CN115198285A - Preparation method of noble metal powder catalyst for hydrogen production by water electrolysis - Google Patents
Preparation method of noble metal powder catalyst for hydrogen production by water electrolysis Download PDFInfo
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- CN115198285A CN115198285A CN202210830686.1A CN202210830686A CN115198285A CN 115198285 A CN115198285 A CN 115198285A CN 202210830686 A CN202210830686 A CN 202210830686A CN 115198285 A CN115198285 A CN 115198285A
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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
- C25B11/093—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 at least one noble metal or noble metal oxide and at least one non-noble metal oxide
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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
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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 a preparation method of a noble metal powder catalyst for hydrogen production by water electrolysis, which comprises the following steps: s1, preparing a carrier: preparing anatase TiO2 nanowires; s2, preparing active liquid: dissolving TiO2 nanowires in an organic solvent, adding an iridium source into the organic solvent, and stirring at normal temperature to form an active solution; s3, drying the active liquid by distillation: heating and stirring the prepared active liquid containing the noble metal in the step S2 until the solution is evaporated to dryness; s4, sintering: and (4) drying and grinding the powder in the active liquid obtained after the S3 is evaporated to dryness, and then placing the powder in a crucible for sintering to obtain the noble metal powder catalyst. The preparation method provided by the invention is that IrO is 2 TiO supported on large specific surface area 2 On the nanowire, improve IrO 2 The catalytic activity of the catalyst is improved. In addition, because the nanowire contains a two-dimensional defect structure, the energy barrier required by catalysis is reduced through the defect structure,further promotion of IrO 2 Intrinsic catalytic activity of (3).
Description
Technical Field
The invention belongs to the technical field of hydrogen production by water electrolysis, and particularly relates to a preparation method of a noble metal powder catalyst for hydrogen production by water electrolysis.
Background
The hydrogen production by electrolyzing water by renewable energy sources presents a rapid development situation internationally, and many countries have set industrial development targets of hydrogen energy outside the traffic field, such as industry, building, electric power and the like, and have positive expression in aspects of government planning, application demonstration and the like.
In the technical aspect, the water electrolysis hydrogen production is mainly divided into AWE, solid polymer PEM water electrolysis, solid polymer Anion Exchange Membrane (AEM) water electrolysis and Solid Oxide (SOE) water electrolysis. From the technical point of view, the PEM water electrolysis technology has the advantages of high current density, small volume of an electrolysis bath, flexible operation, contribution to quick load change and good matching with wind power and photovoltaic power (the fluctuation and randomness of power generation are high). Because the anode of the PEM electrolyzer is in a strong acid environment (pH is approximately equal to 2) and the electrolytic voltage is 1.4-2.0V, most non-noble metals can corrode and possibly combine with sulfonate ions in the PEM, thereby reducing the proton conduction capability of the PEM. The electric catalyst research of PEM electrolyzer is mainly noble metal/oxide of Ir, ru, etc. and binary and ternary alloy/mixed oxide thereof, and supported catalyst with titanium material as carrier. The PEM water electrolysis hydrogen production is in the early stage of commercialization, and the bottleneck restricting the large-scale development of the technology is that the selection of the membrane electrode is monopolized by a few manufacturers, and the anode and cathode catalytic materials need to adopt noble metals, so that the cost is high. Therefore, increasing the activity of noble metal catalysts and reducing the catalyst loading are at a premium.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a precious metal powder catalyst for hydrogen production by water electrolysis, so as to improve the catalytic activity of the catalyst for hydrogen production by water electrolysis.
The technical scheme adopted by the invention for solving the technical problem is as follows: a preparation method of a noble metal powder catalyst for hydrogen production by water electrolysis specifically comprises the following steps:
s1, preparing a carrier: preparation of anatase TiO 2 A nanowire;
s2, preparing active liquid: adding TiO into the mixture 2 Dissolving the nanowires in an organic solvent, adding an iridium source into the organic solvent, and stirring the mixture at normal temperature to form an active solution;
s3, evaporating active liquid: heating and stirring the prepared active liquid containing the noble metal in the step S2 until the solution is evaporated to dryness;
s4, sintering: and (4) drying and grinding the powder in the active liquid obtained after the S3 is evaporated to dryness, and then placing the powder in a crucible for sintering to obtain the noble metal powder catalyst.
