CN113277573B - PEM (proton exchange membrane) electrolyzed water anode catalyst and preparation method thereof - Google Patents
PEM (proton exchange membrane) electrolyzed water anode catalyst and preparation method thereof Download PDFInfo
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- CN113277573B CN113277573B CN202110727144.7A CN202110727144A CN113277573B CN 113277573 B CN113277573 B CN 113277573B CN 202110727144 A CN202110727144 A CN 202110727144A CN 113277573 B CN113277573 B CN 113277573B
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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 discloses a PEM electrolyzed water anode catalyst and a preparation method thereof, belonging to the technical field of nano materials and catalysis. The anode catalyst oxide of the invention has a chemical formula of AxRu1‑xO2‑δThe preparation method takes soluble Ru salt and soluble transition metal salt as raw materials, complex ligands are added, an improved sol-gel method is adopted, low-temperature roasting is adopted, and the prepared nano particles are small and uniform in particle size. The preparation process is simple and feasible, the precursor salt is flexible to select, and the prepared nano catalyst has high activity and high stability on oxygen precipitation reaction, and provides a new choice for a commercial anode catalyst for hydrogen production by water electrolysis.
Description
Technical Field
The invention belongs to the technical field of nano materials and catalysis, and particularly relates to a preparation method of a PEM (proton exchange membrane) electrolyzed water anode catalyst and application of the PEM electrolyzed water anode catalyst in a PEM electrolyzed water device.
Background
Hydrogen energy has long been regarded as the ultimate energy, and hydrogen production by water electrolysis driven by renewable energy sources such as photovoltaic, wind power generation, hydroelectric and the like is a promising hydrogen production strategy. The current main electrolysis water solutions include alkaline water electrolysis, PEM electrolysis water. Compared with alkaline water electrolysis, PEM electrolysis water shows the advantages of quick response, flexible load current, pure hydrogen produced and the like, and the advantages determine the strong adaptability of PEM electrolysis water to fluctuating renewable energy sources. Thus, the scale-up of PEMs is promoted in all countries. The main challenge in this process is the development of an efficient stable anode catalyst, and since most non-noble metals are not suitable for OER under acidic conditions due to their thermodynamic instability in acid, the main research is focused on noble metals such as Ru and Ir and their oxides. Currently, most products adopt iridium oxide as an OER catalyst, but the problems of rare reserves, high price, poor activity and the like become the limit of popularization of PEM devices. Compared with iridium, ruthenium has considerable reserves and price, but the defect of poor stability is not negligible. Therefore, the modification of ruthenium oxide to prepare ruthenium-based catalysts with both high activity and high stability is a real need.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a PEM electrolyzed water anode catalyst which is a nano oxide particle material, wherein the chemical formula of the oxide is AxRu1-xO2-δA is one of transition metals Ta, Nb, V, Mo, W, Zr, Ti and Y, wherein x is a mole fraction and is more than 0 and less than 1, and more than 0 and less than 2.
The invention further provides a preparation method of the PEM electrolyzed water anode catalyst, which comprises the following steps:
(1) preparing a mixed solution containing soluble Ru salt and soluble transition metal salt according to a certain stoichiometric ratio;
(2) preparing a complex ligand dispersion liquid, and adjusting the pH value to 9-10;
(3) mixing the mixed solution obtained in the step (1) with a complexing ligand dispersion liquid, and evaporating and solidifying to obtain a metal chelate precursor;
(4) and carrying out thermal decomposition and oxidation on the metal chelate precursor to obtain the modified nano ruthenium oxide particles.
Wherein the soluble Ru salt is RuCl3、Ru(acac)3、Ru(CH3COO)3At least one of (1).
Among them, the transition metal salt is selected from the chloride, nitrate, organic acid salt and alkoxide of the transition metal.
Wherein, the solvent in the step 1 is water, methanol, ethanol, acetone or isopropanol.
Wherein the complexing ligand is oxygen-containing polybasic organic acid, preferably, the complexing ligand is at least one of ethylene glycol bisaminoethyl ether tetraacetic acid, ethylene diamine tetraacetic acid, citric acid, lactic acid or polyacrylic acid.
Wherein the molar ratio of the complexing ligand to the metal in the metal salt is 0.01-100.
Wherein, the pH is adjusted by alkaline substances, and the alkaline substances are preferably ammonia water or ethylenediamine.
Wherein, the evaporation and solidification method comprises heating, stirring and evaporation, vacuum heating and evaporation or freeze drying.
When the solvent with strong volatility such as alcohols is involved, heating, stirring and evaporation are preferably selected, and the heating temperature is 80-110 ℃.
Wherein the metal chelate precursor is pyrolyzed and oxidized at 200-500 ℃.
Preferably, the metal chelate precursor is pyrolytically oxidized at 200-300 ℃.
Further preferably, the temperature programming step is a two-step temperature raising method, and the temperature raising rate is 1-5 ℃/min.
