CN109097787B - Preparation method and application of metal polyphenol complex crystal electrocatalyst - Google Patents
Preparation method and application of metal polyphenol complex crystal electrocatalyst Download PDFInfo
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- CN109097787B CN109097787B CN201810878119.7A CN201810878119A CN109097787B CN 109097787 B CN109097787 B CN 109097787B CN 201810878119 A CN201810878119 A CN 201810878119A CN 109097787 B CN109097787 B CN 109097787B
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- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
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- C25B11/031—Porous electrodes
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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
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
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- 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 relates to a preparation method and application of a metal polyphenol complex crystal electro-catalyst, wherein the preparation method specifically comprises the following steps: and (3) carrying out in-situ growth on the nickel foam by using the transition metal salt and the polyphenol substances through a solvothermal method to obtain the nickel foam. The invention organically combines transition metal elements with relative abundant reserves in the nature with polyphenol compound ligands to prepare the high-efficiency electrocatalyst for electrolyzing water to generate oxygen. The preparation process is optimized to determine proper reaction conditions, and the prepared point catalyst has many advantages, such as excellent performance, controllable structure and high stability.
Description
Technical Field
The invention relates to an electrocatalyst, in particular to a preparation method and application of a metal polyphenol complex crystal electrocatalyst.
Background
With the continuous development and progress of the human society, the demand of human beings on sustainable energy is continuously increased, and the traditional fossil energy has the problems of non-regeneration and serious pollution of combustion products, so that sufficient power cannot be provided for the advance of the society in future. Therefore, the development of clean and sustainable new energy becomes the key to solve the energy crisis. The current crisis can be effectively relieved by preparing hydrogen and oxygen through electrolyzing water. One of the half reactions of water splitting, the Oxygen Evolution Reaction (OER), severely limits the efficiency of water splitting due to its slow kinetics.
Noble metals (e.g., Ru, Ir oxides) are the most active oxygen evolution reaction catalysts recognized to date. However, the application of noble metal catalysts in industrial hydrogen production is limited to a great extent due to the characteristics of high price, resource shortage, easy agglomeration and corrosion in electrolyte and the like, so that the search for oxygen evolution catalysts with high efficiency, stability and low overpotential becomes a key for breaking through the bottleneck.
Currently, Fe, Ni-based transition metal oxides, sulfides, phosphides, hydroxides have been widely developed for Oxygen Evolution Reaction (OER) electrocatalysts, exhibiting excellent OER, and have been hot spots for the design and selection of catalyst materials.
Active Metal Organic Frameworks (MOFs) are formed by combining metal ions or clusters and organic ligands through coordination bonds, and are applied to a plurality of fields such as gas storage, drug release, catalysis, sensing and the like due to large adjustability in components, structures and pore diameters. In the application of water oxidation catalysis, the nanometer material obtained by directly carbonizing or phosphorizing MOFs shows better catalytic activity, however, the pyrolysis process can cause the decomposition of organic ligands and the agglomeration of central metal, the structural integrity is damaged, and the number of exposed active sites is reduced.
Disclosure of Invention
The invention aims to provide a preparation method of a metal polyphenol complex crystal electrocatalyst, which solves the problems of high production cost, easy collapse of structure, poor stability, serious energy waste caused by higher overpotential and the like of the existing oxygen-making electrocatalyst.
The preparation method of the metal polyphenol complex crystal electro-catalyst provided by the invention specifically comprises the following steps: and (3) carrying out in-situ growth on the nickel foam by using the transition metal salt and the polyphenol substances through a solvothermal method to obtain the nickel foam.
The invention organically combines transition metal elements with relative abundant reserves in the nature with polyphenol compound ligands to prepare the high-efficiency electrocatalyst for electrolyzing water to generate oxygen. The preparation process is optimized to determine proper reaction conditions, and the prepared electrocatalyst has many advantages, such as excellent performance, controllable structure and high stability.