Further, the step S1 of preparing the carrier specifically includes:
s1.1, preparing a precursor solution: putting titanium dioxide P25 into NaOH solution with the concentration of 6-10 mol/L, and stirring at normal temperature to obtain mixed solution;
s1.2 hydrothermal reaction: transferring the mixed solution obtained in the step S1.1 into a reaction kettle with a polytetrafluoroethylene lining stainless steel, and placing the reaction kettle in a drying box at the temperature of between 130 and 150 ℃ for reacting for 18 to 36 hours;
s1.3, washing: soaking the white solid in 0.1-0.3 mol/L dilute hydrochloric acid for 12-24 h, washing the white solid by using ultrasonic centrifugal acid until the pH value is about 1, washing the white solid by using deionized ultrasonic centrifugal water until the white solid is neutral, and drying the white solid in a drying oven at 120-140 ℃.
Further, in the step S1.1, the concentration of the titanium dioxide P25 in the mixed solution is in the range of 1 to 5g/L.
Further, tiO in the step S2 2 The nano-wires are obtained by selecting one of titanium dioxide nano-powders with different particle sizes and performing hydrothermal reaction decomposition.
Further, in the active solution of the step S2, the TiO is 2 The concentration range of the nano wire is 1-5 g/L.
Further, the iridium source in step S2 is any one of chloroiridic acid, iridium trichloride and bromoiridic acid.
Further, the organic solvent in step S2 is any one of n-butanol, isopropanol, ethanol, or a mixture thereof.
Further, the step S4 of sintering specifically includes:
s4.1, drying and grinding the powder in the evaporated active solution;
s4.2, sintering the powder treated in the step S4.1 in a muffle furnace at 400-500 ℃ for 1-3 h, taking out, and cooling to room temperature.
The invention has the beneficial effects that: compared with the prior art, the preparation method of the noble metal powder catalyst for hydrogen production by water electrolysis, provided by the invention, comprises the steps of firstly, dissolving and crystallizing granular P25 in hydrothermal reaction at high temperature and high pressure in an alkali environment with a certain concentration to obtain layered titanate; due to the lack of hydrogen atoms and the influence of mechanical stress, the layered titanate curls to form needle-shaped tubes of different sizes during the formation of the flaky titanate. The washing leads to the change of reaction environment, the acicular tube body is stripped, and the stripped titanate sheet layer is curled to form a small-sized nanotube in order to reduce free energy and electrostatic repulsion. Na in titanate during acid washing + And H + Exchange is carried out, and Ti-O-Na bonds are replaced by Ti-OH bonds to generate titanic acid. During the calcination process, the tubular titanic acid is dehydrated to form tubular titanium oxide and undergoes crystal form transformation at a certain temperature to form anatase. The concentration of the base plays an important role mainly in the dissolution of nanoparticles and the formation of layered sodium titanate crimps. By adding to TiO 2 Adding iridium source into organic solution of nano wire, and finally adding IrO 2 In the form of a supported TiO compound having a large specific surface area 2 On the nanowires. The titanium dioxide nano-wires with different shapes can affect IrO 2 The active site distribution, and the high specific surface area is beneficial to increasing the active area. In addition, the nanowire has a two-dimensional defect structure, so that the energy barrier required by catalysis is reduced through the defect structure, and the IrO is further improved 2 Intrinsic catalytic activity of (3).
Drawings
FIG. 1 is a process for preparing TiO according to the present invention 2 Schematic flow diagram of nanowires.
FIG. 2 is a graph comparing the electrocatalytic properties obtained by the preparation methods provided in example 1 and comparative example 4.
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
In the embodiment, the preparation method of the noble metal powder for hydrogen production by water electrolysis specifically includes:
s1, preparing a carrier: preparation of anatase TiO 2 A nanowire;
s1.1, preparing a precursor solution: 5g of P25 was placed in 100ml of 6mol/L NaOH solution and stirred at room temperature for 2h.
S1.2, hydrothermal reaction: and transferring the uniformly mixed solution into a reaction kettle with a polytetrafluoroethylene lining stainless steel, and placing the reaction kettle in a drying box at the temperature of 140 ℃ for reaction for 24 hours.
S1.3, washing: soaking the white solid in 0.1mol/L diluted hydrochloric acid for 16h, washing with ultrasonic centrifugation for three times until the pH value is about 1, washing with deionized ultrasonic centrifugation water for five times until the solution is neutral, and drying the powder in a drying oven at 130 ℃.
