CN110656348B - Electrocatalytic oxygen evolution electrode and preparation and application thereof - Google Patents
Electrocatalytic oxygen evolution electrode and preparation and application thereof Download PDFInfo
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 239000001301 oxygen Substances 0.000 title claims abstract description 85
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 85
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 91
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 44
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 43
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000011651 chromium Substances 0.000 claims abstract description 41
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 35
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 25
- 229910052742 iron Inorganic materials 0.000 claims abstract description 21
- 239000012266 salt solution Substances 0.000 claims abstract description 11
- 238000009423 ventilation Methods 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 30
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 13
- 150000003839 salts Chemical class 0.000 claims description 11
- 239000003792 electrolyte Substances 0.000 claims description 9
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 9
- 235000011152 sodium sulphate Nutrition 0.000 claims description 9
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229910021555 Chromium Chloride Inorganic materials 0.000 claims description 4
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 claims description 4
- GRWVQDDAKZFPFI-UHFFFAOYSA-H chromium(III) sulfate Chemical compound [Cr+3].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRWVQDDAKZFPFI-UHFFFAOYSA-H 0.000 claims description 4
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 abstract description 38
- 229960001545 hydrotalcite Drugs 0.000 abstract description 38
- 229910001701 hydrotalcite Inorganic materials 0.000 abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 26
- 230000000694 effects Effects 0.000 abstract description 22
- UPHIPHFJVNKLMR-UHFFFAOYSA-N chromium iron Chemical compound [Cr].[Fe] UPHIPHFJVNKLMR-UHFFFAOYSA-N 0.000 abstract description 19
- 239000006260 foam Substances 0.000 abstract description 12
- 238000011161 development Methods 0.000 abstract description 7
- 238000005868 electrolysis reaction Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000010970 precious metal Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 18
- 239000000463 material Substances 0.000 description 15
- 239000003054 catalyst Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 239000002351 wastewater Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 230000003197 catalytic effect Effects 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 8
- 239000010842 industrial wastewater Substances 0.000 description 7
- 239000000758 substrate Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 150000001450 anions Chemical class 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 229910001430 chromium ion Inorganic materials 0.000 description 6
- 229910000604 Ferrochrome Inorganic materials 0.000 description 5
- 230000009471 action Effects 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 238000000975 co-precipitation Methods 0.000 description 4
- 238000005336 cracking Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 230000005684 electric field Effects 0.000 description 4
- 239000010411 electrocatalyst Substances 0.000 description 4
- -1 iron ions Chemical class 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 3
- 229940010514 ammonium ferrous sulfate Drugs 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 239000007800 oxidant agent Substances 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000004528 spin coating Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- 238000004627 transmission electron microscopy Methods 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 2
- 238000004523 catalytic cracking Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000004299 exfoliation Methods 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000013507 mapping Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical class [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001844 chromium Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000004832 voltammetry Methods 0.000 description 1
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- 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
- C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
- C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
- C25B11/031—Porous electrodes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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Abstract
本发明属于环境水处理及电催化技术领域，提供了一种电催化析氧电极及其制备和应用。以三价铬基盐溶液为电解质溶液，以泡沫镍为阴极，以铁为阳极组成标准电极体系；将直流电的正极与阳极连接，负极与阴极连接，在电解质溶液中通入N2一段时间后，停止通气，然后以恒电位或恒电流进行电解反应，至电解质溶液变为无色后，取出阴极，清洗干燥，得到电催化析氧电极。该电催化析氧电极的以泡沫镍为基底，以负载生长在泡沫镍上的铁铬水滑石为活性组分，铁铬水滑石为三维片状结构，拥有极大的电化学活性面积。该电催化析氧电极碱性介质中作为阳极电解水产生氧气，表现出优异的析氧活性，能够代替贵金属促进碱性介质中电解水体系的发展。
The invention belongs to the technical field of environmental water treatment and electrocatalysis, and provides an electrocatalytic oxygen evolution electrode and its preparation and application. A standard electrode system is composed of trivalent chromium base salt solution as electrolyte solution, nickel foam as cathode and iron as anode; the positive electrode of direct current is connected to the anode, the negative electrode is connected to the cathode, and N2 is introduced into the electrolyte solution for a period of time. , stop ventilation, and then carry out electrolysis reaction with constant potential or constant current until the electrolyte solution becomes colorless, take out the cathode, clean and dry to obtain an electrocatalytic oxygen evolution electrode. The electrocatalytic oxygen evolution electrode is based on foamed nickel, and the iron-chromium hydrotalcite supported and grown on the foamed nickel is used as an active component. The electrocatalytic oxygen evolution electrode acts as an anode to electrolyze water to generate oxygen in an alkaline medium, shows excellent oxygen evolution activity, and can replace precious metals to promote the development of an electrolyzed water system in an alkaline medium.