The invention further provides that the transition metal salt is one or more of iron salt, manganese salt, cobalt salt and nickel salt. The electro-catalyst prepared by adopting the iron salt has good properties of transition metals Fe and Ni, can be directly applied to catalytic oxygen evolution reaction, can obtain excellent catalytic activity and greatly reduce the production cost.
Wherein the iron salt is Fe (NO)3)3、FeCl3Or Fe2(SO4)3。
The polyphenol substances are selected from one or more of flavanol, flavonol and tannic acid. Tannic acid is preferably used.
The invention further provides that the feeding ratio of the solution of the transition metal salt to the polyphenol substances is 0.02-0.1 mol/L: 0.15-1.0 g;
preferably 0.02-0.06 mol/L: 0.2-1.0 g; for example: 0.2g of 0.026mol/L, 0.5g of 0.046mol/L, 0.2g of 0.056mol/L, 0.5g of 0.056mol/L, 1.0g of 0.056mol/L and 0.4g of 0.066 mol/L;
more preferably 0.04 to 0.06 mol/L:0.4 to 0.6g, most preferably 0.05 mol/L:0.5 g.
The solvent in the solution of the transition metal salt specifically refers to a solvent in the following solvothermal method; that is, the above ratio includes the ratio of the transition metal salt, the polyphenol substance, and the solvent; at a ratio of 0.05 mol/L:0.5g of the transition metal salt is contained in an amount of 0.05mol per 1L of the solvent, and 0.5g of the polyphenol substance is contained in the solvent.
The invention further provides a solvent thermal method which takes one or more selected from N, N-dimethylformamide, absolute ethyl alcohol, water and methanol as a solvent;
preferably, the solvent is a mixed solution of N, N-dimethylformamide, absolute ethyl alcohol and water; particularly preferably a mixed solution of N, N-dimethylformamide, absolute ethyl alcohol and water in a volume ratio of 12-16: 1: 1;
preferably, the volume ratio is 12:1:1, 14:1:1, 16:1: 1; in particular 14:1: 1.
The invention further provides that the operation temperature of the solvothermal method is 100-180 ℃, and the time is 10-16 h; preferably, the operation temperature is 110-130 ℃, and the time is 10-14 h; most preferably at a temperature of 120 ℃ for 12 h.
The invention further provides that the foamed nickel is subjected to acidification treatment in advance; the acidification treatment can effectively remove oxides on the surface of the foamed nickel; the method specifically comprises the following steps: placing the foamed nickel in a hydrochloric acid solution with the concentration of 2-4 mol/L, and carrying out ultrasonic treatment for 20-50 min;
preferably, the ultrasonic power in the acidification treatment process is 400-1000W;
the sonication time is preferably 30 min.
The invention further provides that after the acidification treatment, the cleaning is also carried out; the cleaning can effectively remove organic substances adsorbed on the surface of the foamed nickel; the method specifically comprises the following steps: cleaning the acidified foam nickel with water, putting the cleaned foam nickel into a mixed solution of ethanol and acetone with a volume ratio of 1: 1-4, and carrying out ultrasonic treatment for 20-50 min; taking out, washing with water, and oven drying.
Preferably, in the cleaning, the volume ratio of ethanol to acetone is 1: 1; the power of the ultrasonic wave is 400-1000W;
the sonication time is preferably 30 min.
Preferably, the drying temperature is 50-70 ℃, and more particularly 60 ℃.
The invention provides a preferable scheme, and the preparation method comprises the following steps:
1) putting the foamed nickel into a hydrochloric acid solution with the concentration of 2-4 mol/L, performing ultrasonic treatment for 20-50 min, cleaning with water, then putting into a mixed solution of ethanol and acetone with the volume ratio of 1: 1-4, and performing ultrasonic treatment for 20-50 min; taking out, washing with water, and oven drying;
2) iron salt and polyphenol compounds are added according to the proportion of 0.04-0.06 mol/L: 0.4-0.6 g, adding the iron salt into the solvent, and adding the polyphenol compound after completely dissolving to completely dissolve the iron salt.
