CN114990576A - IrO with load structure 2 Preparation method and application of catalyst - Google Patents
IrO with load structure 2 Preparation method and application of catalyst Download PDFInfo
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- CN114990576A CN114990576A CN202210655948.5A CN202210655948A CN114990576A CN 114990576 A CN114990576 A CN 114990576A CN 202210655948 A CN202210655948 A CN 202210655948A CN 114990576 A CN114990576 A CN 114990576A
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
Abstract
The invention discloses an IrO with a load structure 2 The preparation method of the catalyst comprises the following steps: 1) dispersion g-C 3 N 4 : preparation of g-C in organic solvent 3 N 4 A solution; 2) adding an iridium (Ir) precursor aqueous solution into the carbon nitride solution prepared in the step 1) to obtain a mixed solution; 3) adjusting the acidity of the mixed solution prepared in the step 2) to an alkaline area, and stirring and precipitating; 4) sintering the precipitate obtained in the step 3) in a muffle furnace to form IrO 2 /g‑C 3 N 4 A composite nanocatalyst. The invention provides an IrO with a load structure 2 The preparation method and the application of the catalyst improve the catalytic efficiency of the noble metal and obtain more stable catalytic performance; obtained IrO with load structure 2 The catalyst may be used as a catalyst for PEM water electrolysis.
Description
Technical Field
The invention relates to the technical field of water electrolysis catalysts, in particular to IrO with a load structure 2 A preparation method of the catalyst and application thereof.
Background
Recently, the demand for new energy and renewable energy has been rapidly increased, and related research has become a hot spot. With respect to new and renewable energy sources, such as solar, wind and tidal energy, research and development to utilize surplus electric energy to produce hydrogen in a water electrolysis stack, the produced hydrogen is stored and then supplied to a fuel cell and used when needed as an energy source, is increasingly being considered as a new form of energy storage.
Among various hydrogen production methods, water electrolysis techniques are mainly classified into alkaline water electrolysis solid oxide electrolysis and polymer electrolyte membrane water electrolysis. Among them, the polymer electrolyte membrane water electrolysis (hereinafter abbreviated as PEM water electrolysis) technique does not require the use of corrosive solution, so mixing of generated gases does not occur, and since water is the only circulating liquid, problems such as corrosion and the like are not caused, no environmental pollution is generated during the production process, and the generated hydrogen is called green hydrogen.
An important component in the electrolysis of PEM water is the Membrane Electrode Assembly (MEA), which is essential to develop Oxygen Evolution Reaction (OER) catalysts. In particular, in the water electrolysis reaction, the reduction of the electrolysis efficiency is affected by an excessively high oxygen overpotential, and many studies have been made on the catalyst participating in the overpotential reduction in the oxygen production reaction.
Iridium oxide (IrO) 2 ) And ruthenium oxide (RuO) 2 ) Are two representative OER catalysts, but these catalysts are equivalent to expensive noble metal catalysts. Particularly, ruthenium oxide shows excellent catalytic activity in an initial state, but is difficult to use for a long period of time due to its low stability. There is an increasing need for a technology for preparing a catalyst having a new structure so as to simultaneously exhibit excellent electrochemical activity and durability.
Disclosure of Invention
In view of the shortcomings of the prior art, the present invention is directed to an IrO having a load structure 2 The preparation method and the application of the catalyst improve the catalytic efficiency of the noble metal and obtain more stable catalytic performance; IrO as described above 2 The catalyst may be used as a catalyst for PEM water electrolysis.
The technical scheme adopted by the invention for solving the technical problem is as follows: IrO with load structure 2 A method for preparing a catalyst, the method comprising the steps of:
1) dispersion g-C 3 N 4 : preparation of g-C in organic solvent 3 N 4 A solution;
2) adding an iridium (Ir) precursor aqueous solution into the carbon nitride solution prepared in the step 1) to obtain a mixed solution;
3) adjusting the acidity of the mixed solution prepared in the step 2) to an alkaline region, and stirring and precipitating;
4) sintering the precipitate obtained in the step 3) in a muffle furnace to form IrO 2 /g-C 3 N 4 Composite nanoparticles.
Further, in the step 1), the organic solvent is any one of ethanol, ethylene glycol and dimethylformamide or a mixture thereof.
Further, in the step 2), the iridium precursor is selected from one or more of chloroiridic acid, iridium fluoride, iridium chloride, iridium bromide, iridium iodide, iridium acetate, iridium acetylacetonate, iridium nitrate and hydrates thereof.
Further, in the step 3), the acidity adjustment is specifically performed by adjusting the pH of the mixed solution to 9 to 11 to adjust the acidity to an alkaline region.
Further, in the step 3), after stirring and precipitating, the method also comprises a centrifugation and washing step of the precipitate and further drying; the drying step is carried out at 70-90 ℃.
Further, in the step 4), the sintering is specifically carried out for 1-3 h under 500-550 ℃ with aerobic sintering, the temperature rise rate is 5 ℃/min, and furnace cooling is carried out after sintering.