Description
Technical Field
The invention belongs to the technical field of environmental water treatment and electrocatalysis, and particularly relates to an electrocatalysis oxygen evolution electrode and preparation and application thereof.
Background
Hydrotalcite is a double-layer sheet metal hydroxide, and the most common methods for synthesizing hydrotalcite at present mainly comprise two methods: one is an oxidation method and one is a coprecipitation method. The two processes are briefly described below by way of example with Fe/Al-LDH (Fe/Al-double hydroxide).
The oxidation process is carried out in a neutral or alkaline environment with anions (SO)4 2-、CO3 2-、Cl-Etc.) in the presence of an oxidizing agent (O)2、H2O2、K2MnO7Etc.) are added to M in a certain amount2+In the solution, the hydrotalcite is obtained by partial oxidation. In the preparation of FeAl-LDH, firstly a certain amount of FeSO is dissolved in the solution4And Al2(SO4)3Adjusting the pH to neutral and adding a certain amount of waterThe generated precipitate, namely FeAl-LDH with the interlaminar anion being sulfate radical, is fully reacted with the hydrogen peroxide. The oxidation method mainly has two problems, firstly, the strength and the dosage of the oxidant can have certain influence on the formation of the hydrotalcite; second is OH-/M2+And pH are also important factors affecting hydrotalcite. From this, it is clear that although the principle of the oxidation method for producing hydrotalcite is simple, oxidation of an oxidizing agent, pH, and hydroxide is difficult to control during the operation, and therefore hydrotalcite is generally not produced by the oxidation method.
The coprecipitation method is to add a certain amount of M under the condition of no oxygen2+、M3+Adding a certain amount of sodium hydroxide into water according to a certain proportion, slowly stirring to form hydrotalcite containing specific anions (SO)4 2-、CO3 2-、Cl-Etc.). When FeAl-LDH is prepared by a coprecipitation method, ferrous salt and trivalent aluminum salt in a certain proportion are dissolved in deionized water, the pH value is adjusted to about 9-10 by sodium hydroxide, the mixture is slowly stirred until the precipitation is complete, and the obtained precipitation is FexAly-LDH。
In conclusion, different M's were used in the synthesis of hydrotalcite by both the oxidation and coprecipitation methods2+/M3+And different OH-The content of (a) will have different effects on the formation of hydrotalcite and different products will be formed.
Hydrogen is a green and environment-friendly renewable energy source which can replace fossil energy. The electrolysis of water to produce hydrogen is one of the most efficient ways. However, since the electrolytic water is very slow in dynamics and has a large reaction overpotential, the oxygen evolution half-reaction of the anode severely limits the hydrogen evolution reaction efficiency of the cathode. Therefore, the development of highly efficient electrocatalytic oxygen evolution catalysts is of great importance to drive the commercialization of energy storage and conversion technologies. The noble metal catalyst has good catalytic performance for electrocatalytic oxygen evolution, but has high catalytic cost and poor stability. With the continuous development of material chemistry and the continuous innovation of synthesis technology, the practical process of preparing the low-cost high-efficiency OER (oxygen evolution reaction) catalyst is greatly enhanced.