Wherein the polyphenol compound is selected from one or more of flavanol, flavonol and tannic acid;
the solvent is a mixed solution of N, N-dimethylformamide, absolute ethyl alcohol and water in a volume ratio of 12-16: 1: 1;
3) placing the foamed nickel obtained in the step 1) into the solution obtained in the step 2), heating to 110-130 ℃, and carrying out in-situ growth for 10-14 h to obtain the nickel-based composite material.
Another object of the present invention is to provide a metal polyphenol complex crystal electrocatalyst prepared by any one of the above-mentioned preparation methods.
The present invention also provides the application of the metal polyphenol complex crystal electrocatalyst in electrocatalytic oxygen evolution reaction.
The invention has at least the following advantages:
the invention grows iron, nickel and polyphenol complex crystals with electrocatalytic water oxidation performance in situ on large-size foamed nickel with a three-dimensional porous structure by a one-step solvothermal method.
The preparation method is simple and feasible, the raw materials are cheap and easy to obtain, and the components are controllable; compared with the existing Fe and Ni-based transition metal oxides, sulfides, phosphides and hydroxides, the prepared metal polyphenol complex crystal electro-catalyst still has excellent electro-catalytic oxygen evolution activity in a strong alkaline potassium hydroxide solution environment; nickel ions generated in an acidic synthesis environment can form a synergistic effect, so that the catalytic performance of the metal polyphenol complex crystal is improved; the metal polyphenol complex crystal electro-catalyst prepared by the invention has good stability.
Drawings
FIG. 1 is a photograph of a pure nickel foam in comparison with a metal polyphenol complex crystal electrocatalyst prepared in example 1;
FIG. 2 is a scanning electron microscope photograph showing the metal polyphenol complex crystal electrocatalyst prepared in example 1 at different magnifications;
FIG. 3 is a graph showing a polarization curve of the electrocatalyst for a metal polyphenol complex crystal prepared in example 1 according to the oxygen evolution reaction process;
FIG. 4 is a graph showing polarization curves of the metal polyphenol complex crystal electrocatalysts prepared in examples 2 to 4 with respect to the oxygen evolution reaction process;
FIG. 5 is a graph showing polarization curves of the metal polyphenol complex crystal electrocatalysts prepared in examples 5 to 7 with respect to the oxygen evolution reaction process;
FIG. 6 is a chronopotentiometric curve of the metal polyphenol complex crystal electrocatalyst prepared in example 1.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications. The reagents or instruments used are conventional products available from regular distributors, not indicated by the manufacturer.
The foamed nickel used in the following examples was purchased from the department of sales of source batteries of tarnish force in taiyuan; the area used is 1 × 3cm2。
Example 1
The present embodiment provides a method for preparing a metal polyphenol complex crystal electrocatalyst, comprising the following steps:
1) putting foamed nickel (Ni) into hydrochloric acid solution with the concentration of 3mol/L, performing ultrasonic treatment for 30min at the power of 800W, taking out, cleaning with deionized water, putting into a mixed solution of ethanol and acetone with the volume ratio of 1:1, and performing ultrasonic treatment for 30min at the power of 800W; taking out, cleaning with deionized water, and drying the foamed nickel in a 60 deg.C oven for 180 min;
2) after 10.5mL of N, N-dimethylformamide, 0.75mL of absolute ethanol and 0.75mL of deionized water were mixed, 0.2424g of iron nitrate granules were added, and after magnetic stirring was performed until complete dissolution, 0.5g of tannic acid was added thereto and stirring was performed until complete dissolution (the solution was indigo).
3) And (2) placing the foamed nickel obtained in the step 1) into the solution obtained in the step 2 (placing the foamed nickel in a reaction kettle, and enabling the foamed nickel to form a certain inclination angle with the inner wall of the reaction kettle, so that the foamed nickel is fully contacted with the solution), heating to 120 ℃, carrying out in-situ growth for 12 hours, naturally cooling to room temperature, cleaning with deionized water, and placing in a drying oven at 60 ℃ for drying to obtain the polyphenol complex crystal electrocatalyst (foamed nickel attached with the indigo substance).
