CN114045514A - Preparation method of V @ CoxP catalyst - Google Patents
Preparation method of V @ CoxP catalyst Download PDFInfo
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- CN114045514A CN114045514A CN202111461136.9A CN202111461136A CN114045514A CN 114045514 A CN114045514 A CN 114045514A CN 202111461136 A CN202111461136 A CN 202111461136A CN 114045514 A CN114045514 A CN 114045514A
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Abstract
The invention belongs to the technical field of electrolytic 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 concentration3)2·6H2Pouring the O solution into the 2-methylimidazole solution fixed with the foam nickel, and standing at room temperature for 5 hours for reaction; after the reaction is finished, washing with deionized water and drying in the air to obtain ZIF-67/NF; (2) placing ZIF-67/NF in Na3VO4After the reaction is finished, washing and drying to obtain V @ Co (OH)2A catalytic material; (3) putting the catalytic material obtained in the step (2) and sodium hypophosphite into a tubular furnace, and calcining in a nitrogen atmosphere to obtain V @ CoxA P catalyst; the invention uses bubblesThe foamed nickel is used as a matrix, and the high-activity OER electrocatalyst is obtained through simple hydrothermal reaction and phosphating treatment, can keep good catalytic activity for a long time in an alkaline environment, and has wide application prospect and good economic value.
Description
Technical Field
The invention belongs to the technical field of electrolytic water catalytic materials, and particularly relates to a preparation method of a V @ CoxP catalyst.
Background
The gradual development of the world economy and the continuous increase of the demand of people for energy resources lead to the exhaustion of non-renewable energy resources, bring serious environmental pollution problems such as greenhouse effect and ozone layer Deng, cause obstacles to the development of social sustainability, and bring great harm to human health and life, so that the search and development of new energy resources and renewable energy resources become important in the sustainable development of the world economy and human society.
For the exploration and development of new energy, the electrochemical process plays a crucial role, and in the electrochemical process, electric energy and chemical energy are mutually converted, so that the sustainable development of hydrogen energy economy is greatly promoted. However, the obstruction in the water electrolysis process mainly comes from the oxygen evolution reaction (abbreviated as OER) of the anode, the OER process is a complex four-electron transfer process, the reaction barrier is high, and the whole process involves three activated intermediate products (OH)-、O2-And OOH-) Adsorption process and O2The desorption process, so the development of the anode OER catalytic material is crucial to improving the hydrogen production efficiency of the electrolysis water. OER catalysts currently recognized to have excellent performance are noble metal catalysts such as ruthenium dioxide and iridium dioxide; however, the storage amount is small, the price is expensive, and the like, so that the wide application is difficult to achieve, and a general transition metal-based catalyst has the defects of weak performance, poor stability and the like, so that the design and development of an efficient, cheap, sustainable and stable electrocatalysis system which is required to realize energy conversion and is generally applied to the society is indispensable.
Disclosure of Invention
The invention overcomes the defects of the prior art, and aims to solve the technical problem of providing a preparation method of a V @ CoxP catalyst, wherein an electrocatalyst with excellent catalytic performance and good stability is synthesized by adopting a strategy of different elements with complementary composite properties.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a method of making a V @ cox p catalyst, comprising the steps of:
(1) fixing the pretreated foam nickel in a beaker containing 2-methylimidazole solution, and adding Co (NO) with a certain concentration3)2·6H2Pouring the O solution into the 2-methylimidazole solution fixed with the foam nickel, and standing at room temperature for 5 hours for reaction; after the reaction is finished, washing with deionized water and drying in the air to obtain ZIF-67/NF;
(2) placing ZIF-67/NF in Na3VO4After the reaction is finished, washing and drying to obtain V @ Co (OH)2A catalytic material;
(3) putting the catalytic material obtained in the step (2) and sodium hypophosphite into a tubular furnace, and calcining in a nitrogen atmosphere to obtain V @ CoxAnd (3) a P catalyst.
The method provided by the invention is economical and applicable, the preparation process is simple, and the prepared V @ CoxThe P catalyst has high-efficiency oxygen evolution function. The invention takes the foam nickel as a matrix, obtains the high-activity OER electrocatalyst through simple hydrothermal reaction and phosphorization treatment, can keep good catalytic activity for a long time in an alkaline environment, and has wide application prospect and good economic value.
