CN113529132A - Cobalt-based catalyst electrode and preparation method thereof - Google Patents
Cobalt-based catalyst electrode and preparation method thereof Download PDFInfo
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- CN113529132A CN113529132A CN202110906452.6A CN202110906452A CN113529132A CN 113529132 A CN113529132 A CN 113529132A CN 202110906452 A CN202110906452 A CN 202110906452A CN 113529132 A CN113529132 A CN 113529132A
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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
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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
- C25B1/24—Halogens or compounds thereof
- C25B1/26—Chlorine; Compounds thereof
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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
- C25B11/054—Electrodes comprising electrocatalysts supported on a carrier
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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
- C25B11/055—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
- C25B11/063—Valve metal, e.g. titanium
Abstract
The invention relates to the technical field of marine antifouling, in particular to a cobalt-based catalyst electrode and a preparation method thereof. A cobalt-based catalyst electrode comprising a substrate on which a cobalt-based composite catalyst is deposited. The cobalt-based composite catalyst consists of Co and Co (OH)2And (4) forming. The main components of the cobalt-based catalyst electrode prepared by the invention are Co and Co (OH)2The composite catalyst has larger specific surface area, can provide more active sites and is more beneficial to the implementation of electrocatalytic reaction; the composite material has excellent electro-catalysis chlorine evolution activity, high chlorine evolution selectivity and stability in seawater, and is beneficial to the antifouling application of relevant equipment in marine environment.
Description
Technical Field
The invention relates to the technical field of marine antifouling, in particular to a cobalt-based catalyst electrode and a preparation method thereof.
Background
With the observation of people on marine ecology and the development of marine resources, the development and utilization of various marine instruments and equipment are greatly promoted, so that the change of relevant characteristic parameters in the marine environment can be continuously monitored. However, when these equipments are exposed to seawater, biofouling inevitably occurs, which not only requires frequent cleaning and maintenance of the equipments, but also affects the collection of the relevant data. Therefore, finding an efficient, simple and controllable technique to solve the problem of biofouling of marine instruments is crucial to marine observation and utilization.
At present, the protection methods for marine instruments mainly comprise mechanical wiping, release of copper or tributyltin biocides, ultraviolet irradiation, chlorine preparation from seawater electrolysis, antifouling and the like. Among them, the technology of electrolyzing seawater to produce chlorine is concerned by people because of its advantages of simple operation, stability and high efficiency. On one hand, the method can control the generation amount of the effective chlorine, so that the method can prevent the biofouling of marine instruments and cannot cause damage to marine environment. On the other hand, seawater is rich in chloride ions, and the effective substances participating in the reaction are inexhaustible, so that the method also has excellent sustainability.
The most important technology for preparing chlorine and preventing pollution by electrolyzing seawater is the preparation and selection of electrodes. The chlorine industry commonly uses a Dimension Stability Anode (DSA) composed of Ru and Ir-based Mixed Metal Oxide (MMO) as a high-efficiency catalyst, and although the electrode has excellent catalytic chlorine evolution effect in the chlor-alkali industry, the marine antifouling property and the electrolysis condition of a chlorine production system are greatly different. The seawater electrolytic chlorine production antifouling is carried out under the conditions of typical neutral pH value and relatively low chloride ion concentration, and under the conditions, the DSA not only carries out chlorine evolution reaction, but also accompanies a large amount of oxygen evolution reaction. In addition, the electrode is made of precious metal materials and is expensive, which further limits the wide application of the electrode to seawater electrolysis. Therefore, the electrolytic seawater anti-fouling technology still needs to develop a chlorine evolution electrode with high activity, high selectivity and low cost.
Disclosure of Invention
In order to make up for the defects in the existing electrolytic seawater antifouling technology, the invention provides the cobalt-based catalyst electrode and the preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows: a cobalt-based catalyst electrode comprising a substrate on which a cobalt-based composite catalyst is deposited.
In a preferred embodiment of the present invention, the cobalt-based composite catalyst comprises Co and Co (OH)2And (4) forming.
Further preferably, the substrate is metallic titanium.
The invention further provides a preparation method of the cobalt-based catalyst electrode, which is to prepare a cobalt-based composite catalyst on the surface of a substrate by adopting a constant potential electrodeposition method; CoSO with electrodeposition liquid of 0.005-0.1 mol/L4Solution, electrodeposition parameter setting: the voltage is-0.9V to-1.8V vs. SCE, and the time is 400 to 1800 s.