Examples 2 to 4
This example provides a method for preparing a metal polyphenol complex crystal electrocatalyst, which is different from example 1 only in that the weights of the iron nitrate are 0.0969g, 0.1939g, and 0.3878g, respectively.
Examples 5 to 7
This example provides a method for preparing a metal polyphenol complex crystal electrocatalyst, which is different from example 1 only in that the weights of tannic acid are 0.15g, 0.4g, and 0.6g, respectively.
Comparative example 1
This comparative example provides a method for preparing an electrocatalyst, which differs from example 1 only in that "ferric nitrate" is not added in step 2), and nickel salt of the same concentration is used instead, specifically as follows:
"2") after mixing 10.5mL of N, N-dimethylformamide, 0.75mL of anhydrous ethanol and 0.75mL of deionized water, 0.1717g of nickel nitrate was added and stirred until completely dissolved. "
Comparative example 2
This comparative example provides a method of preparing an electrocatalyst which differs from example 1 only in that no metal salt is added, only involving the treated nickel foam participating in the solvothermal reaction. Experimental example 1
The electrocatalytic water oxidation performance of the metal polyphenol complex crystal electrocatalysts ((FeNi) -Tan/NF) prepared in examples 1 to 7 in a KOH solution (pH 14) having a concentration of 1mol/L was verified. The specific operation is as follows:
a standard three-electrode system is adopted, an Ag/AgCl electrode is taken as a reference electrode, a Pt wire electrode is taken as a counter electrode, the feeding ratio of ferric salt and tannic acid is 50mmol/L:0.5g, a linear scanning cyclic voltammetry experiment is carried out on the metal polyphenol complex crystal electro-catalyst prepared in the example 1-3, 1mol/L KOH solution is used as an electrolyte, the water oxidation oxygen evolution performance is measured within the range of 0-1.0V (vs. Ag/AgCl) of an applied potential window at the sweeping speed of 2mV/s, the change of electrode current along with the scanning potential is recorded,
1. the picture of the (FeNi) -Tan/NF prepared in example 1 is shown in FIG. 1; as shown in FIG. 1, the digital picture corresponding to pure nickel (Ni) foam and (FeNi) -Tan/NF prepared in example 1 shows that the appearance color of the sample is greatly changed before and after the reaction; a) the figure (front figure) corresponds to the metallic color material being the processed pure foam nickel, and b) the figure (back figure) corresponds to the indigo color foam nickel material being the correspondingly prepared (FeNi) -Tan/NF sample; in the (FeNi) -Tan/NF sample prepared by the method, the (FeNi) -Tan grows on the foam nickel in situ.
2. FIG. 2 shows the corresponding SEM pictures of (FeNi) -Tan/NF prepared in example 1 in (a), (b), (c) and (d), which shows that the prepared (FeNi) -Tan has the morphology of particle assembly and interconnected pores inside, and is beneficial to oxygen desorption and active site increase.
3. Figure 3 shows a plot of the OER polarisation curve (jvs V) characterisation in example 1 and comparative example 2 (barenf). It is clear from the figure that the OER of (FeNi) -Tan/NF obtained in example 1 was 50mA cm-2The oxygen evolution overpotentials of the nickel foam are respectively 208mV, which is lower than 500mV needed by the nickel foam material to reach the same current density, so that the overpotentials to be applied by the (FeNi) -Tan/NF and Ni foam are obviously reduced. (in FIG. 3, the abscissa is the potential value converted into the reversible hydrogen potential, and the ordinate is the current density at different potential values;)
4. FIG. 4 is a graph representing the OER polarization curve (j vs V) of (FeNi) -Tan/NF prepared in examples 2-4; (in FIGS. 4 to 5, the abscissa is the potential value converted into the reversible hydrogen potential, and the ordinate is the current density at different potential values;)
5. FIG. 5 is a graph representing the OER polarization curves (j vs V) of (FeNi) -Tan/NF obtained in examples 5 to 7.
As can be seen from FIGS. 3 to 5, the (FeNi) -Tan/NF prepared in example 1 has the best performance.
