CN114045514B - Preparation method of V@CoxP catalyst - Google Patents
Preparation method of V@CoxP catalyst Download PDFInfo
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- CN114045514B CN114045514B CN202111461136.9A CN202111461136A CN114045514B CN 114045514 B CN114045514 B CN 114045514B CN 202111461136 A CN202111461136 A CN 202111461136A CN 114045514 B CN114045514 B CN 114045514B
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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
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- 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
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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
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention belongs to the technical field of electrolyzed water catalytic materials, and particularly relates to a preparation method of a V@CoxP catalyst; the method comprises the following steps: (1) Fixing the pretreated foam nickel in a beaker containing 2-methylimidazole solution, and adding Co (NO) with a certain concentration 3 ) 2 ·6H 2 Pouring the O solution into the 2-methylimidazole solution fixed with the foam nickel, and standing at room temperature for reaction 5 h; washing with deionized water after the reaction is finished, and airing to obtain ZIF-67/NF; (2) Put ZIF-67/NF in Na 3 VO 4 Is put into a vacuum drying box, washed and dried after the reaction is finished, and V@Co (OH) is obtained 2 A catalytic material; (3) Placing the catalytic material obtained in the step (2) and sodium hypophosphite in a tube furnace, and calcining under nitrogen atmosphere to obtain V@Co x A P catalyst; the invention uses foam nickel as a matrix, obtains the OER electrocatalyst with high activity through simple hydrothermal reaction and phosphating treatment, can keep good catalytic activity for a long time in alkaline environment, and has wide application prospect and good economic value.
Description
Technical Field
The invention belongs to the technical field of electrolyzed water catalytic materials, and particularly relates to a preparation method of a V@CoxP catalyst.
Background
The gradual development of world economy and the continuous increase of the demand of people for energy resources lead to the increasing exhaustion of non-renewable energy resources, bring about the problems of environmental pollution such as greenhouse effect and serious ozone layer dane, prevent the sustainable development of society, bring about great harm to the health and life of people, and therefore the searching and developing of new energy resources and renewable energy resources become the great importance of the sustainable development of world economy and human society.
The electrochemical process plays a vital role in the exploration and development of new energy, and in the electrochemical process, the electric energy and the chemical energy are mutually converted, so that the sustainable development of the hydrogen energy economy is greatly promoted. However, the inhibition of the electrolysis of water is mainly derived from the oxygen evolution reaction of the anode (OER for short), which is a complex four-electron transfer process with a high reaction barrier, and the whole process involves three activated intermediates (OH - 、O 2- And OOH (OOH) - ) Adsorption process of (2) and O 2 The development of the anode OER catalytic material is important to the improvement of the hydrogen production efficiency of the electrolysis water. The OER catalysts currently accepted to be excellent in performance are noble metal catalysts such as ruthenium dioxide and iridium dioxide; however, the advantages of low reserves and high price are difficult to achieve wide application, while the general transition metal-based catalyst has the disadvantages of weak performance, poor stability and the like, so that the catalyst is indispensable for realizing energy conversion and is widely applied to society, and the design and development of an electrocatalytic system with high efficiency, low cost, sustainability and stability are indispensable.
Disclosure of Invention
The invention overcomes the defects of the prior art, and aims to provide a preparation method of a V@CoxP catalyst, which synthesizes an electrocatalyst with excellent catalytic performance and good stability by adopting strategies of different elements with complementary composite performances.
In order to solve the technical problems, the invention adopts the following technical scheme: a preparation method of a V@CoxP catalyst comprises the following steps:
(1) Fixing the pretreated foam nickel in a beaker containing 2-methylimidazole solution, and then fixing the foam nickel with a certain concentrationCo(NO 3 ) 2 ·6H 2 Pouring the O solution into the 2-methylimidazole solution fixed with the foam nickel, and standing at room temperature for reaction 5 h; washing with deionized water after the reaction is finished, and airing to obtain ZIF-67/NF;
(2) Put ZIF-67/NF in Na 3 VO 4 Is put into a vacuum drying box, washed and dried after the reaction is finished, and V@Co (OH) is obtained 2 A catalytic material;
(3) Placing the catalytic material obtained in the step (2) and sodium hypophosphite in a tube furnace, and calcining under nitrogen atmosphere to obtain V@Co x And (3) a P catalyst.