Further, the pretreated nickel foam is used for removing impurities on the surface, and the specific method comprises the following steps: respectively carrying out ultrasonic treatment on the foamed nickel in a 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) is 0.4 mol/L, and the concentration of cobalt ions before the reaction of the mixed solution in the step (1) is 0.05 mol/L.
Further, Na in step (2)3VO4The concentration of vanadium ions in the solution is 0.4 mol/L; the Co (NO)3)2·6H2O and Na3VO4Is 4: 1.
Further, said Na3VO4With sodium hypophosphiteThe molar ratio is 1: 23.
Further, the hydrothermal reaction condition in the step (2) is 100 ℃ and 3 hours.
Further, the calcination process in step (3) is heating to 400 ℃ at room temperature at a rate of 5 ℃/min, and keeping for 1 h.
In addition, the invention also provides application of the V @ CoxP catalyst prepared by the preparation method as an OER catalyst in water electrolysis oxygen evolution electrocatalysis.
The invention also provides a method for testing the catalytic performance of the V @ CoxP catalyst prepared by the preparation method in electrolytic water oxygen evolution electrocatalysis, which comprises the following steps: the performance of the carbon-based conductive material after heat treatment is used as a working electrode, a carbon rod is used as a counter electrode, a mercury/mercury oxide electrode (Hg/HgO) is used as a reference electrode, a cyclic voltammetry method is adopted to test the performance in a standard three-electrode system, 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 sources and easy realization of large-scale application.
2. V@CoxThe P composite catalyst has good conductivity and high stability, improves the catalytic activity of OER, reduces the production cost of the oxygen evolution electrode, saves more energy in the whole water electrolysis process, and provides an implementable technical method for a high-efficiency water electrolysis catalyst material.
3. V @ Co of the inventionxThe P catalyst has stronger oxygen evolution catalytic activity in an alkaline solution environment, shows 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 1xXRD spectrum of P catalyst;
FIG. 3: v @ Co obtained in example 1xSEM image of P catalyst;
FIG. 4: v @ Co obtained in example 1xEDX mapping plot of P catalyst;
FIG. 5: v @ Co obtained in example 1xEDX energy spectrum of P catalyst;
FIG. 6: v @ Co obtained in example 1xXPS spectrum of P catalyst;
FIG. 7: v @ Co obtained in example 1xP catalytic material and noble metal IrO2The catalyst has OER catalytic performance when water is electrolyzed to generate oxygen in a KOH solution of 1M.
FIG. 8: ZIF-67 and V @ Co prepared in example 1xP and Co from example 2xThe P catalytic materials respectively have OER catalytic performance when water is electrolyzed in a KOH solution of 1M to generate oxygen.
FIG. 9: v @ Co obtained in example 1xP catalytic material and noble metal IrO2The catalysts were subjected to impedance test in a 1M KOH solution for producing oxygen by electrolyzing water.
FIG. 10: v @ Co obtained in example 1xVoltage-time stability test curve of P catalyst in alkaline (1M KOH) electrolyte.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
1.3136 g of 2-methylimidazole were weighed, dissolved in 40 mL of deionized water, and the pretreated nickel foam (3 cm. times.4 cm) was placed in the prepared 2-methylimidazole solution and sonicated for 20 seconds to fix the nickel foam in a beaker containing the above solutions, respectively. 0.5821 g of Co (NO) were weighed out3)2·6H2And O, dissolving the mixed solution in 40 mL of deionized water, pouring the mixed solution into the 2-methylimidazole solution, and reacting for 5 hours at room temperature under a standing condition. And then washing the foamed nickel by using deionized water, and airing to obtain ZIF-67. Weigh 0.1 g of Na3VO4Dissolving the mixed solution in 35 mL of deionized water, performing ultrasonic treatment to completely dissolve the mixed solution, transferring the solution into a reaction kettle, adding the prepared ZIF-67, reacting for 3 hours at 100 ℃, washing with water and drying to obtain V @ Co (OH)2. Then respectively putting the mixture and 1 g of sodium hypophosphite into two ends of two porcelain boats, putting the porcelain boats into a tube furnace, heating the porcelain boats to 400 ℃ at the speed of 5 ℃/min under the nitrogen atmosphere and keeping the temperature for 1 h,finally cooling to room temperature to obtain V @ CoxAnd (3) a P catalyst.