Recent studies have shown that layered double oxides or hydroxides exhibit high activity and stability in electrocatalytic oxygen production reactions. The exchangeable anions between the layers are balanced with the positive charges between the layers, so that the catalyst presents electric neutrality and is easy to be loaded on a proper metal substrate. However, the traditional preparation method of the layered bimetallic catalyst loaded on the foamed nickel generally adopts a solvothermal method or methods such as spin coating and spray coating, and the catalyst is dispersed unevenly and combined infirm on the surface of the carrier, so that the charge transmission is hindered, the electrode is easy to fall off, and the final catalytic activity and the service life of the electrode are seriously influenced.
Disclosure of Invention
The present invention has been made to solve the above problems, and an object of the present invention is to provide an electrocatalytic oxygen evolution electrode, which is prepared from industrial wastewater and has excellent catalytic activity and stability, and a preparation and application thereof.
The invention provides a preparation method of an electrocatalytic oxygen evolution electrode, which is characterized by comprising the following steps: step 1, taking a trivalent chromium base salt solution as an electrolyte solution, taking foamed nickel as a cathode and taking iron as an anode to form a standard electrode system; step 2, connecting the positive pole of the direct current with the anode, connecting the negative pole of the direct current with the cathode, and introducing N into the electrolyte solution2Stopping ventilation after a period of time, then carrying out electrolytic reaction at constant potential or constant current until the electrolyte solution becomes colorless, taking out the cathode, cleaning, and drying at room temperature to obtain the electrocatalytic oxygen evolution electrode.
The preparation method of the electrocatalytic oxygen evolution electrode provided by the invention can also have the following characteristics: wherein, in the step 2, N is introduced into the electrolyte solution2The time of the reaction is 20min to 30 min.
The preparation method of the electrocatalytic oxygen evolution electrode provided by the invention can also have the following characteristics: wherein, the trivalent chromium-based salt contains chromium-based soluble salt, and the chromium-based soluble salt is any one or more of chromium chloride, chromium nitrate or chromium sulfate.
The preparation method of the electrocatalytic oxygen evolution electrode provided by the invention can also have the following characteristics: wherein the trivalent chromium-based salt contains sodium sulfate.
The preparation method of the electrocatalytic oxygen evolution electrode provided by the invention can also have the following characteristics: wherein, in the chromium-based salt solution, the molar concentration of sodium sulfate is 5 mmol/L-10 mmol/L, and the molar concentration of chromium element is 100 mmol/L-500 mmol/L.
The preparation method of the electrocatalytic oxygen evolution electrode provided by the invention can also have the following characteristics: wherein in the step 2, the current is less than 0.5mA/cm during the electrolytic reaction2。
The preparation method of the electrocatalytic oxygen evolution electrode provided by the invention can also have the following characteristics: in the step 1, the purity of the foamed nickel is 99.99%, the foamed nickel has a three-dimensional porous structure, and the porosity is about 95%.
The invention also provides an electrocatalytic oxygen evolution electrode which is prepared by the preparation method of the electrocatalytic oxygen evolution electrode and is characterized in that the electrode substrate of the electrocatalytic oxygen evolution electrode is foamed nickel, the active component is ferrochrome hydrotalcite, and the ferrochrome hydrotalcite is loaded and grown on the foamed nickel.
The invention also provides the application of the electrocatalytic oxygen evolution electrode in electrocatalytic cracking water oxygen evolution, which is characterized in that the electrocatalytic oxygen evolution electrode is used as an anode in an alkaline medium to electrolyze water to generate oxygen.
In the application of the electrocatalytic oxygen evolution electrode provided by the invention in electrocatalytic cracking water oxygen evolution, the electrocatalytic oxygen evolution electrode also has the following characteristics: wherein the alkaline medium is potassium hydroxide solution or sodium hydroxide solution, and the concentration is 0.1-10 mol/L.