6. FIG. 6 shows the stability testing of the (FeNi) -Tan/NF product of example 1, characterized by chronopotentiometry with a set current density of 50, 100, 150mA cm-2The change with time of the recording potential within 40000s was recorded. The chronopotentiometric curve shows that the product has strong structural stability. (in FIG. 6, the abscissa represents the intensity of the applied radiation with respect to the time and the ordinate represents the current density)
The results of the electrochemical tests show that (FeNi) -Tan/NF in the material has the lowest overpotential compared with Ni foam, and the prepared catalyst has the overpotential of 50 mA-cm-2The overpotential of the Oxygen Evolution Reaction (OER) was 208mV, respectively. Compared with pure foam nickel with certain catalytic activity, the foam nickel has the concentration of 50mA cm-2The overpotential for the treatment is 500mV, which is respectively reduced by 292 mV. That is, (FeNi) -Tan/NF obtained in example 1 had the best electrocatalytic effect.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (7)
1. A preparation method of a metal polyphenol complex crystal electro-catalyst is characterized in that transition metal salt and polyphenol substances are subjected to in-situ growth on foamed nickel by a solvothermal method to prepare the metal polyphenol complex crystal electro-catalyst; the transition metal salt is Fe (NO)3)3、FeCl3Or Fe2(SO4)3(ii) a The feeding ratio of the solution of the transition metal salt to the polyphenol substances is 0.05-0.1 mol/L: 0.4-0.5 g; the polyphenol substances are tannic acid; the solvent is a mixed solution of N, N-dimethylformamide, absolute ethyl alcohol and water in a volume ratio of 12-16: 1: 1; the operation temperature of the solvothermal method is 100-180 ℃, and the time is 10-16 h.
2. The method according to claim 1, wherein the operating temperature is 110-130 ℃ and the time is 10-14 h.
3. The method according to claim 1 or 2, characterized in that the nickel foam is previously subjected to an acidification treatment as follows: and (3) placing the foamed nickel into a hydrochloric acid solution with the concentration of 2-4 mol/L, and carrying out ultrasonic treatment for 20-50 min.
4. The preparation method according to claim 3, wherein the acidified nickel foam is washed with water, and then placed into a mixed solution of ethanol and acetone in a volume ratio of 1: 1-4 for ultrasonic treatment for 20-50 min; taking out, washing with water, and oven drying.
5. The method of claim 1, comprising the steps of:
1) putting the foamed nickel into a hydrochloric acid solution with the concentration of 2-4 mol/L, performing ultrasonic treatment for 20-50 min, cleaning with water, then putting into a mixed solution of ethanol and acetone with the volume ratio of 1: 1-4, and performing ultrasonic treatment for 20-50 min; taking out, washing with water, and oven drying;
2) ferric salt and tannic acid are added according to the proportion of 0.05-0.06 mol/L: 0.4-0.5 g, adding iron salt into a solvent, and adding the tannic acid after completely dissolving to completely dissolve the iron salt;
the solvent is a mixed solution of N, N-dimethylformamide, absolute ethyl alcohol and water in a volume ratio of 12-16: 1: 1;
3) placing the foamed nickel obtained in the step 1) into the solution obtained in the step 2), heating to 110-130 ℃, and carrying out in-situ growth for 10-14 h to obtain the nickel-based composite material.
6. A metal polyphenol complex crystal electrocatalyst according to any one of claims 1 to 5, wherein the metal polyphenol complex crystal electrocatalyst is prepared by a process as described in any one of claims.
7. Use of the metal polyphenol complex crystal electrocatalyst according to claim 6 for electrocatalytic oxygen evolution reaction.
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