The invention also provides application of the cobalt-based catalyst electrode, which is used as a catalyst anode for preparing chlorine by electrolyzing seawater and is used for preventing fouling of an underwater optical window.
The cobalt-based catalyst electrode and the preparation method thereof have the following beneficial effects:
(1) the electrochemical technology used by the process is simple to operate, and the catalyst electrode can be obtained without complicated processes;
(2) the main components of the cobalt-based catalyst electrode prepared by the invention are Co and Co (OH)2The composite catalyst has larger specific surface area, can provide more active sites and is more beneficial to the implementation of electrocatalytic reaction;
(3) the cobalt-based catalyst electrode prepared by the method has a low cost effect, and the prepared material is transition metal with rich reserves, so that the method is beneficial to practical popularization and application;
(4) the cobalt-based catalyst electrode prepared by the invention has excellent electro-catalysis chlorine evolution activity, high chlorine evolution selectivity and stability in seawater, and is beneficial to the antifouling application of relevant equipment in marine environment.
Drawings
FIG. 1 is an SEM image of a cobalt-based catalyst electrode provided in example 1 of the present invention;
FIG. 2 is an XRD pattern of a cobalt-based catalyst electrode provided in example 1 of the present invention;
FIG. 3 shows a cobalt-based catalyst electrode and Co provided in example 1 of the present invention3O4The electrodes were immersed in 0.6M NaCl solution (equivalent to Cl in seawater)-Concentration) and a linear scan in saturated sodium chloride solution;
FIG. 4 shows a cobalt-based catalyst electrode and a commercial DSA of example 1 in 0.6M NaCl and 0.4M Na2SO4Linear scan of (1);
FIG. 5 is a graph showing the stability of a cobalt-based catalyst electrode provided in example 1 of the present invention in a 0.6M NaCl solution.
Detailed Description
In order to facilitate an understanding of the invention, the invention is described in more detail below with reference to the accompanying drawings and specific examples. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Example 1: a cobalt-base catalyst electrode for preparing chlorine by electrolyzing seawater features that a Ti net is used as substrate on which the composite catalyst Co and Co (OH) is deposited2。
The cobalt-based catalyst electrode of this example was prepared by the following method:
(1) pretreatment of a titanium mesh: selecting titanium mesh as matrix, cutting into sample (1 cm × 3 cm) with fixed size, sequentially ultrasonic cleaning with acetone, ethanol and distilled water for 20min, drying at room temperature, packaging with Teflon adhesive tape to fix working area of 1cm2;
(2) Preparing a cobalt-based catalyst electrode: the preparation of the cobalt-based catalyst electrode is carried out at room temperature by adopting a constant voltage electrodeposition technology, a three-electrode system is used in an electrodeposition experiment, the treated titanium mesh is taken as a working electrode, a Saturated Calomel Electrode (SCE) and a platinum (Pt) mesh are respectively taken as a reference electrode and a counter electrode, and then the electrode is placed in 0.01M CoSO4Solutions ofAnd applying a voltage of-1.5V vs. SCE between the electrodes for 1200s, taking out the electrode after the voltage is finished, washing the electrode by using distilled water, and drying the electrode at room temperature to obtain the cobalt-based catalyst electrode.
The cobalt-based catalyst electrode for preparing chlorine by electrolyzing seawater, prepared in the above example 1, was subjected to morphology and composition characterization by SEM and XRD. From the SEM image of a cobalt-based catalyst electrode in FIG. 1, it can be seen that the cobalt-based catalyst electrode prepared in example 1 has a flower-like nanosheet structure, and the flaky structures are connected with each other, so that the structure has a larger specific surface area, can provide more reactive active sites, and is more beneficial to the electrocatalytic chlorine evolution reaction.
FIG. 2 is an XRD pattern of a cobalt-based catalyst electrode, which, by comparison with a standard XRD card, demonstrates Co-Co (OH)2Successful preparation of the catalyst.
FIG. 3 shows the results of chlorine evolution activity test of a cobalt-based catalyst electrode, and it can be seen from FIG. 3 that the electrode is compatible with Co of comparative example3O4The electrode (prepared by the method of the patent publication reference referred to 202110050042.6) exhibited more excellent electrocatalytic chlorine evolution activity in both 0.6M NaCl solution and saturated NaCl solution.