Action and Effect of the invention
According to the preparation method of the electrocatalytic oxygen evolution electrode, a trivalent chromium base salt solution is used as an electrolyte solution, foamed nickel is used as a cathode, and iron is used as an anode to form a standard electrode system; connecting the positive pole of the direct current with the anode, connecting the negative pole of the direct current with the cathode, and introducing N into the electrolyte solution2After stopping introducing the gas for a period of time, carrying out electrolytic reaction by constant potential or constant current to obtain the electrocatalytic oxygen evolution electrode. During the reaction process, the anode iron is dissolved and adsorbed near the cathode under the action of the electric field, and the cathode also contains ironThe raw water generates hydroxide radical to create an alkaline environment to promote iron ions and chromium ions in the solution to generate iron-chromium hydrotalcite to be loaded on the foamed nickel. As the electrolysis proceeds, the excess chromium ions are directly combined with iron ions free in the solution to form iron-chromium hydrotalcite, and the iron-chromium hydrotalcite is precipitated in water in the form of flocs until the chromium ions in the solution are completely removed. Because the electrochemical sacrificial anode method is adopted for one-step synthesis, raw materials are derived from industrial wastewater, the traditional hydrotalcite preparation method by solvothermal or chemical precipitation-spin coating and the like is abandoned, and the conditions of high temperature, high pressure and the like are not needed, so that the preparation method has the advantages of simple process, mild conditions and environmental friendliness, and is suitable for the application of industrial electrolyzed water.
The electrode substrate of the prepared electrocatalytic oxygen evolution electrode is foamed nickel, and the active component is iron-chromium hydrotalcite loaded and grown on the foamed nickel.
The prepared electro-catalytic oxygen evolution electrode is used in electro-catalytic cracking water oxygen evolution, and because the iron-chromium hydrotalcite generated by cathode reduction is of a three-dimensional sheet structure, the structure has a very large electrochemical active area, and the oxygen evolution activity of the electro-catalyst is greatly increased. In addition, the iron-chromium hydrotalcite is reduced and grown on the foamed nickel substrate by utilizing the action of an external electric field and an alkaline environment created by hydroxyl generated by cathode reduced water, so that the charge transmission efficiency and the structural stability are ensured, the final catalytic activity of the electrode is enhanced, and the service life is prolonged. Therefore, the prepared electrocatalytic oxygen evolution electrode shows excellent oxygen evolution activity in an alkaline medium, and the current density is 100mA/cm2Can reach over potential of 290mV, and can replace noble metal to promote the development of an electrolytic water system in an alkaline medium.
In conclusion, the embodiment of the invention prepares the electrocatalyst by using the industrial chromium-containing wastewater, the reaction condition is mild, the environment is friendly, and the preparation method is simple and convenient. Cr in the material is directly derived from trivalent Cr in industrial wastewater, and pollutant Cr in the wastewater is degraded in a flocculation sedimentation mode in the process of gradually synthesizing the material. The iron-chromium hydrotalcite nano material loaded on the foamed nickel and generated by the electrochemical sacrificial anode method has better development prospect in the electrocatalytic oxygen evolution reaction. Not only solves the preparation problem of the layered bimetallic material loaded on the foamed nickel, but also can degrade the industrial chromium-containing wastewater by 100 percent. The method has clear and novel design thought and simple and convenient operation, and accords with the concept of green chemistry.
Drawings
FIG. 1 is a scanning electron micrograph of a FeCrxH hydrotalcite supported on nickel foam grown in example 1 of the present invention;
FIG. 2 is a transmission electron microscopy mapping (element distribution) graph of the iron-chromium hydrotalcite material exfoliated by ultrasonic exfoliation loaded on foamed nickel in example 1 of the present invention;
FIG. 3 is the results of the activity test of the electrocatalytic oxygen evolution electrode in example 1 of the present invention; and
fig. 4 is the result of the activity test of the electrocatalytic oxygen evolution electrode in example 2 of the present invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the electrocatalytic oxygen evolution electrode and the preparation and the application thereof are specifically described in the following with the embodiment and the attached drawings.
The raw materials and reagents used in the following examples can be purchased from conventional commercial sources unless otherwise specified.