Further, in the step 4), the IrO 2 /g-C 3 N 4 In the composite nanoparticle, includeg-C 3 N 4 A carrier and a peptide located at said g-C 3 N 4 Iridium and/or iridium oxide nanoparticles on the surface of the support;
further, the size of the iridium and iridium oxide nanoparticles is 1nm to 3 nm.
Further, in the step 4), the IrO 2 /g-C 3 N 4 In the composite nanoparticles, the iridium and/or iridium oxide nanoparticles account for 10 wt% -40 wt% of the total weight of the composite nanoparticles.
IrO with load structure 2 Use of a catalyst, said IrO 2 The catalyst may be used in PEM water electrolysis.
The invention has the beneficial effects that: compared with the prior art, the IrO with the load structure provided by the invention 2 In the preparation method of the catalyst, lamellar g-C is introduced 3 N 4 As the iridium oxide carrier, on one hand, the electron conductivity of the catalyst is effectively improved, so that the conductivity of the oxide catalyst is improved; in addition, two-dimensional lamellar g-C in priming solution 3 N 4 The attachment area of the catalyst is greatly increased, so that the effective catalytic activity area is increased, and the catalytic activity of the electrode is improved.
Drawings
FIG. 1 shows g-C prepared by thermal decomposition according to the present invention 3 N 4 X-ray electron diffraction pattern of (a).
FIG. 2 is a scanning electron microscope photograph of the catalyst prepared in example 1 of the present invention.
FIG. 3 is a scanning electron microscope photograph of the catalyst prepared in comparative example 1 of the present invention.
Fig. 4 is a graph showing the electrocatalytic performance of electrocatalysts prepared using example 1 and comparative example 1.
Detailed Description
The invention is further illustrated by the following specific examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention.
Example 1
An IrO having a load structure provided in this embodiment 2 Method for preparing a catalyst, iridium and/or iridium oxide nanoparticles in g-C 3 N 4 For loading and forming a nanometer Ir crystal cluster, the preparation method specifically comprises the following steps:
s1, preparation g-C 3 N 4 Weighing a certain amount of urea, placing into a crucible, placing into a muffle furnace, heating to 600 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 2h, and cooling with the furnace to obtain the required g-C 3 N 4 ；
S2, preparation g-C 3 N 4 Dispersion liquid: accurately weighing 50mg g-C 3 N 4 Dissolving in 2.5ml of ethylene glycol and 2.5ml of DMF solution, stirring at normal temperature until the mixture is completely dissolved to form dispersion liquid, and storing for later use;
s3, preparing a mixed solution: accurately weighing a certain amount of chloroiridic acid, dissolving the chloroiridic acid in 5ml of aqueous solution, uniformly stirring the chloroiridic acid at room temperature to obtain iridium-containing aqueous solution, and uniformly dropwise adding the dispersion liquid into the iridium-containing aqueous solution to obtain mixed solution;
s4, adjusting pH: dropwise adding 0.1M KOH solution into the mixed solution, and stirring at 45 ℃ until the pH is adjusted to 9-11; continuing stirring until a precipitate is generated, collecting the precipitate, centrifuging, cleaning, and drying in an oven at 80 ℃;
s5, placing the dried powder into a crucible, placing the crucible into a muffle furnace for sintering, wherein the sintering temperature is 500-550 ℃, the temperature rising speed is 5 ℃/min, keeping the temperature for 2h, and then cooling the furnace to obtain IrO 2 /g-C 3 N 4 A nanocomposite catalyst.
Comparative example 1
The comparative example provides a preparation method of a composite nano catalyst, which comprises the following specific preparation steps:
s1, preparing a solution: accurately weighing a certain amount of chloroiridic acid, dissolving the chloroiridic acid in 5ml of aqueous solution, and uniformly stirring at room temperature to obtain a mixed solution;
s2, adjusting pH: dropwise adding 0.1M KOH solution into the mixed solution, and stirring at 45 ℃ until the pH is adjusted to 9-11; continuing stirring until a precipitate is generated, collecting the precipitate, centrifuging, cleaning, and drying in an oven at 80 ℃;
s3, mixing the obtained powderPlacing the mixture into a crucible, placing the crucible into a muffle furnace for sintering, wherein the sintering temperature is 500-550 ℃, the heating rate is 5 ℃/min, keeping the temperature for 2h, and then cooling the mixture along with the furnace to obtain IrO 2 A nano-catalyst.
And (3) performance testing:
h in the electrolyte is 0.5mol/L 2 SO 4 The Ag/AgCl electrode is used as a reference electrode, the Pt electrode is used as a counter electrode, the catalysts prepared by the preparation methods provided by the embodiment 1 and the comparative example 1 are respectively loaded on a glassy carbon electrode to be used as working electrodes, and the electrocatalytic performance of a sample is tested in an electrochemical workstation under a three-electrode system. As shown in FIG. 4, under the same iridium oxide condition, 20mA/cm was reached 2 The overvoltage required for current density is lower than for pure iridium oxide loading, indicating that g-C 3 N 4 The catalyst has the function of improving the catalytic performance as a carrier.