FIG. 4 is a graph showing the results of chlorine evolution performance tests of a cobalt-based catalyst electrode with DSA, showing that the current increase of the cobalt-based catalyst electrode in NaCl solution starts at 1.05V vs. SCE, but in Na containing no chloride2SO4The potential required for the oxidation current to occur in the solution was 1.23V vs. SCE. Meanwhile, for DSA, the current change trends in the two solutions are almost the same, which indicates that DSA has poor chlorine evolution selectivity in 0.6M NaCl solution. It can be seen that for marine environments (Cl)-The concentration is 0.6M), the cobalt-based catalyst electrode prepared by the method has high chlorine evolution selectivity.
FIG. 5 is a graph showing the chlorine evolution stability test results for a cobalt-based catalyst electrode, which shows that the electrode performance is stable and substantially free of decay after 10 hours of testing using chronopotentiometric techniques.
Example 2: a cobalt-base catalyst electrode for preparing chlorine by electrolyzing seawater features that a Ti net is used as basic body and the composite catalyst Co is deposited on said basic bodyAnd Co (OH)2。
The cobalt-based catalyst electrode of this example was prepared by the following method:
(1) pretreatment of a titanium mesh: selecting titanium mesh as matrix, cutting into sample (1 cm × 3 cm) with fixed size, sequentially ultrasonic cleaning with acetone, ethanol and distilled water for 20min, drying at room temperature, packaging with Teflon adhesive tape to fix working area of 1cm2;
(2) Preparing a cobalt-based catalyst electrode: the preparation of the cobalt-based catalyst electrode is carried out at room temperature by adopting a constant voltage electrodeposition technology, a three-electrode system is used in an electrodeposition experiment, the treated titanium mesh is taken as a working electrode, a Saturated Calomel Electrode (SCE) and a platinum (Pt) mesh are respectively taken as a reference electrode and a counter electrode, and then the electrode is placed in 0.05M CoSO4And in the solution, applying a voltage of-1.3V vs. SCE between the electrodes for 800s, taking out the electrode after the voltage is finished, washing the electrode with distilled water, and drying the electrode at room temperature to obtain the cobalt-based catalyst electrode.
Example 3: a cobalt-base catalyst electrode for preparing chlorine by electrolyzing seawater features that a Ti net is used as substrate on which the composite catalyst Co and Co (OH) is deposited2。
The cobalt-based catalyst electrode of this example was prepared by the following method:
(1) pretreatment of a titanium mesh: selecting titanium mesh as matrix, cutting into sample (1 cm × 3 cm) with fixed size, sequentially ultrasonic cleaning with acetone, ethanol and distilled water for 20min, drying at room temperature, packaging with Teflon adhesive tape to fix working area of 1cm2;
(2) Preparing a cobalt-based catalyst electrode: the preparation of the cobalt-based catalyst electrode is carried out at room temperature by adopting a constant voltage electrodeposition technology, a three-electrode system is used in an electrodeposition experiment, the treated titanium mesh is taken as a working electrode, a Saturated Calomel Electrode (SCE) and a platinum (Pt) mesh are respectively taken as a reference electrode and a counter electrode, and then the electrode is placed in 0.1M CoSO4And in the solution, applying a voltage of-1.0V vs. SCE between the electrodes for 400s, taking out the electrode after the voltage is finished, washing the electrode by using distilled water, and drying the electrode at room temperature to obtain the cobalt-based catalyst electrode.
Claims (5)
1. A cobalt-based catalyst electrode comprising a substrate, characterized in that: and depositing a cobalt-based composite catalyst on the substrate.
2. A cobalt-based catalyst electrode according to claim 1, characterized in that: the cobalt-based composite catalyst consists of Co and Co (OH)2And (4) forming.
3. A cobalt-based catalyst electrode according to claim 1 or 2, characterized in that: the substrate is metal titanium.
4. A method for preparing a cobalt-based catalyst electrode according to claim 1 or 2, wherein: preparing a cobalt-based composite catalyst on the surface of a substrate by adopting a constant potential electrodeposition method; CoSO with electrodeposition liquid of 0.005-0.1 mol/L4Solution, electrodeposition parameter setting: the voltage is-0.9V to-1.8V vs. SCE, and the time is 400 to 1800 s.
5. Use of a cobalt-based catalyst electrode, characterized in that: it is used as catalyst anode to electrolyze sea water to prepare chlorine, and is used for preventing fouling of underwater optical window.
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CN114717590A (en) * | 2022-03-10 | 2022-07-08 | 中国科学院海洋研究所 | Preparation method of cobalt-based chlorine evolution catalyst electrode |
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