte is 6.2-6.8, and the reaction temperature is room temperature.
  • the new energy can be photovoltaic new energy, wind energy and the like.
  • the graphite electrode substrate was put into the above electroplating solution, and electroplating was performed with a deposition current density of -3mA/cm 2 , a total deposition electricity of 2.5C/cm 2 , and a prepared catalyst layer with a thickness of 12 ⁇ M.
  • the molar ratio of polyaniline with camphorsulfonic acid as a dopant: aniline monomer: camphorsulfonic acid is 1:8.
  • Faraday efficiency refers to the percentage of the actual product and the amount of the theoretical product.
  • the amount of the theoretical product is the reduction electrons generated by the catalytic electrode using electric energy.
  • the number of electron transfers in the catalytic reaction is calculated, which is theoretically used to reduce CO 2
  • the content of the product was detected by gas chromatography.
  • the modified copper electrode prepared in the above example is used as the cathode, the inert metal platinum electrode is used as the anode, and the 0.1M sodium bicarbonate solution saturated with CO2 is used as the electrolyte to construct a carbon dioxide reduction energy storage system, and the CO2 gas source is passed into The system electrolyte is saturated to saturation, and the solar power supply system is used for power supply to carry out the electrochemical catalytic reaction.
  • the working voltage applied to the cathode is -0.82V (vs silver/silver chloride electrode).
  • the reaction temperature is room temperature and the pH value is 6.8.
  • the difficulty of protonation in the microenvironment of different polymers can be achieved by electrochemical in situ Raman characterization combined with in situ electrochemical pH probes. Spike potential -0.82V acquisition data calculation.
  • the local pH of different polymer modified electrodes changes in the reaction onset potential (OCP) and the reaction peak current potential value (-0.82V) as follows
  • OCP reaction onset potential
  • -0.82V reaction peak current potential value
  • the initial local pH of the electrode surface is all less than the pH of the electrolyte, but as the catalytic reduction reaction progresses, the The CO* radicals generated on the electrode surface continuously obtain protons from the environment, thereby generating methane, and the local pH will continue to rise, while in Examples 3 and 4, due to the higher local sulfonic acid group density, there is a stronger The proton-providing ability and proton-conducting ability, so the increase of its pH is
  • Example 3 Using the same preparation method as in Example 1, the modified polymer used in Table 3 was used to replace the sodium polybutadiene sulfonate in Example 4, and the rest remained unchanged to prepare different electrolytes.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
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Abstract

L'invention concerne un catalyseur à base de cuivre pour la réduction catalytique électrochimique du dioxyde de carbone et pour un stockage d'énergie sous l'effet d'une nouvelle énergie et d'énergie électrique, qui est préparé par copolymérisation de nanoparticules de cuivre et d'un polymère modifié. Le polymère modifié est un polymère ayant une chaîne latérale conductrice de protons et une chaîne principale conductrice d'électrons. Selon le catalyseur, un groupe modifié entièrement nouveau est utilisé pour modifier le catalyseur à base de cuivre en tant qu'électrode catalytique électrochimique, ce qui améliore le rendement catalytique et le rendement de Faraday d'un catalyseur existant à base de cuivre, réduit la perte d'énergie d'entrée et permet de réaliser un stockage efficace et une neutralisation du carbone de l'énergie électrique.
PCT/CN2021/138135 2021-11-09 2021-12-15 Catalyseur à base de cuivre et électrode pour réduction catalytique électrochimique du dioxyde de carbone et pour stockage de l'énergie, procédé de préparation associé et son application WO2023082409A1 (fr)

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CN202111323665.2A CN113957480B (zh) 2021-11-09 2021-11-09 电化学催化二氧化碳还原储能用铜基催化剂、电极、其制备方法及应用
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KR20240103467A (ko) 2022-12-27 2024-07-04 서울대학교산학협력단 금속 이온 구조체 제조방법, 이에 의하여 제조된 촉매 및 이를 포함하는 전극
KR20240104922A (ko) 2022-12-28 2024-07-05 서울대학교산학협력단 비스무트 구조체 제조방법 및 이를 포함하는 이산화탄소 환원용 전극

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US4959131A (en) * 1988-10-14 1990-09-25 Gas Research Institute Gas phase CO2 reduction to hydrocarbons at solid polymer electrolyte cells
US20060008697A1 (en) * 2004-07-08 2006-01-12 Hae-Kyoung Kim Supported catalyst and fuel cell using the same
US20080193827A1 (en) * 2007-02-12 2008-08-14 Jang Bor Z Conducting polymer-transition metal electro-catalyst compositions for fuel cells
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