CN116103700A - Copper electrocatalyst and preparation method thereof - Google Patents

Copper electrocatalyst and preparation method thereof Download PDF

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Publication number
CN116103700A
CN116103700A CN202211398153.7A CN202211398153A CN116103700A CN 116103700 A CN116103700 A CN 116103700A CN 202211398153 A CN202211398153 A CN 202211398153A CN 116103700 A CN116103700 A CN 116103700A
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copper
electrocatalyst
substrate
electrolytic cell
type electrolytic
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Inventor
任博华
文国斌
陈逸明
钟坤伟
张晓文
王新
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South China Normal University
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South China Normal University
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
    • 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
    • C25B11/065—Carbon
    • 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
    • C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
    • 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

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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)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a copper electrocatalyst and a preparation method thereof, and relates to the technical field of preparation of electrocatalyst reducing agents, wherein the method comprises the following steps: providing an H-type electrolytic cell, wherein the H-type electrolytic cell contains 0.01-0.03 mol/L copper tartrate solution; electrodepositing and preparing a copper electrocatalyst on a substrate by utilizing the H-type electrolytic cell; the substrate is selected from carbon cloth, foam copper or foam nickel. The prepared copper electrocatalyst (Cu-CuF) has better conductivity and higher selectivity to carbon-containing products, and the total current density under-0.83V vs RHE can reach-85 mA/cm at the highest 2 FE of Cu-CuF catalyst Ctol The effect on the applied potential was volcanic, with the highest overall carbon conversion Faraday efficiency of about 83%, showing Cu-CuF versus CO 2 RR has good catalytic activity.