Regarding the realization of the pyrolytic oxidation, the roasting method is preferred, the precursor obtained in the step 3 is placed in a porcelain boat, placed in a muffle furnace or a tubular furnace, programmed to 200-500 ℃ in an air atmosphere or by introducing oxygen, and naturally cooled to room temperature after the reaction, wherein the roasting time is 6 hours, and the preferred atmosphere is air. The heating mode is a two-step heating method, and the preferred heating rate is 5 ℃/min.
The invention has the beneficial effects that:
1. the modified ruthenium oxide nano-particles prepared by the method adopt an improved sol-gel method and low-temperature roasting, and the prepared nano-particles have small and uniform particle size;
2. the preparation process described by the invention is simple and easy to implement, the precursor salt is flexible to select, and the synthesis method has high expansibility in preparing the nano oxide, thereby providing a preparation way for the fields of catalysis, energy, environment and the like of the nano oxide;
3. the nano catalyst prepared by the invention has high activity and high stability for oxygen precipitation reaction, and provides a new choice for a commercialized anode catalyst for hydrogen production by water electrolysis;
4. the invention utilizes the self-made PEM device to assemble and test the catalytic performance of the catalyst in a real application scene, and the cathode obtains pure hydrogen without purification treatment, thereby providing reference for the transition of the catalyst from laboratory research to industrial application.
Drawings
FIG. 1 shows Ta obtained in example 10.1Ru0.9O2-δX-ray diffraction patterns (a) and (b) structural characterization and elemental profile of the nanocatalyst;
FIG. 2 shows Ta in example 10.1Ru0.9O2-δThe method comprises the following steps that (1) a catalytic performance diagram (a) and an EIS diagram (b) of an acidic oxygen precipitation reaction of a nano catalyst are tested in a three-electrode system by utilizing a linear voltammetry scanning method and an alternating current impedance method;
FIG. 3 shows Ta in embodiment 10.1Ru0.9O2-δThe nano catalyst is used for a PEM electrolytic device at 50mA/cm2Stability test chart at current density.
Detailed Description
Example 1
Ta0.1Ru0.9O2-δThe synthesis of the nano catalyst comprises the following steps:
1) preparing a tantalum ethanol solution: and weighing tantalum ethoxide with corresponding mass in a glove box according to the molar ratio of the tantalum ruthenium element, taking out, and immediately dissolving with 3mL of absolute ethyl alcohol for later use.
2) Preparing mixed metal salt solution: weighing ruthenium trichloride with corresponding mass according to the molar ratio of the tantalum ruthenium element, dissolving the ruthenium trichloride in 2-3mL of absolute ethanol, adding the tantalum ethanol solution obtained in the step 1), and performing ultrasonic dispersion to obtain a solution 1 for later use;
3) preparing a ligand solution: weighing ethylene glycol bisaminoethylether tetraacetic acid and citric acid with corresponding mass according to the molar ratio of 1:1, dissolving the ethylene glycol bisaminoethylether tetraacetic acid and the citric acid in 5mL of deionized water, and adjusting the pH value to 9-10 by using strong ammonia water to obtain a solution 2;
4) heating the solution 2 in a heating sleeve to 90 ℃, injecting the solution 1 into the heated solution 2, keeping the temperature at 90 ℃, stirring and evaporating, and curing to obtain a metal chelate precursor;
5) and (2) placing the precursor in a muffle furnace in an air atmosphere, heating to 200 ℃ in a first stage of procedure, roasting for 3 hours, then heating to 300 ℃, roasting for 3 hours at a heating rate of 5 ℃/min, carrying out pyrolysis oxidation on the metal chelate, and naturally cooling to room temperature after roasting is finished to obtain the modified nano ruthenium oxide particles.
And performing test characterization on the sample. FIG. 1a is Ta0.1Ru0.9O2-δX-ray diffraction pattern of the nanocatalyst, FIG. 1b is Ta0.1Ru0.9O2-δThe morphology and the element distribution of the nano-catalyst.
Example 2
Ta obtained in example 10.1Ru0.9O2-δThe nano catalyst is used for oxygen precipitation reaction in an acid environment, a three-electrode test system is adopted, a platinum wire is used as a counter electrode, and a mercury/mercurous sulfate electrode is used as a reference electrode; taking 5mg of Ta0.1Ru0.9O2-δDispersing the nano catalyst into uniform catalyst ink in 1mL of mixed solvent of water and isopropanol, uniformly dripping a certain amount of the uniform catalyst ink on a 5mm glassy carbon electrode serving as a working electrode, wherein the loading capacity is 0.25mg/cm2To be tested. The test system selects 0.5M sulfuric acid solution as electrolyte, oxygen is continuously introduced to maintain an oxygen saturation state, and electrochemical data are tested by utilizing a linear voltammetry scanning method and an alternating current impedance method, wherein the linear voltammetry scanning rate is 5mV/s, and the test potential of the alternating current impedance is 1.5V (vs. The results showed that, as shown in FIG. 2a, at 10mA/cm2At current density of (1), Ta0.1Ru0.9O2-δOverpotential of nano catalyst is 258mV, commercial RuO2The overpotential of the catalyst is 358 mV; ta as shown in FIG. 2b0.1Ru0.9O2-δThe charge transfer resistance of the nanocatalyst is less than that of the commercial RuO2Charge transfer resistance of the catalyst, indicating Ta0.1Ru0.9O2-δThe charge transfer speed between the nano-catalyst interface and the electrolyte is higher, showing thatHigh oxygen evolution catalytic activity.