In summary, the present invention employs pyrogenically prepared g-C 3 N 4 An electrically conductive support for an iridium oxide catalyst. g-C 3 N 4 Has a graphite-like layered structure, good thermal stability and chemical stability, no toxicity, rich sources and simple preparation and molding process. The specific surface area of the catalyst can be effectively improved by adopting the two-dimensional layered structure as a carrier, so that IrO (iridium oxide) is optimized 2 The catalytic performance of (2).
The above embodiments are only for illustrating the invention and are not to be construed as limiting the invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention, therefore, all equivalent technical solutions also belong to the scope of the invention, and the scope of the invention is defined by the claims.
Claims (9)
1. IrO with load structure 2 The preparation method of the catalyst is characterized by comprising the following steps:
1) dispersion g-C 3 N 4: Preparation of g-C in organic solvent 3 N 4 A solution;
2) adding an iridium (Ir) precursor aqueous solution into the carbon nitride solution prepared in the step 1) to obtain a mixed solution;
3) adjusting the acidity of the mixed solution prepared in the step 2) to an alkaline region, and stirring and precipitating;
4) sintering the precipitate obtained in the step 3) in a muffle furnace to form IrO 2 /g-C 3 N 4 A composite nanocatalyst.
2. IrO with load structure according to claim 1 2 The preparation method of the catalyst is characterized by comprising the following steps: in the step 1), the organic solvent is any one of ethanol, ethylene glycol and dimethylformamide or a mixture thereof.
3. IrO with load structure according to claim 1 2 The preparation method of the catalyst is characterized by comprising the following steps: in the step 2), the iridium precursor is selected from one or more of chloroiridic acid, iridium fluoride, iridium chloride, iridium bromide, iridium iodide, iridium acetate, iridium acetylacetonate, iridium nitrate and hydrates thereof.
4. IrO with load structure according to claim 1 2 The preparation method of the catalyst is characterized by comprising the following steps: in the step 3), the acidity adjustment is specifically performed by adjusting the pH of the mixed solution to 9-11 to adjust the acidity to an alkaline region.
5. IrO with load structure according to claim 1 2 The preparation method of the catalyst is characterized by comprising the following steps: in the step 3), after stirring and precipitating, the method also comprises the steps of centrifuging and washing the precipitate and further drying; the drying step is carried out at 70-90 ℃.
6. IrO with load structure according to claim 1 2 The preparation method of the catalyst is characterized by comprising the following steps: in the step 4), the sintering is specifically carried out for 1-3 h under 500-550 ℃, the temperature rise speed is 5 ℃/min, and the sintered material is cooled along with the furnace.
7. IrO with load structure according to claim 1 2 The preparation method of the catalyst is characterized by comprising the following steps: in the step 4), the IrO 2 /g-C 3 N 4 In the composite nano catalyst, g-C is included 3 N 4 A carrier and a dispersant dispersed in said g-C 3 N 4 Iridium and/or iridium oxide nanoparticles on the surface of the support.
8. IrO with load structure according to claim 7 2 The preparation method of the catalyst is characterized by comprising the following steps: the size of the iridium and iridium oxide nano particles is 1 nm-3 nm.
9. IrO with load structure according to claim 7 2 The preparation method of the catalyst is characterized by comprising the following steps: in the step 4), the IrO 2 /g-C 3 N 4 In the composite nano-catalyst, the iridium and/or iridium oxide nano-particles account for 10 wt% -40 wt% of the total amount of the composite nano-particles.
IrO with load structure 2 The application of the catalyst is characterized in that: the IrO 2 The catalyst may be used in PEM water electrolysis.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104209121A (en) * | 2014-08-14 | 2014-12-17 | 中国科学院长春应用化学研究所 | IrO2 catalyst used for water electrolysis, and preparation method thereof |
| CN112981432A (en) * | 2021-02-05 | 2021-06-18 | 宁波中科科创新能源科技有限公司 | Anode catalyst for preparing ozone by electrolyzing pure water, membrane electrode and preparation method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104209121A (en) * | 2014-08-14 | 2014-12-17 | 中国科学院长春应用化学研究所 | IrO2 catalyst used for water electrolysis, and preparation method thereof |
| CN112981432A (en) * | 2021-02-05 | 2021-06-18 | 宁波中科科创新能源科技有限公司 | Anode catalyst for preparing ozone by electrolyzing pure water, membrane electrode and preparation method |
Non-Patent Citations (2)
| Title |
|---|
| SEN WANG ET AL.: "Defect engineering assisted support effect:IrO2/N defective g-C3N4 composite as highly efficient anode catalyst in PEM water electrolysis", 《CHEMICAL ENGINEERING JOURNAL》 * |
| 谢小缔等: "负载氧化铟纳米颗粒多壁碳纳米管的制备与表征", 《机械工程材料》 * |
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