The preparation method provided by the invention specifically comprises the following steps:
step 1, forming a standard electrode system by taking trivalent chromium base salt solution as electrolyte solution, foam nickel as a cathode and iron as an anode.
Wherein, the purity of the foamed nickel is 99.99%, the foamed nickel has a three-dimensional porous structure, and the porosity is about 95%.
The trivalent chromium-based salt comprises chromium-based soluble salt and anhydrous sodium sulfate, wherein the chromium-based soluble salt is any one or more of chromium chloride, chromium nitrate or chromium sulfate. In the chromium-based salt solution, the molar concentration of sodium sulfate is 5 mmol/L-10 mmol/L, and the molar concentration of chromium element is 100 mmol/L-500 mmol/L.
In the step 2, the current is less than 0.5mA/cm during the electrolytic reaction2In order to completely avoid the influence of dissolved oxygen, the prepared electrolyte solution needs to be introduced with nitrogen N before electrolysis220min～30min。
And 2, after the reaction is finished, taking out the cathode, cleaning the redundant electrolyte and precipitate with ultrapure water, and drying at room temperature to obtain the electrocatalytic oxygen evolution electrode.
In the embodiment of the invention, trivalent chromium base salt solution is used for simulating chromium-containing industrial wastewater, and the preparation method comprises the following steps: taking anhydrous sodium sulfate as a main electrolyte, and directly dissolving trivalent chromium salt in a sodium sulfate solution; wherein the molar concentration of the sodium sulfate is 5 mmol/L-10 mmol/L, and the molar concentration of the chromium element is 100 mmol/L-500 mmol/L.
Furthermore, in the examples of the present invention, a commercial nickel foam was pretreated: ultrasonic cleaning in acetone or alcohol to eliminate oil stain on the surface of foamed nickel, water washing to neutrality, ultrasonic activation in 1-2 mol/L hydrochloric acid, and final ultrasonic cleaning in ultrapure water at least twice.
In addition, in the embodiment of the present invention, the iron plate is pretreated: cutting the iron plate into proper size with a saw blade, and polishing with 100-1200 mesh abrasive paper until the oxide on the surface of the iron plate is completely cleaned.
In addition, in the embodiment of the invention, the prepared trivalent chromium base salt solution is used as an electrolyte solution, the pretreated foamed nickel is used as a cathode, and the treated iron plate is used as an anode to form a standard electrode system.
In the embodiment of the invention, the content change of trivalent chromium in the solution in the reaction process is detected by adopting an ammonium ferrous sulfate titration method, and the degradation effect of the trivalent chromium in the simulated wastewater is judged.
The electrode substrate of the prepared electrocatalytic oxygen evolution electrode is foamed nickel, and the active component is iron-chromium hydrotalcite loaded and grown on the foamed nickel.
The prepared electrocatalytic oxygen evolution electrode is applied to electrocatalytic cracking water oxygen evolution in an alkaline environment, and the specific process is as follows:
(1) performing electrochemical representation by using a CHI660 electrochemical workstation of a three-electrode electrochemical system, wherein the working electrode is an Ag/AgCl electrode with saturated potassium chloride filling liquid, a platinum wire is used as a counter electrode, the prepared electro-catalytic oxygen evolution electrode is used as the working electrode, the electrolyte is 0.1-10 mol/L potassium hydroxide solution, inert gas is continuously introduced in the test process for saturation treatment so as to thoroughly avoid the influence of dissolved oxygen, and the test temperature is kept at 25 ℃.
(2) Before recording the catalytic activity, the stability of the catalyst was determined by first performing 100 cyclic voltammetric scans in potassium hydroxide solution using sweep voltammetry (LSV). The test scan rate was 1 mV. s-1The electrode potentials are all subjected to iR correction for eliminating the influence caused by solution resistance and the like, and are converted into electrode potentials relative to a reversible electrode (RHE), and the calculation formula is as follows: overpotential + electrode potential + pH 0.0591+0.1976-iR-1.23v (v).