Example 3
Ta obtained in example 10.1Ru0.9O2-δThe nano catalyst is used for testing in a PEM water electrolysis device, and two electrodes are used for testing; the cathode uses a commercial platinum-carbon catalyst for hydrogen evolution reaction and the anode uses Ta0.1Ru0.9O2-δThe nano catalyst is used for oxygen evolution reaction, after the catalysts of the anode and the cathode are prepared into a membrane electrode by a spraying-pressure conversion method, the loading capacity of the anode catalyst is 1.5mg/cm2And assembled into a PEM device. At 50mA/cm2Measuring Ta with 0.5M sulfuric acid solution as electrolyte at a flow rate of 20ml/min under current density0.1Ru0.9O2-δThe stability of the nano-catalyst is shown in figure 3, and the result shows that the operation life of the nano-catalyst exceeds 400h, which indicates that Ta0.1Ru0.9O2-δThe nano catalyst has high stability and corrosion resistance, and the covalent property of Ru-O is strengthened due to the modification of Ta species, the reactivity of lattice oxygen is enhanced, and the generation of high-valence Ru species is inhibited at the same time, so the nano catalyst becomes one of the most competitive anode oxygen evolution catalysts in a PEM (proton exchange membrane) electrolytic water device.
The foregoing is a more detailed description of the invention in connection with specific/preferred embodiments and is not intended to limit the practice of the invention to those descriptions. Several alternatives or modifications to the described embodiments may be made without departing from the inventive concept and such alternatives or modifications should be considered as falling within the scope of the present invention.
Claims (10)
1. A PEM electrolyzed water anode catalyst, comprising: the catalyst is a nano oxide particle material, and the chemical formula of the oxide is AxRu1-xO2-δA is a transition metal Ta, wherein x is a mole fraction and 0 < x < 1, 0 < δ < 2.
2. The PEM electrolyzed water anode catalyst of claim 1, wherein: the size of the nano-oxide particles is 20-40 nm.
3. A method of making a PEM electrolyzed water anode catalyst as defined in claim 1 or 2, comprising the steps of:
(1) preparing a mixed solution containing soluble Ru salt and soluble transition metal salt according to a certain stoichiometric ratio;
(2) preparing a complex ligand dispersion liquid, and adjusting the pH value to 9-10; the complexing ligand is at least one of ethylene glycol bisaminoethyl ether tetraacetic acid, ethylene diamine tetraacetic acid, citric acid, lactic acid or polyacrylic acid;
(3) mixing the mixed solution obtained in the step (1) with a complexing ligand dispersion liquid, and evaporating and solidifying to obtain a metal chelate precursor;
(4) the precursor of the metal chelate is pyrolyzed and oxidized at 200-500 ℃ to obtain the modified nano ruthenium oxide particles.
4. The method for preparing a nano-oxide material according to claim 3, characterized in that: the soluble Ru salt is RuCl3、Ru(acac)3、Ru(CH3COO)3At least one of (1).
5. The method of making a PEM electrolyzed water anode catalyst of claim 3 or 4, wherein: the soluble transition metal salt is chloride, nitrate, organic acid salt or alkoxide.
6. The method of making a PEM electrolyzed water anode catalyst of claim 3, wherein: the solvent in step 1 is water, methanol, ethanol, acetone or isopropanol.
7. The method of making a PEM electrolyzed water anode catalyst of claim 3, wherein: the molar ratio of the complexing ligand to the metal in the metal salt is 0.01-100.
8. The method of making a PEM electrolyzed water anode catalyst of claim 3, wherein: step 2, adjusting the pH value by using an alkaline substance; the alkaline substance is ammonia water or ethylenediamine.
9. The method of making a PEM electrolyzed water anode catalyst of claim 3, wherein: the evaporation and solidification method comprises heating, stirring and evaporation, vacuum heating and evaporation or freeze drying.
10. The method of making a PEM electrolyzed water anode catalyst of claim 3, wherein: the metal chelate precursor is pyrolyzed and oxidized at the temperature of 200-300 ℃ to obtain the modified nano ruthenium oxide particles.
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| CN114921808B (en) * | 2022-03-22 | 2023-07-04 | 温州大学 | Vanadium-doped iridium dioxide electrocatalyst, and preparation method and application thereof |
| CN115094434B (en) * | 2022-06-07 | 2023-12-05 | 清氢(北京)科技有限公司 | Iridium oxide electrocatalyst batch preparation method and application of iridium oxide electrocatalyst in hydrogen production by water electrolysis |
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