S2, preparing active liquid: 2.5g of TiO 2 Dissolving the nanowires in 50ml of organic solvent, adding an iridium source into the organic solvent, and stirring the mixture at normal temperature to form a base solution;
s3, drying the active liquid by distillation: heating and stirring the prepared active liquid containing the noble metal at the heating temperature of 100 ℃ until the solution is evaporated to dryness;
s4, sintering: and drying and grinding the powder in the active liquid after drying to dryness, and then placing the active liquid in a crucible to roast for 2 hours at 450 ℃.
Example 2
The embodiment of the invention utilizes the preparation method of the noble metal powder for hydrogen production by water electrolysis, and the preparation method specifically comprises the following steps:
s1, preparing a carrier: preparation of anatase TiO 2 A nanowire;
s1.1, preparing a precursor solution: 5g of P25 was placed in 100ml of 8mol/L NaOH solution and stirred at room temperature for 2 hours.
S1.2, hydrothermal reaction: and transferring the uniformly mixed solution into a reaction kettle with a polytetrafluoroethylene lining stainless steel, and placing the reaction kettle in a drying box at the temperature of 140 ℃ for reaction for 24 hours.
S1.3, washing: soaking the white solid in 0.1mol/L dilute hydrochloric acid for 16h, washing with ultrasonic centrifugation for three times until the pH value is about 1, washing with deionized ultrasonic centrifugation water for five times until the solution is neutral, and drying the powder in a drying oven at 130 ℃.
S2, preparing active liquid: 2.5g of TiO 2 Dissolving the nanowires in 50ml of organic solvent, adding an iridium source into the organic solvent, and stirring the mixture at normal temperature to form a base solution;
s3, evaporating active liquid: heating and stirring the prepared active liquid containing the noble metal at the heating temperature of 100 ℃ until the solution is evaporated to dryness;
s4, sintering: and drying and grinding the powder in the active liquid after drying to dryness, and then placing the active liquid in a crucible to roast for 2 hours at 450 ℃.
Example 3
The embodiment of the invention utilizes the preparation method of the noble metal powder for hydrogen production by water electrolysis, and the preparation method specifically comprises the following steps:
s1, preparing a carrier: preparation of anatase TiO 2 A nanowire;
s1.1, preparing a precursor solution: 5g of P25 was placed in 100ml of a 10mol/L NaOH solution and stirred at room temperature for 2 hours.
S1.2, hydrothermal reaction: and transferring the uniformly mixed solution into a reaction kettle with a polytetrafluoroethylene lining stainless steel, and placing the reaction kettle in a drying box at the temperature of 140 ℃ for reaction for 24 hours.
S1.3, washing: soaking the white solid in 0.1mol/L dilute hydrochloric acid for 16h, washing with ultrasonic centrifugation for three times until the pH value is about 1, washing with deionized ultrasonic centrifugation water for five times until the solution is neutral, and drying the powder in a drying oven at 130 ℃.
S2, preparing active liquid: 2.5g of TiO 2 Dissolving the nanowires in 50ml of organic solvent, adding an iridium source into the organic solvent, and stirring the mixture at normal temperature to form a base solution;
s3, drying the active liquid by distillation: heating and stirring the prepared active liquid containing the noble metal at the heating temperature of 100 ℃ until the solution is evaporated to dryness;
s4, sintering: and drying and grinding the powder in the active liquid after evaporation to dryness, and then placing the active liquid in a crucible to be roasted for 2 hours at 450 ℃.
Comparative example 4
The embodiment of the invention utilizes the preparation method of the noble metal powder for hydrogen production by water electrolysis, and the preparation method specifically comprises the following steps:
s1, preparing active liquid: dissolving an iridium source in 50ml of organic solvent, and stirring at normal temperature to form a base solution;
s2, evaporating active liquid: heating and stirring the prepared active liquid containing the noble metal at the heating temperature of 100 ℃ until the solution is evaporated to dryness;
s3, sintering: and drying and grinding the powder in the active liquid after evaporation to dryness, and then placing the active liquid in a crucible to be roasted for 2 hours at 450 ℃.
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 electrolyzed water hydrogen production powder prepared by the preparation methods provided by the embodiment 1 and the comparative example 4 is used as a working electrode, and the electro-catalysis performance of the sample is tested in an electrochemical workstation under a three-electrode system. As can be seen from FIG. 2, irO 2 Powder Supported to TiO 2 The catalytic activity of the electrode can be effectively improved on the nano wire, and the overpotential of the OER reaction is reduced.