Example 2
Same as example 1 except that Na3VO4The content of (A) is changed from 100 mg to 0 mg, other synthesis conditions are not changed, and Co can be obtainedxAnd (3) a P catalyst.
Example 3
Same as example 1 except that Na3VO4The content of (A) is changed from 100 mg to 50 mg, other synthesis conditions are not changed, and V can be obtained50@CoxP catalyst, current density up to 10 mA cm-2Overpotential 247 mV is required.
Example 4
Same as example 1 except that Na3VO4The content of (A) is changed from 100 mg to 200 mg, other synthesis conditions are not changed, and V can be obtained200@CoxP catalyst, current density up to 10 mA cm-2The overpotential is required to be 230 mV.
The necessary structural characterization and property studies were performed on the catalytic material prepared by the above method, as shown below. FIG. 1 is an SEM photograph of ZIF-67 after hydrothermal treatment, showing that the morphology of ZIF-67 is plate-like. FIG. 2 is V @ CoxThe X-ray diffraction (XRD) pattern, "#" is the peak of the nickel foam, and the comparison with the standard cards (29-0496 and 29-0497) shows that the Co is successfully synthesizedxAnd P. FIG. 3 shows the resulting V @ CoxSEM photograph of P catalyst, it can be seen that V @ CoxThe P particles were uniformly supported on a foamed nickel substrate. FIG. 4 shows the resulting V @ CoxEDX mapping chart of P catalytic material, it can be seen that the catalytic material contains four elements of Co, V, P and Ni, and is uniformly distributed in a sample, and at the same time, it can be proved that V element is successfully doped to CoxIn P, further indicates V @ CoxSuccessful synthesis of the P catalyst. FIG. 5 shows the resulting V @ CoxAn EDX energy spectrum of the P catalytic material shows that the content of Ni element in the material is the highest and is 53.5 Wt%, the content of P element is 29.7 Wt%, the content of Co element is 11.1Wt%, and the content of V element is 5.7 Wt%. FIG. 6 shows the resulting V @ CoxX-ray photoelectron energy of P catalystSpectrum (XPS) spectrum, from which it can be seen that Co 2p spectrum is divided into two spin-orbit coupling Co2+(780.1, 799.2 eV) and Co3+(780.1, 795.9 eV), indicating the existence of oxidation state Co, it is probably generated by oxidation of Co in surface 0 valence state by oxygen in air. The two peaks at 778.8 and 793.8 eV can be attributed to Co 2p3/2And Co 2p1/2Because Co in CoP is in the 0 valence state. Furthermore, the two peaks at 786.7 and 803.5 eV can be attributed to two vibrosatellite peaks. From the XPS spectrum of V2 p, it can be seen that two strong peaks 516.9 and 524.4 eV correspond to V2 p respectively3/2And V2 p1/2V of valence 0, and fitting peaks centered at 513.7, 516.9 and 521.1 eV are respectively V3+、V4+、V5+. From the XPS spectrum of P2P, it can be seen that P2P is divided into three main peaks, among which the peaks at 130.1 and 129.5 eV can be assigned to P2P with P in the 0 valence state1/2And P2P3/2This is because of CoxP is in the zero valence state, and the peak at 134 eV can be attributed to the P-O state because the P element at the surface is oxidized.
The catalytic material prepared by the method is subjected to an electro-catalytic water oxygen production (OER) performance test in a standard three-electrode electrolytic cell, a carbon rod is used as a counter electrode in the electrolytic cell, a mercury/mercury oxide electrode (Hg/HgO) is used as a reference electrode, and V @ Co prepared in example 1xP catalyst (0.5X 1 cm)2) As a working electrode, the electrocatalytic OER performance was tested using cyclic voltammetry with an electrolyte of 1M KOH.