< example 1>
In this example, when the nickel foam was pretreated, the nickel foam was ultrasonically activated in 1mol/L hydrochloric acid. When the iron plate is pretreated, sand paper of 100 meshes, 500 meshes, 1000 meshes and 1200 meshes is sequentially used for polishing until iron oxide on the surface is completely cleaned.
Step 1, preparing an electrolyte solution by using chromium chloride and anhydrous sodium sulfate, wherein the molar concentration of the sodium sulfate is 5mmol/L, and the molar content of chromium element is 200 mmol/L. Introducing nitrogen for 30min for later use to completely avoid the influence of dissolved oxygen.
And 2, taking the solution prepared in the step 1 as an electrolyte solution, taking the pretreated foamed nickel as a cathode, and taking the treated iron plate as an anode to form a standard electrode system. Connecting the positive pole of the direct current with an iron plate, connecting the negative pole of the direct current with the nickel foam, and introducing N into the electrolyte solution220min, then constant current 0.4mA/cm2The electrolytic reaction is carried out for 1h, the electrolyte solution becomes colorless,the power is turned off and the electrode is removed. And (3) standing the reaction solution to ensure that flocs in the solution are completely settled and centrifugally removed. And washing the taken cathode with ultrapure water to remove electrolyte and precipitate, cleaning, and drying at room temperature to obtain the electrocatalytic oxygen evolution electrode.
In the electrolytic reaction in the step 2, the content change of trivalent chromium in the solution in the reaction process is detected by adopting an ammonium ferrous sulfate titration method, and the degradation effect of the trivalent chromium in the simulated wastewater is judged.
The obtained electrocatalytic oxygen evolution electrode was scanned by means of a scanning electron microscope (model ESCALB 250, manufactured by Thermo-VGscientific Co., U.S.A.) and the scanning electron microscope is shown in FIG. 1.
FIG. 1 is a scanning electron micrograph of a FeCr-LDH @ NF (FeCr-LDH @ NF) material supported on nickel foam grown in example 1 of the present invention.
FIG. 1 shows scanning electron micrographs of materials at different magnifications. As can be seen from fig. 1, the prepared ferrochrome hydrotalcite was flaky and grown on the surface of the foamed nickel skeleton, thereby indicating the successful preparation of the catalyst electrode material. The foam nickel skeleton can be obviously seen from figures 1a and 1b, a layer of substance is uniformly coated on the foam nickel skeleton material, the coating material can be seen from figures 1c and 1d to be formed by stacking porous sheet materials and is preliminarily judged to be an iron-chromium hydrotalcite material, and figures 1e and 1f can show that the iron-chromium hydrotalcite is uniform in shape and size and is formed by stacking sheets with the size of 200 nm-300 nm.
The FeCr-LDH thus obtained was characterized by a transmission electron microscope (manufactured by Thermo-VGscientific Co., U.S.A.) and the transmission electron microscopy mapping (element distribution) was shown in FIG. 2.
FIG. 2 is a transmission electron microscopy element distribution diagram of an iron-chromium hydrotalcite (FeCr-LDH) material obtained by carrying iron-chromium hydrotalcite grown on foamed nickel in example 1 of the present invention and carrying out ultrasonic exfoliation.
As shown in fig. 2, fig. 2b is a general view of fig. 2a, and fig. 2c and 2d show the element distribution diagrams of fe and cr, respectively, wherein the fe and cr elements can be found to be uniformly distributed, which indicates the successful preparation of the ferrochrome hydrotalcite. Fig. 2e is an element energy spectrum and an element ratio chart of iron and chromium, wherein the content of the iron element is 75.95%, and the content of the chromium element is 24.05%.
The prepared electrocatalytic oxygen evolution electrode is used for electrocatalytic cracking water oxygen evolution reaction in an alkaline environment. Wherein the electrolyte is 1M or 0.1M potassium hydroxide solution. The test results are shown in FIG. 3.