In conclusion, the IrO is prepared by the invention 2 TiO supported on large specific surface area 2 On the nanowire, improve IrO 2 The catalytic activity of the catalyst is improved. In addition, the nanowire has a two-dimensional defect structure, so that the energy barrier required by catalysis is reduced through the defect structure, and the IrO is further improved 2 Intrinsic catalytic activity of (3).
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 (8)
1. A preparation method of a noble metal powder catalyst for hydrogen production by water electrolysis is characterized by comprising the following steps:
s1, preparing a carrier: preparation of anatase TiO 2 A nanowire;
s2, preparing active liquid: adding TiO into the mixture 2 Dissolving the nano-wire in an organic solvent, adding an iridium source into the organic solvent, and stirring the mixture at normal temperature to form an active solution;
s3, evaporating active liquid: heating and stirring the prepared active liquid containing the noble metal in the step S2 until the solution is evaporated to dryness;
s4, sintering: and (4) drying and grinding the powder in the active liquid obtained after the S3 is evaporated to dryness, and then placing the powder in a crucible for sintering to obtain the noble metal powder catalyst.
2. The method for preparing the noble metal powder catalyst for hydrogen production by electrolysis of water according to claim 1, wherein the step S1 of preparing the carrier specifically comprises:
s1.1, preparing a precursor solution: putting titanium dioxide P25 into NaOH solution with the concentration of 6-10 mol/L, and stirring at normal temperature to obtain mixed solution;
s1.2 hydrothermal reaction: transferring the mixed solution obtained in the step S1.1 into a reaction kettle with polytetrafluoroethylene lining stainless steel, and placing the reaction kettle in a drying box at the temperature of 130-150 ℃ for reacting for 18-36 h;
s1.3, washing: soaking the white solid in 0.1-0.3 mol/L dilute hydrochloric acid for 12-24 h, washing the white solid by using ultrasonic centrifugal acid until the pH value is about 1, washing the white solid by using deionized ultrasonic centrifugal water until the white solid is neutral, and drying the white solid in a drying oven at 120-140 ℃.
3. The method according to claim 2, wherein in step S1.1, the concentration of titanium dioxide P25 in the mixed solution is in the range of 1 to 5g/L.
4. The method as claimed in claim 1 for producing hydrogen by electrolyzing waterThe preparation method of the noble metal powder catalyst is characterized by comprising the following steps: tiO in the step S2 2 The nano-wires are obtained by selecting one of titanium dioxide nano-powders with different particle sizes and performing hydrothermal reaction decomposition.
5. The method for preparing a noble metal powder catalyst for hydrogen production by electrolysis of water according to claim 1, wherein: in the active solution of the step S2, the TiO 2 The concentration range of the nano wire is 1-5 g/L.
6. The method for preparing a noble metal powder catalyst for hydrogen production by electrolysis of water according to claim 1, wherein: the iridium source in the step S2 is any one of chloro-iridic acid, iridium trichloride and bromoiridic acid.
7. The method for preparing a noble metal powder catalyst for hydrogen production by electrolysis of water according to claim 1, wherein: the organic solvent in the step S2 is any one or a mixture of n-butanol, isopropanol and ethanol.
8. The method for preparing the noble metal powder catalyst for hydrogen production by water electrolysis according to claim 1, wherein the sintering in step S4 specifically comprises:
s4.1, drying and grinding the powder in the evaporated active solution;
s4.2, sintering the powder treated in the step S4.1 in a muffle furnace at 400-500 ℃ for 1-3 h, taking out, and cooling to room temperature.
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| CN102302932A (en) * | 2011-06-22 | 2012-01-04 | 南京师范大学 | Anode Sn-Ru-Ir/TiO2 nano-particle catalyst for seawater electrolytic reaction and preparation method thereof |
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| CN114182307A (en) * | 2021-11-23 | 2022-03-15 | 西安泰金工业电化学技术有限公司 | Preparation method of noble metal anode for electrolytic copper foil |
| CN114561662A (en) * | 2022-03-21 | 2022-05-31 | 天津大学 | PEM (proton exchange membrane) electrolyzed water catalyst, and preparation method and application thereof |
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| CN102302932A (en) * | 2011-06-22 | 2012-01-04 | 南京师范大学 | Anode Sn-Ru-Ir/TiO2 nano-particle catalyst for seawater electrolytic reaction and preparation method thereof |
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