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CN-121976221-A - For electrochemical CO2Preparation method and application method of reduced copper-based catalyst

CN121976221ACN 121976221 ACN121976221 ACN 121976221ACN-121976221-A

Abstract

The invention relates to a preparation method and an application method of a copper-based catalyst for electrochemical CO 2 reduction, wherein the preparation method of the copper-based catalyst for electrochemical CO 2 reduction comprises the following steps of S100, obtaining copper powder, dissolving the copper powder in a solvent, carrying out ultrasonic mixing to obtain a copper-based mixed solution, S200, transferring the copper-based mixed solution into an autoclave for heating, charging CO 2 gas to a supercritical state after the temperature is raised to a preset temperature, carrying out constant-temperature reaction for 3-24 hours, cooling to room temperature, centrifuging, taking out bottom solid, washing and drying to obtain the copper-based catalyst for electrochemical CO 2 reduction.

Inventors

  • YANG HUANHUAN
  • CHEN YANG
  • ZHANG SHASHA
  • YAN PENGFEI
  • XU QUN

Assignees

  • 郑州大学

Dates

Publication Date
20260505
Application Date
20260116

Claims (10)

  1. 1. A method for preparing a copper-based catalyst for electrochemical CO 2 reduction, comprising the steps of: S100, obtaining copper powder, dissolving the copper powder in a solvent, and uniformly mixing the copper powder with the solvent by ultrasonic waves to obtain a copper-based mixed solution; And S200, transferring the copper-based mixed solution into an autoclave for heating, after the temperature is raised to a preset temperature, filling CO 2 gas into the autoclave for supercritical state, reacting at constant temperature for 3-24 hours, cooling to room temperature, centrifuging, taking out the bottom solid, washing and drying to obtain the copper-based catalyst for electrochemical CO 2 reduction.
  2. 2. The method for preparing a copper-based catalyst for electrochemical CO 2 reduction according to claim 1, wherein in step S100, the copper powder is nano copper powder.
  3. 3. The method for preparing a copper-based catalyst for electrochemical CO 2 reduction according to claim 1, wherein in step S100, the weight-to-volume ratio of copper powder to solvent is 5mg/10mL to 20mg/10mL.
  4. 4. The method for preparing a copper-based catalyst for electrochemical CO 2 reduction according to claim 1, wherein in step S100, the solvent is a mixed solvent or a single solvent; the single solvent is deionized water or an alcohol solvent; the mixed solvent is a mixed solvent of deionized water and alcohol.
  5. 5. The method for preparing a copper-based catalyst for electrochemical CO 2 reduction according to claim 1, wherein in step S100, the volume ratio of deionized water to alcohol solvent in the mixed solvent is 1:0-1:4.
  6. 6. The method of preparing a copper-based catalyst for electrochemical CO 2 reduction according to claim 5, wherein the crystal plane of the copper-based catalyst is controlled by controlling the volumetric ratio of deionized water to alcohol.
  7. 7. The method for preparing a copper-based catalyst for electrochemical CO 2 reduction according to claim 1, wherein in step S200, the preset temperature is 40-100 ℃.
  8. 8. The method for preparing a copper-based catalyst for electrochemical CO 2 reduction according to claim 1, wherein in step S200, the supercritical state gas pressure of carbon dioxide is 8-20 mpa.
  9. 9. A method of using a copper-based catalyst for electrochemical CO 2 reduction, characterized in that the copper-based catalyst for electrochemical CO 2 reduction is prepared by the preparation method according to any one of claims 1 to 8.
  10. 10. The method of using a copper-based catalyst for electrochemical CO 2 reduction according to claim 8, comprising the steps of: a100, dispersing a copper-based catalyst in an alcohol solution, adding 5wt.% of perfluorosulfonic acid ion exchange resin solution and carbon powder, performing ultrasonic dispersion to obtain uniform slurry, and coating the slurry on the surface of a pretreated carbon paper electrode; A200, adopting a three-electrode test system, taking carbon paper coated with catalyst slurry as a working electrode, ag/AgCl as a reference electrode, and a Pt electrode as a counter electrode, and introducing CO 2 into the electrolyte to obtain a CO 2 saturated electrolyte; A300, adopting an electrochemical workstation, applying voltage, and reducing CO 2 .