Description

Copper electrocatalyst and preparation method thereof
Technical Field
The invention relates to the technical field of electrocatalytic reducing agent preparation, in particular to a copper electrocatalyst and a preparation method thereof.
Background
Due to CO 2 Urgent need for recovery and carbon neutralization, electrocatalytic CO 2 Reduction reaction (CO) 2 RR) is of great importance for the synthesis of valuable chemicals and fuels under mild conditions. However CO 2 Is a stable linear molecule, CO 2 The selectivity and yield of a range of products produced by RR are limited.
Existing methods for electrocatalytic CO 2 The electrocatalyst selectivity of the reduction reaction is low in faraday efficiency.
Accordingly, there is still a need in the art for further improvements and enhancements.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a copper electrocatalyst and a preparation method thereof, which aims to solve the problem of low faraday efficiency of the existing electrocatalyst applied to carbon dioxide catalytic reduction reaction.
The preparation method of the copper electrocatalyst comprises the following steps:
providing an H-type electrolytic cell, wherein the H-type electrolytic cell contains 0.01-0.03 mol/L of copper tartrate solution and 0.1-0.6mol/L of potassium bicarbonate solution;
electrodepositing and preparing a copper electrocatalyst on a substrate by utilizing the H-type electrolytic cell; the substrate is selected from carbon cloth, foam copper or foam nickel.
Optionally, the preparation method of the copper electrocatalyst, wherein the catholyte of the H-type electrolytic cell comprises: 0.01mol/L to 0.03mol/L of copper tartrate solution and 0.1mol/L to 0.5mol/L of potassium bicarbonate solution; the anolyte comprises 0.3mol/L-0.6mol/L potassium bicarbonate solution.
Optionally, the preparation method of the copper electrocatalyst, wherein the step of preparing the copper electrocatalyst by electrodeposition of the H-type electrolytic cell on a substrate specifically comprises the following steps:
and (3) continuously electrolyzing the substrate for 5-20 minutes under a preset current density by adopting a constant current electrolysis method to obtain the copper electrocatalyst.
Optionally, the pH of the catholyte is 4-7, and the pH range is effective to prevent hydrolysis of copper ions in solution to a certain extent.
Optionally, the preparation method of the copper electrocatalyst, wherein the predetermined current density is from-5 to-20 mA/cm 2 。
The copper electrocatalyst is prepared by the preparation method.
Optionally, the copper electrocatalyst comprises a substrate and nano copper particles deposited on the surface of the substrate, wherein the particle size of the copper nano particles is 100 to 200nm.
The use of the copper electrocatalyst described above, wherein the copper electrocatalyst is used in an electrocatalytic carbon dioxide reduction reaction.
Optionally, the use of said copper electrocatalyst, wherein said copper electrocatalyst has a total carbon product faraday efficiency greater than 80% at a-0.83 vs RHE potential.
The beneficial effects are that: compared with the prior art, the preparation method of the copper electrocatalyst provided by the invention has the advantages that the synthesis method is simple, the operability is strong, the prepared copper electrocatalyst can obviously change the distribution of the catalyst and the flow field of the water electrolyte, and the CO is regulated 2 Adsorption energy, thereby promoting reaction rate and improving selectivity of activated polarized region multi-carbon product (FE is expressed by Faraday efficiency C2+ )。
Drawings
FIG. 1 is a scanning electron microscope image of a carbon cloth as a substrate;
FIG. 2 is a scanning electron microscope image of copper foam as a substrate;
FIG. 3 is a scanning electron microscope image of nickel foam as a substrate;
FIG. 4 is a graph showing CO of a copper catalyst on different substrates using carbon cloth as a substrate 2 RR performance;
FIG. 5 is a graph of CO of copper catalyst on different substrates with copper foam as the substrate 2 RR performance;
FIG. 6 is a graph of CO of copper catalyst on different substrates with nickel foam as substrate 2 RR performance;
FIG. 7 is a graph showing current densities of total carbon conversion for different substrates at different potentials;
figure 8 shows faraday efficiencies for total carbon conversion for different substrates at different potentials.
Detailed Description
The invention provides a copper electrocatalyst and a preparation method thereof, which are used for making the purposes, technical schemes and effects of the invention clearer and more definite, and are further described in detail below. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
In order to solve the problems of low Faraday efficiency and low selectivity of the existing electrocatalyst applied to carbon dioxide catalytic reduction reaction. The embodiment provides a preparation method of a copper electrocatalyst, which comprises the following steps:
s10, providing an H-type electrolytic cell, wherein the H-type electrolytic cell contains 0.01-0.03 mol/L of copper tartrate solution and 0.1-0.6mol/L of potassium bicarbonate solution;
s20, electrodepositing and preparing a copper electrocatalyst on a substrate by utilizing the H-type electrolytic cell; the substrate is selected from carbon cloth, foam copper or foam nickel.
In this example, the H-cell is a typical cell in the art, consisting of a cathode, an anode, a cation exchange membrane (CEM, nafion 211), a catholyte and an anolyte for controlled synthesis. Wherein, the substrate of the cathode material can be carbon Cloth (CF), copper foam (CuF) or nickel foam (NiF); the catholyte comprises 0.01mol/L to 0.03mol/L of copper tartrate solution, 0.1mol/L to 0.5mol/L of potassium bicarbonate solution and hydrochloric acid for adjusting the pH value of the catholyte, and the pH value of the catholyte is in the range of 4 to 7 by adding the hydrochloric acid, so that the hydrolysis of copper ions can be prevented to a certain extent; the anolyte comprises 0.3mol/L-0.6mol/L potassium bicarbonate solution. The deposition rate on the cathode and the anode can be controlled by controlling the concentration of the catholyte and the anolyte, so that the deposition is more uniform, the obtained copper particles are in close contact with the substrate, and the conductivity of the copper electrocatalyst is enhanced.
In this embodiment, a Constant Current (CCE) method is adopted, and at a certain current density, such as-5 to-20 mA/cm 2 And continuously electrolyzing the substrate to form copper nano particle deposition on the surface of the substrate, thereby obtaining the copper electrocatalyst.
Exemplary, a Constant Current (CCE) method is employed at 10mA/cm 2 Continuously electrolyzing the copper foam for 10 minutes under the condition of (2) to obtain the copper foam base copper electrocatalyst.
In this example, copper-based catalysts (Cu-CuF) based on copper foam, which have a macroporous structure (about 200 μm), are advantageous for mass transport and electron transfer. The obtained electrocatalytic reduction performance test is carried out at ambient pressure and room temperature, has higher total current density under smaller potential, and the Faraday efficiency of the total carbon product can exceed 80%, thereby achieving the purpose of reducing the operation cost.
Based on the same inventive concept, the invention provides a copper electrocatalyst, which is prepared by adopting carbon cloth, foam copper or foam nickel as a substrate and adopting a constant current electrolysis method to deposit copper on the surface of the carbon cloth, foam copper or foam nickel. The specific preparation method is as described above, and is not described herein. It is readily understood that the copper electrocatalyst provided by the invention may be used in a reduction reaction to carbon dioxide.