The electrochemical catalytic performance of the catalyst is tested by adopting a standard three-electrode system with the prepared catalyst as a working electrode.
As can be seen in FIG. 7, V @ CoxThe P catalyst showed the best OER catalytic performance when the current density was 10 mA cm-2When the over-potential is only 208 mV, the noble metal IrO2The catalyst has a current density of 10 mA cm-2When the over-potential is 237 mV, V @ CoxThe OER performance of the P catalyst exceeds that of IrO2A catalyst.
As can be seen from FIG. 8, when the current density was 10 mA cm-2At first, beforeThe overpotential of bulk ZIF-67 requires 336 mV, CoxThe overpotential of P needs 231 mV, V @ CoxThe overpotential of the P catalyst is only 208 mV, so that V @ Co can be seenxThe performance of the P catalyst is superior to that of CoxP and the precursor ZIF-67, proving V @ CoxThe P catalyst can further improve the catalytic effect of the electrolyzed water.
As can be seen in FIG. 9, IrO is a noble metal2Catalyst comparison, V @ CoxThe P-catalyst has the lowest resistance, revealing the fastest electron transfer capability.
As can be seen in FIG. 10, V @ Co can be seenxOverpotential of P catalyst at current density of 10 mA cm-2The catalyst can be maintained for more than 12 hours and in a stable state, the performance is not reduced, and the excellent stability of the catalyst is shown.
Claims (9)
1. A preparation method of V @ CoxP catalyst is characterized by comprising the following steps:
(1) fixing the pretreated foam nickel in a beaker containing 2-methylimidazole solution, and then adding Co (NO)3)2·6H2Pouring the O solution into the 2-methylimidazole solution fixed with the foam nickel, and standing at room temperature for 5 hours for reaction; after the reaction is finished, washing with deionized water and drying in the air to obtain ZIF-67/NF;
(2) placing ZIF-67/NF in Na3VO4After the reaction is finished, washing and drying to obtain V @ Co (OH)2A catalytic material;
(3) putting the catalytic material obtained in the step (2) and sodium hypophosphite into a tubular furnace, and calcining in a nitrogen atmosphere to obtain V @ CoxAnd (3) a P catalyst.
2. The method for preparing a V @ CoxP catalyst according to claim 1, wherein the pretreated foamed nickel is subjected to surface impurity removal by the following specific method: respectively carrying out ultrasonic treatment on the foamed nickel in a dilute HCl solution and deionized water for 10 min and 2 min, and airing.
3. The method of claim 1 wherein the concentration of the 2-methylimidazole solution in step (1) is 0.4 mol/L and the concentration of cobalt ions before the reaction of the mixed solution of step (1) is 0.05 mol/L.
4. The process of claim 1 wherein in step (2) Na is added3VO4The concentration of vanadium ions in the solution is 0.4 mol/L; the Co (NO)3)2·6H2O and Na3VO4Is 4: 1.
5. The process of claim 1 wherein said Na @ CoxP catalyst is added to said catalyst3VO4The molar ratio of the sodium hypophosphite to the sodium hypophosphite is 1: 23.
6. The process for preparing a V @ CoxP catalyst according to claim 1, wherein the hydrothermal reaction in the step (2) is carried out at 100 ℃ for 3 hours.
7. The method for preparing a V @ CoxP catalyst according to claim 1, wherein the calcination process in the step (3) is performed by heating at room temperature and at a rate of 5 ℃/min to 400 ℃ and maintaining for 1 h.
8. Use of the V @ cox p catalyst prepared by the preparation process of any one of claims 1 to 7 as an OER catalyst in electrolytic water oxygen evolution electrocatalysis.
9. A method for testing the catalytic performance of the V @ CoxP catalyst prepared by the preparation method of any one of claims 1 to 7 in the electro-catalysis of oxygen evolution by electrolysis of water, which is characterized by comprising the following steps: the performance of the carbon-based conductive material after heat treatment is used as a working electrode, a carbon rod is used as a counter electrode, a mercury/mercury oxide electrode (Hg/HgO) is used as a reference electrode, a cyclic voltammetry method is adopted to test the performance in a standard three-electrode system, and the electrolyte is 1M KOH.
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