The method provided by the invention is economical and applicable, the preparation process is simple, and the prepared V@Co x The P catalyst has high-efficiency oxygen evolution function. The invention uses foam nickel as a matrix, obtains the OER electrocatalyst with high activity through simple hydrothermal reaction and phosphating treatment, can keep good catalytic activity for a long time in alkaline environment, and has wide application prospect and good economic value.
Further, the pretreated foam nickel means to remove impurities on the surface, and the specific method is as follows: respectively carrying out ultrasonic treatment on the foam nickel in dilute HCl solution and deionized water for 10 min and 2 min, and airing.
Further, the concentration of the 2-methylimidazole solution in the step (1) was 0.4 mol/L, and the concentration of cobalt ions before the reaction of the mixed solution in the step (1) was 0.05 mol/L.
Further, na in the step (2) 3 VO 4 The concentration of vanadium ions in the solution is 0.4 mol/L; the Co (NO) 3 ) 2 ·6H 2 O and Na 3 VO 4 The molar ratio of (2) was 4:1.
Further, the Na is 3 VO 4 The molar ratio of the sodium hypophosphite to the sodium hypophosphite is 1:23.
Further, the hydrothermal reaction condition in the step (2) is 100 ℃,3 h.
Further, the calcination process in the step (3) is to heat at a rate of 5 ℃/min to 400 ℃ at room temperature, and keep 1 h.
In addition, the invention also provides an application of the V@CoxP catalyst prepared by the preparation method as an OER catalyst in electrolytic water oxygen evolution electrocatalysis.
The invention also provides a catalytic performance test method for applying the V@CoxP catalyst prepared by the preparation method to electrolytic water oxygen evolution electro-catalysis, which comprises the following steps: the performance of the carbon-based conductive material after heat treatment is tested in a standard three-electrode system by adopting a cyclic voltammetry method, wherein a carbon rod is used as a counter electrode, a mercury/mercury oxide electrode (Hg/HgO) is used as a reference electrode, and the electrolyte is 1M KOH.
Compared with the prior art, the invention has the following beneficial effects:
1. the preparation method has the advantages of simple operation process, low cost, high efficiency, sufficient source and easy realization of large-scale application.
2. V@Co x The P composite catalyst has good conductivity and high stability, improves the catalytic activity of OER, reduces the production cost of oxygen evolution electrodes, saves more energy in the whole water electrolysis process, and provides a practical technical method for high-efficiency water electrolysis catalyst materials.
3. V@Co of the invention x The P catalyst has stronger oxygen evolution catalytic activity in an alkaline solution environment and very stable performance, and has good application prospect in industrial development.
Drawings
Fig. 1: SEM photograph of ZIF-67 material obtained in example 1;
fig. 2: V@Co obtained in example 1 x XRD pattern of the P catalyst;
fig. 3: V@Co obtained in example 1 x SEM image of P catalyst;
fig. 4: V@Co obtained in example 1 x EDX mapping graph of P catalyst;
fig. 5: V@Co obtained in example 1 x EDX energy spectrum of the P catalyst;
fig. 6: V@Co obtained in example 1 x XPS spectrum of P catalyst;
fig. 7: V@Co prepared in example 1 x P catalytic material and noble metal IrO 2 The catalyst has OER catalytic performance when the water is electrolyzed in a KOH solution of 1M to produce oxygen.
Fig. 8: ZIF-67 prepared in example 1 and V@Co x P and Co from example 2 x The P catalytic material has OER catalytic performance when electrolyzed in 1M KOH solution to produce oxygen.
Fig. 9: V@Co prepared in example 1 x P catalytic material and noble metal IrO 2 Impedance test patterns of catalysts when electrolyzed in KOH solution of 1M to produce oxygen, respectively.
Fig. 10: V@Co obtained in example 1 x Voltage-time stability test curve of P-catalyst in alkaline (1M KOH) electrolyte.
Detailed Description
The invention is further illustrated below with reference to specific examples.