The preparation method of the copper electrocatalyst provided by the invention is further explained below through specific preparation examples.
Example 1
An H-type cell is provided, consisting of a cathode, a platinum sheet anode, a cation exchange membrane (CEM, nafion 211). The cathode substrate is carbon Cloth (CF). The catholyte consisted of 10mL of 0.01M copper (II) tartrate and 30mL of 0.5M KHCO 3 Composition and pH was adjusted with hydrochloric acid (HCl, 37%) to avoid hydrolysis. The anolyte is prepared from 0.5M KHCO 3 Composition is prepared. Continuous CO feed to catholyte 2 To saturate the solution.
By Constant Current Electrolysis (CCE), at-15 mA/cm 2 Continuously electrolyzing the carbon Cloth (CF) for 20 minutes to obtain the copper electrocatalyst taking the carbon cloth as a substrate. As can be seen from the scanning electron microscope of FIG. 1, copper nano particles are accumulated on the surface of the carbon fiber, and the in-situ growth of the copper particles on the surface of the high-conductivity carbon fiber ensures that the electrocatalyst Cu and the carbon fiber realize close contact on the nano scale, the conductivity is enhanced, and the high-performance electrochemical catalysis is realized.
Example 2
To investigate the effect of different substrate materials on the catalytic performance of electrocatalysts, an H-type cell was provided, consisting of a cathode, a platinum anode, and a cation exchange membrane (CEM, nafion 211). The cathode substrate is copper foam (CuF). The catholyte consisted of 10mL of 0.01M copper (II) tartrate and 30mL of 0.5M KHCO 3 Composition and pH was adjusted with hydrochloric acid (HCl, 37%) to avoid hydrolysis. The anolyte is prepared from 0.5M KHCO 3 Composition is prepared. Continuous CO feed to catholyte 2 To saturate the solution.
By Constant Current Electrolysis (CCE), at-15 mA/cm 2 The electrolysis of copper foam (CuF) was continued for 20 minutes under the conditions of the above to obtain a copper electrocatalyst based on copper foam. From the scanning electron microscope image of fig. 2, it can be seen that needle-like copper dendrites densely grow on top of the copper foam.
Example 3
To investigate the effect of different substrate materials on the catalytic performance of electrocatalysts, an H-type cell was provided, consisting of a cathode, a platinum anode, and a cation exchange membrane (CEM, nafion 211). The cathode substrate was nickel foam (NiF). The catholyte consisted of 10mL of 0.01M copper (II) tartrate and 30mL of 0.5M KHCO 3 Composition and pH was adjusted with hydrochloric acid (HCl, 37%) to avoid hydrolysis. The anolyte is prepared from 0.5M KHCO 3 Composition is prepared. Continuous CO feed to catholyte 2 To saturate the solution.
By Constant Current Electrolysis (CCE), at-15 mA/cm 2 Continuously electrolyzing the foam Nickel (NiF) for 20 minutes under the condition of taking the foam nickel as a substrateCopper electrocatalyst of (a). As can be seen from the scanning electron microscope image of FIG. 3, copper is uniformly distributed on the foam nickel, and a large number of nanocubes are formed.
Example 4
To investigate the effect of different solution concentrations on the catalytic performance of the electrocatalyst, an H-type cell was provided, consisting of a cathode, a platinum anode, and a cation exchange membrane (CEM, nafion 211). The cathode substrate is carbon Cloth (CF). The catholyte consisted of 10mL of 0.03M copper (II) tartrate and 30mL of 0.1M KHCO 3 Composition and pH was adjusted with hydrochloric acid (HCl, 37%) to avoid hydrolysis. The anolyte is prepared from 0.5M KHCO 3 Composition is prepared. Continuous CO feed to catholyte 2 To saturate the solution.
By Constant Current Electrolysis (CCE), at-15 mA/cm 2 Continuously electrolyzing the carbon Cloth (CF) for 20 minutes to obtain the copper electrocatalyst taking the carbon cloth as a substrate.
Example 5
To investigate the effect of different current densities on the catalytic performance of electrocatalysts, an H-type cell was provided, consisting of a cathode, a platinum anode, and a cation exchange membrane (CEM, nafion 211). The cathode substrate is carbon Cloth (CF). The catholyte consisted of 10mL of 0.1M copper (II) tartrate and 30mL of 0.5M KHCO 3 Composition and pH was adjusted with hydrochloric acid (HCl, 37%) to avoid hydrolysis. The anolyte is prepared from 0.5M KHCO 3 Composition is prepared. Continuous CO feed to catholyte 2 To saturate the solution.
By Constant Current Electrolysis (CCE), at-5 mA/cm 2 The electrolysis of copper foam (CuF) was continued for 20 minutes under the conditions of the above to obtain a copper electrocatalyst based on copper foam.
CO of the copper electrocatalyst prepared in the above example on different substrates 2 RR performance was tested and the test results are shown in fig. 4 to 6. Wherein, the gas generated in the performance test and the content thereof are all detected by gas chromatography (jin island GC 2014C). The specific detection method comprises the following steps: CO is added before electrolysis 2 The gas is introduced into the cathode chamber of the H-type electrolytic cell through a hose, and then the H-type electrolytic cell is connected with a gas chromatograph through the hose. CO is introduced into the catholyte before the experiment 2 Make it CO 2 The content is saturated, the electrolysis duration is set to be 40 minutes, and when the electrolysis duration is respectively 15 minutes and 30 minutes, the gas in the cathode chamber of the H-type electrolytic cell is introduced into a gas chromatograph for detection, so that the detection purpose is realized. As a result of examination, most of the products were ethylene (C 2 H 4 ) And hydrogen (H) 2 ) The maximum Faraday efficiency of ethylene at-0.83V vs RHE was 44%. The faraday efficiency of hydrogen remains below 20% in the range of-1.03V vs RHE to-0.63V vs RHE due to significant suppression of Hydrogen Evolution Reactions (HER). And Cu-CF showed higher ethylene selectivity, the faraday efficiency of ethylene at-0.83V vs RHE increased significantly to 48%.
As shown in FIGS. 7 to 8, the current density and Faraday efficiency of the total carbon conversion of different substrates at different potentials can be shown by FIGS. 7 and 8, because the Cu-CuF catalyst has better conductivity and higher selectivity to carbon-containing products, the total current density at-0.83V vs RHE can reach-85 mA/cm at most 2 The Cu-CF total current density at the same voltage is-74 mA/cm 2 . Through FIG. 8, FE of Cu-CuF and Cu-CF catalysts Ctol The effect on the applied potential was volcanic, with the highest overall carbon conversion Faraday efficiency of about 83%, showing that Cu-CF and Cu-CuF vs. CO 2 RR has good catalytic activity.
In summary, the present invention provides a copper electrocatalyst and a preparation method thereof, the method comprising: providing an H-type electrolytic cell, wherein the H-type electrolytic cell contains 0.01-0.03 mol/L of copper tartrate solution and 0.1-0.6mol/L of potassium bicarbonate solution; electrodepositing and preparing a copper electrocatalyst on a substrate by utilizing the H-type electrolytic cell; the substrate is selected from carbon cloth, foam copper or foam nickel. The prepared copper electrocatalyst (Cu-CuF) has better conductivity and higher selectivity to carbon-containing products, and the total current density under-0.83V vs RHE can reach-85 mA/cm at the highest 2 FE of Cu-CuF catalyst Ctol The effect on the applied potential was volcanic, with the highest overall carbon conversion Faraday efficiency of about 83%, showing Cu-CuF versus CO 2 RR has good catalytic activity.
It is to be understood that the invention is not limited in its application to the examples described above, but is capable of modification and variation in light of the above teachings by those skilled in the art, and that all such modifications and variations are intended to be included within the scope of the appended claims.