Fig. 3 is the result of the activity test of the electrocatalytic oxygen evolution electrode in example 1 of the present invention. Wherein the abscissa represents the overpotential (unit: V) and the ordinate represents the current density (unit: mA · cm)-2)。
As shown in FIG. 3, the electrocatalytic electrode shows a current density of 50mA/cm in an electrolyte with an extremely high oxygen evolution activity of 1mol/L in an alkaline medium2And 100mA/cm2The overpotential is 265mV and 290mV, and the current density is 50mA/cm in 0.1mol/L electrolyte2And 100mA/cm2Next, the overpotential was 275mV and 320 mV. The oxygen evolution reaction of the catalyst shows extremely high catalytic activity.
< example 2>
The same operation as that in embodiment 1 will not be described again in this embodiment.
In this example, when the nickel foam was pretreated, the nickel foam was ultrasonically activated in 2mol/L hydrochloric acid. When the iron plate is pretreated, sand paper of 100 meshes, 500 meshes and 1000 meshes is sequentially used for polishing until iron oxide on the surface is completely cleaned.
Step 1, preparing an electrolyte solution by using chromium sulfate and anhydrous sodium sulfate, wherein the molar concentration of the sodium sulfate is 10mmol/L, and the molar content of chromium element is 100 mmol/L. Introducing nitrogen for 30min for later use to completely avoid the influence of dissolved oxygen.
And 2, carrying out an electrolytic reaction for 2 hours at a constant potential of 0.1V, turning the electrolyte solution into colorless, turning off a power supply, and taking out the electrode. And cleaning and drying to obtain the electrocatalytic oxygen evolution electrode.
The electrocatalytic oxygen evolution electrode obtained in this example was subjected to an activity test, the test results of which are shown in fig. 4.
Fig. 4 is the result of the activity test of the electrocatalytic oxygen evolution electrode in example 2 of the present invention. Wherein the abscissa represents the overpotential (unit:v), and the ordinate represents the current density (unit: mA.cm-2)。
As shown in fig. 4, the electrocatalytic electrode showed slightly lower oxygen evolution activity in alkaline medium than that of example 1, and it can be seen that the content of chromium element in the simulated wastewater solution influences the activity of the prepared electrocatalytic oxygen evolution catalyst. In 1mol/LKOH electrolyte, the current density of the ferrochrome hydrotalcite loaded on the foamed nickel is 50mA/cm2And 100mA/cm2Next, the overpotential was 270mV and 380 mV.
Effects and effects of the embodiments
The preparation method of the electrocatalytic oxygen evolution electrode provided by the embodiment of the invention adopts trivalent chromium base salt solution as electrolyte solution, foamed nickel as cathode and iron as anode to form a standard electrode system; connecting the positive pole of the direct current with the anode, connecting the negative pole of the direct current with the cathode, and introducing N into the electrolyte solution2After 20min to 30min, carrying out electrolytic reaction with constant potential or constant current to obtain the electro-catalytic oxygen evolution electrode. In the reaction process, anode iron is dissolved and adsorbed near a cathode under the action of an electric field, and the cathode reduces water to generate hydroxyl to create an alkaline environment so as to promote iron ions and chromium ions in the solution to generate iron-chromium hydrotalcite to be loaded on the foamed nickel. As the electrolysis proceeds, the redundant chromium ions are directly combined with iron ions free in the solution to generate iron-chromium hydrotalcite which is deposited in the form of flocs in water until the chromium ions in the solution are completely removed. Meanwhile, the content change of the trivalent chromium in the solution in the reaction process is detected by adopting an ammonium ferrous sulfate titration method, and the degradation effect of the trivalent chromium in the simulated wastewater is judged.
Because the electrochemical sacrificial anode method is adopted for one-step synthesis, raw materials are derived from industrial wastewater, the traditional hydrotalcite preparation method by solvothermal or chemical precipitation-spin coating and the like is abandoned, and the conditions of high temperature, high pressure and the like are not needed, so that the preparation method has the advantages of simple process, mild conditions and environmental friendliness, and is suitable for the application of industrial electrolyzed water.