Example 1
2-methylimidazole of 1.3136 g was weighed, dissolved in 40 mL deionized water, and the pretreated nickel foam (3 cm. Times.4 cm) was placed in the prepared 2-methylimidazole solution and sonicated for 20 s, and the nickel foam was separately held in a beaker containing the above solution. Weigh 0.5821 g Co (NO) 3 ) 2 ·6H 2 O, dissolving in 40 mL deionized water, pouring into the 2-methylimidazole solution, and reacting at room temperature under standing condition for 5 h. Then the foam nickel is rinsed with deionized water and dried to obtain ZIF-67. Weigh 0.1 Na 0.1 g 3 VO 4 Dissolving in 35 mL deionized water, ultrasonic treating to dissolve completely, transferring the solution into a reaction kettle, adding into prepared ZIF-67, reacting at 100deg.C for 3 h, washing with water, and air drying to obtain V@Co (OH) 2 . Then respectively placing the mixture and sodium hypophosphite 1 g at two ends of two porcelain boats, placing the porcelain boats in a tube furnace, heating to 400 ℃ at a speed of 5 ℃/min under nitrogen atmosphere and keeping the temperature at 1 h, and finally cooling to room temperature to obtain V@Co x And (3) a P catalyst.
Example 2
Is the same as in example 1 except that Na 3 VO 4 The content of (2) is changed from 100 mg to 0 mg, and other synthesis conditions are not adoptedChanges to obtain Co x And (3) a P catalyst.
Example 3
Is the same as in example 1 except that Na 3 VO 4 The content of (2) is changed from 100 mg to 50 mg, and other synthesis conditions are not changed, so that V can be obtained 50 @Co x P catalyst, current density of 10 mA cm -2 An overpotential 247 mV is required.
Example 4
Is the same as in example 1 except that Na 3 VO 4 The content of (2) is changed from 100 mg to 200 mg, and other synthesis conditions are not changed, so that V can be obtained 200 @Co x P catalyst, current density of 10 mA cm -2 An overpotential 230 mV is required.
The necessary structural characterization and property studies were carried out on the catalytic materials prepared by the above method, as shown below. FIG. 1 is an SEM photograph of ZIF-67 after hydrothermal treatment, and it can be seen that the morphology of ZIF-67 is lamellar. FIG. 2 is V@Co x The X-ray diffraction (XRD) pattern of the P catalytic material, "#" is the peak of nickel foam, and is compared with standard cards (29-0496 and 29-0497), indicating that Co was successfully synthesized x P. FIG. 3 shows the obtained V@Co x SEM photograph of P catalyst, it can be seen that V@Co x The P particles are uniformly supported on the foamed nickel substrate. FIG. 4 shows the obtained V@Co x The EDX mapping graph of the P catalytic material shows that the catalytic material contains Co, V, P, ni four elements and is uniformly distributed in the sample, and meanwhile, the V element can be successfully doped into Co x In P, further indicated is V@Co x Successful synthesis of P-catalyst. FIG. 5 shows the obtained V@Co x The EDX spectrum of the P catalytic material shows that the content of Ni element in the material is the highest, 53.5 and Wt percent, the content of P element is 29.7 and Wt percent, the content of Co element is 11.1Wt percent, and the content of V element is 5.7 and Wt percent. FIG. 6 shows the obtained V@Co x X-ray photoelectron spectrum (XPS) spectrum of P catalyst, it can be seen from XPS spectrum of Co 2P that Co 2P spectrum is divided into two spin orbit coupled Co 2+ (780.1, 799.2 eV) and Co 3+ (780.1, 795.9 eV) shows that Co in the oxidized state, possibly Co in the 0-valence state on the surface, is oxidized by airThe gas is oxidized to produce. The two peaks at 778.8 and 793.8 eV can be ascribed to Co 2p 3/2 And Co 2p 1/2 Since Co in CoP is in the 0-valence state. Furthermore, the two peaks of 786.7 and 803.5 eV can be attributed to the two oscillating satellite peaks. From the XPS spectrum of V2 p, it can be seen that the two strong peaks 516.9 and 524.4 eV correspond to V2 p, respectively 3/2 And V2 p 1/2 The fitted peaks centered on 513.7, 516.9 and 521.1 eV are V respectively for V in the 0-valence state of (2) 3+ 、V 4+ 、V 5+ . From the XPS spectrum of P2P, it can be seen that P2P is divided into three major peaks, where the peaks at 130.1 and 129.5 eV can be assigned to P2P in the 0-valent state P 1/2 And P2P 3/2 This is because of Co x P is zero-valent and the peak at 134, eV, can be attributed to the P-O state because the P element at the surface is oxidized.
The electrocatalytic water oxygen production (OER) performance test was performed on the catalytic material prepared by the method described above in a standard three-electrode electrolytic cell, in which a carbon rod was used as a counter electrode, a mercury/mercury oxide electrode (Hg/HgO) was used as a reference electrode, and V@Co prepared in example 1 x P catalyst (0.5X cm) 2 ) As a working electrode, the electrocatalytic OER performance was tested using cyclic voltammetry with an electrolyte of 1M KOH.