Claims (9)

1. The preparation method of the copper electrocatalyst is characterized by comprising the following steps of:
providing an H-type electrolytic cell, wherein the H-type electrolytic cell contains 0.01-0.03 mol/L copper tartrate solution;
electrodepositing and preparing a copper electrocatalyst on a substrate by utilizing the H-type electrolytic cell; the substrate is selected from carbon cloth, foam copper or foam nickel.
2. The method for preparing a copper electrocatalyst according to claim 1, wherein the catholyte of the H-type electrolytic cell comprises: 0.01mol/L to 0.03mol/L of copper tartrate solution and 0.1mol/L to 0.5mol/L of potassium bicarbonate solution; the anolyte comprises 0.3mol/L-0.6mol/L potassium bicarbonate solution.
3. The method for preparing the copper electrocatalyst according to claim 1, wherein the step of preparing the copper electrocatalyst by electrodeposition of the H-type electrolytic cell on a substrate specifically comprises:
and (3) continuously electrolyzing the substrate for 5-20 minutes under a preset current density by adopting a constant current electrolysis method to obtain the copper electrocatalyst.
4. The method for preparing a copper electrocatalyst according to claim 2, wherein the pH of the catholyte is from 4 to 7.
5. The method for producing a copper electrocatalyst according to claim 3, wherein the predetermined current density is from-5 to-20 mA/cm 2 。
6. A copper electrocatalyst, wherein the copper electrocatalyst is prepared by the method according to any one of claims 1 to 5.
7. The copper electrocatalyst according to claim 6, comprising a substrate and copper nanoparticles deposited on the surface of the substrate, the nanoparticles having a particle size of from 100 to 200nm.
8. Use of a copper electrocatalyst according to claim 6, wherein the copper electrocatalyst is used in an electrocatalytic carbon dioxide reduction reaction.
9. The use of a copper electrocatalyst according to claim 8, wherein the copper electrocatalyst has a total carbon product faradaic efficiency greater than 80% at a-0.83 vs RHE potential.
CN202211398153.7A 2022-11-09 2022-11-09 Copper electrocatalyst and preparation method thereof Pending CN116103700A (en)

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