Description

Preparation method and application method of copper-based catalyst for electrochemical CO 2 reduction Technical Field The invention relates to the technical field of new energy materials and catalysis, in particular to a preparation method and an application method of a copper-based catalyst for electrochemical CO 2 reduction. Background Copper-based catalysts have been widely used in the catalytic field, including but not limited to methanol synthesis, hydrocarbon reforming, carbon monoxide oxidation, water gas shift reactions, and electrochemical carbon dioxide reduction (CO 2 RR), by virtue of their core advantages of abundant reserves, low cost, excellent catalytic performance, etc. Under the electric drive of renewable energy conversion such as solar energy, wind energy and the like, CO 2 is reduced into high-added-value chemicals by using a copper-based catalyst, and the method is an important way for realizing renewable energy storage and carbon circulation. In a copper-based catalyst system, cuprous oxide is a key phase for optimizing the catalytic performance of CO 2 RR, and the exposed crystal face of the cuprous oxide can obviously influence the catalytic performance by regulating and controlling key factors such as the atomic arrangement, the coordination unsaturated degree, the electronic structure and the like of the surface of the catalyst, namely, the surface atomic arrangement, the coordination condition and the electronic structure of the catalyst of different crystal faces are different, the activation of CO 2 and the adsorption conversion capability of an intermediate are also different, and the catalytic performance is influenced. At present, the regulation and control of the cuprous oxide crystal face mainly depends on methods such as surfactant modification, pH value adjustment, element doping, electrochemical deposition and the like, but the problems of difficult removal of surfactant residues, limited crystal face regulation and control precision, complex synthesis process, higher equipment requirement and the like generally exist in the technologies. Disclosure of Invention In view of the above analysis, embodiments of the present invention aim to provide a method for preparing and applying a copper-based catalyst for electrochemical CO 2 reduction, which is used to solve at least one of the above problems. In one aspect, the invention provides a method for preparing a copper-based catalyst for electrochemical CO 2 reduction, comprising the steps of: S100, obtaining copper powder, dissolving the copper powder in a solvent, and uniformly mixing the copper powder with the solvent by ultrasonic waves to obtain a copper-based mixed solution; And S200, transferring the copper-based mixed solution into an autoclave for heating, after the temperature is raised to a preset temperature, filling CO 2 gas into the autoclave for supercritical state, reacting at constant temperature for 3-24 hours, cooling to room temperature, centrifuging, taking out the bottom solid, washing and drying to obtain the copper-based catalyst for electrochemical CO 2 reduction. Further, in step S100, the copper powder is nano copper powder. Further, in step S100, the weight-volume ratio of the copper powder to the solvent is 5mg/10 mL-20 mg/10mL. Further, in step S100, the solvent is a mixed solvent or a single solvent; the single solvent is deionized water or an alcohol solvent; the mixed solvent is a mixed solvent of deionized water and alcohol. Further, in step S100, the volume ratio of deionized water to alcohol solvent in the mixed solvent is 1:0-1:4. Further, the crystal face of the copper-based catalyst is controlled by controlling the volumetric ratio of the deionized water to the alcohol. Further, in step S200, the preset temperature is 40 to 100 ℃. Further, in step S200, the air pressure in the supercritical state of the carbon dioxide is 8 to 20mpa. In another aspect, the invention provides a method of using a copper-based catalyst for electrochemical CO 2 reduction, the copper-based catalyst for electrochemical CO 2 reduction being prepared using the preparation method described above. Further, the application method comprises the following steps: a100, dispersing a copper-based catalyst in an alcohol solution, adding 5wt.% of perfluorosulfonic acid ion exchange resin solution and carbon powder, performing ultrasonic dispersion to obtain uniform slurry, and coating the slurry on the surface of a pretreated carbon paper electrode; A200, adopting a three-electrode test system, taking carbon paper coated with catalyst slurry as a working electrode, ag/AgCl as a reference electrode, and a Pt electrode as a counter electrode, and introducing CO 2 into the electrolyte to obtain a CO 2 saturated electrolyte; A300, adopting an electrochemical workstation, applying voltage, and reducing CO 2. Compared with the prior art, the invention has the following at least realized beneficial effects: (1) The supercritical