The electrode substrate of the prepared electrocatalytic oxygen evolution electrode is foamed nickel, and the active component is iron-chromium hydrotalcite loaded and grown on the foamed nickel.
The prepared electro-catalytic oxygen evolution electrode is used in electro-catalytic cracking water oxygen evolution, and because the iron-chromium hydrotalcite generated by cathode reduction is of a three-dimensional sheet structure, the structure has a very large electrochemical active area, and the oxygen evolution activity of the electro-catalyst is greatly increased. In addition, the iron-chromium hydrotalcite is reduced and grown on the foamed nickel substrate by utilizing the action of an external electric field and an alkaline environment created by hydroxyl generated by cathode reduced water, so that the charge transmission efficiency and the structural stability are ensured, the final catalytic activity of the electrode is enhanced, and the service life is prolonged. Therefore, the prepared electrocatalytic oxygen evolution electrode shows excellent oxygen evolution activity in an alkaline medium, and the current density is 100mA/cm2Can reach over potential of 290mV, and can replace noble metal to promote the development of an electrolytic water system in an alkaline medium.
In conclusion, the embodiment of the invention prepares the electrocatalyst by using the industrial chromium-containing wastewater, the reaction condition is mild, the environment is friendly, and the preparation method is simple and convenient. Cr in the material is directly derived from trivalent Cr in industrial wastewater, and pollutant Cr in the wastewater is degraded in a flocculation sedimentation mode in the process of gradually synthesizing the material. The hydrotalcite nano material generated by the electrochemical sacrificial anode method has better development prospect in the treatment of industrial wastewater containing trivalent chromium and the electro-catalytic oxygen evolution reaction. Not only solves the preparation problem of the layered bimetallic material loaded on the foamed nickel, but also can degrade the industrial chromium-containing wastewater by 100 percent. The method has clear and novel design thought and simple and convenient operation, and accords with the concept of green chemistry.
The above embodiments are preferred examples of the present invention, and are not intended to limit the scope of the present invention.
Claims (7)
1. A preparation method of an electrocatalytic oxygen evolution electrode is characterized by comprising the following steps:
step 1, taking a trivalent chromium base salt solution as an electrolyte solution, taking foamed nickel as a cathode and taking iron as an anode to form a standard electrode system;
step 2, connecting the positive pole of the direct current with the anode, connecting the negative pole of the direct current with the cathode, and introducing the electrolyte solutionInto N2And stopping ventilation after a period of time, then carrying out electrolytic reaction at constant potential or constant current until the electrolyte solution becomes colorless, taking out the cathode, cleaning, and drying at room temperature to obtain the electrocatalytic oxygen evolution electrode.
2. The method for preparing an electrocatalytic oxygen evolution electrode according to claim 1, characterized in that:
wherein in the step 2, N is introduced into the electrolyte solution2The time of the reaction is 20min to 30 min.
3. The method for preparing an electrocatalytic oxygen evolution electrode according to claim 1, characterized in that:
the trivalent chromium-based salt contains chromium-based soluble salt, and the chromium-based soluble salt is any one or more of chromium chloride, chromium nitrate or chromium sulfate.
4. The method for preparing an electrocatalytic oxygen evolution electrode according to claim 3, characterized in that:
wherein the trivalent chromium-based salt contains sodium sulfate.
5. The method for preparing an electrocatalytic oxygen evolution electrode according to claim 4, characterized in that:
wherein, in the chromium-based salt solution, the molar concentration of the sodium sulfate is 5 mmol/L-10 mmol/L, and the molar concentration of the chromium element is 100 mmol/L-500 mmol/L.
6. The method for preparing an electrocatalytic oxygen evolution electrode according to claim 1, characterized in that:
wherein in the step 2, the current is less than 0.5mA/cm during the electrolytic reaction2。
7. The method for preparing an electrocatalytic oxygen evolution electrode according to claim 1, characterized in that:
in the step 1, the purity of the foamed nickel is 99.99%, the foamed nickel has a three-dimensional porous structure, and the porosity is 95%.
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