We tested the electrochemical catalytic performance of the catalyst using a standard three electrode system with the catalyst prepared as the working electrode.
As can be seen from FIG. 7, V@Co x The P catalyst shows the best OER catalytic performance when the current density is 10 mA cm -2 At the time, the overpotential only needs 208 mV, and the noble metal IrO 2 The catalyst had a current density of 10 mA cm -2 At the time of overpotential, 237 mV, V@Co is needed x OER performance of the P catalyst exceeds IrO 2 A catalyst.
As can be seen from FIG. 8, when the current density is 10 mA cm -2 When the overpotential of the precursor ZIF-67 is 336 mV, co x The overpotential of P is 231 mV, V@Co x The overpotential of the P catalyst only needs 208 mV, from which it can be seen that V@Co x The performance of the P catalyst is superior to Co x P and precursor ZIF-67, demonstrating V@Co x The P catalyst can further improve the catalytic effect of electrolyzed water.
As can be seen from FIG. 9, irO with noble metal 2 Compared with the catalyst, V@Co x The least resistance of the P-catalyst reveals the fastest electron transfer capability.
As can be seen in FIG. 10, V@Co x The overpotential of the P catalyst was 10 mA cm at a current density -2 The catalyst can be maintained for more than 12 hours and is in a stable state, the performance is not reduced, and the excellent stability of the catalyst is shown.
Claims (3)
1. The preparation method of the V@CoxP catalyst is characterized by comprising the following steps of: weighing 1.3136 g of 2-methylimidazole, dissolving in 40 mL deionized water, placing 3cm x 4cm of pretreated foam nickel in the prepared 2-methylimidazole solution, performing ultrasonic treatment for 20 s, and fixing the foam nickel in a beaker containing the 2-methylimidazole solution; weigh 0.5821 g Co (NO) 3 ) 2 ·6H 2 O, dissolving in 40 mL deionized water, pouring into the 2-methylimidazole solution, and reacting under the condition of standing at room temperature for 5 h; then washing foam nickel with deionized water, and airing to obtain ZIF-67; weigh 0.1 Na 0.1 g 3 VO 4 Dissolving in 35 mL deionized water, ultrasonic treating to dissolve completely, transferring the solution into a reaction kettle, adding into prepared ZIF-67, reacting at 100deg.C for 3 h, washing with water, and air drying to obtain V@Co (OH) 2 The method comprises the steps of carrying out a first treatment on the surface of the Then V@Co (OH) 2 Respectively placing the ceramic boat and sodium 1 g hypophosphite at two ends, placing in a tube furnace, heating to 400deg.C at a rate of 5deg.C/min under nitrogen atmosphere and maintaining at 1 h, and cooling to room temperature to obtain V@Co x And (3) a P catalyst.
2. Use of the v@coxp catalyst prepared by the preparation method of claim 1 as OER catalyst in electrolytic water oxygen evolution electrocatalyst.
3. A method for testing the catalytic performance of the v@coxp catalyst prepared by the preparation method according to claim 1 in the electrolytic water oxygen evolution electro-catalysis, which is characterized in that: the performance of the carbon-based conductive material after heat treatment is tested in a standard three-electrode system by adopting a cyclic voltammetry method, wherein a carbon rod is used as a counter electrode, a mercury/mercury oxide electrode (Hg/HgO) is used as a reference electrode, and the electrolyte is 1M KOH.
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| ES2549636T3 (en) * | 2012-04-05 | 2015-10-30 | Commissariat à l'énergie atomique et aux énergies alternatives | Method for preparing a catalyst that mediates the evolution of H2, said catalyst and uses thereof |
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| WO2020068872A1 (en) * | 2018-09-24 | 2020-04-02 | Massachusetts Institute Of Technology | Electrochemical oxidation of organic molecules |
| CN112439459A (en) * | 2019-08-29 | 2021-03-05 | 复旦大学 | Ultrathin nanosheet material with coexisting crystal and amorphous interface and application thereof in water electrolysis |
| CN110935480A (en) * | 2019-11-28 | 2020-03-31 | 浙江理工大学 | Vanadium-doped cobalt phosphide nano-thorn catalytic material for full-hydrolytic reaction |
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