CN102477564A - Method for preparing SPE (solid polymer electrolyte) anodic oxygen evolution catalysts for water electrolysis - Google Patents
Method for preparing SPE (solid polymer electrolyte) anodic oxygen evolution catalysts for water electrolysis Download PDFInfo
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- CN102477564A CN102477564A CN2010105546771A CN201010554677A CN102477564A CN 102477564 A CN102477564 A CN 102477564A CN 2010105546771 A CN2010105546771 A CN 2010105546771A CN 201010554677 A CN201010554677 A CN 201010554677A CN 102477564 A CN102477564 A CN 102477564A
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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
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- 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
Abstract
The invention relates to a method for preparing SPE (solid polymer electrolyte) anodic oxygen evolution catalysts for water electrolysis. The method mainly includes steps of dissolving precursors of metal salt, such as RuCl3, H2PtCl6, H2IrCl6 and the like, into ethanol/water solution, regulating the pH (potential of hydrogen) value of the solution by NaHCO3 ethanol/water, then ageing, separating, washing, roasting and the like, so that noble metal oxides with high oxygen evolution activity are prepared. Accordingly, the noble metal load amount is reduced, and cost of the SPE water electrolysis technology is lowered, and foundation for further commercialized application of the SPE water electrolysis technology is laid.
Description
Technical field
The present invention relates to solid polymer electrolyte (SPE) water electrolysis, specifically a kind of preparation technology of SPE water electrolysis anode oxygen-separating catalyst.
Background technology
In today that energy and environment receive much concern, low-carbon economy has become the favorite in epoch.National governments and business circles just are being devoted to how to tap a new source of energy, and how to utilize the energy efficiently, to satisfy the requirement of human kind sustainable development.Hydrogen Energy is described as the most ergastic energy carrier, and it has cleaning, advantages such as efficient, wide material sources.Brine electrolysis is as a kind of traditional hydrogen producing technology, and current about 4% of the hydrogen manufacturing total amount that but only accounts for is needed badly at aspects such as energy consumption, cost, stability, securities and improved.And SPE water electrolysis technology is efficient because of it, zero release, compact construction, environmental friendliness, and the product purity advantages of higher become the research focus of hydrogen preparation field in recent years, and the highly purified oxygen of its product also has been used for fields such as space flight, medical treatment, analysis.Yet cost an arm and a leg is the further major cause of commercial applications of restriction SPE water electrolysis technology, and therefore around how to reduce cost, improving electrolytic efficiency is various countries researchist's focus.
In the SPE water electrolytic cell, the membrane electrode of being made up of cathode and anode Catalytic Layer and cationic exchange membrane is the core component of electrolyzer, is the place that electrolytic reaction takes place.Wherein, because platinum has significant catalytic activity and stability to evolving hydrogen reaction, platinum is optimum catalyst [J.P.2,006 of evolving hydrogen reaction all the time; 104,502, J.P.2,006; 193,768, U.S.20,080; 230,380], and the anode oxygen evolution reaction is considered to the main source of electrolyzer overpotential.Therefore be necessary that the antianode catalyzer studies, to improve energy utilization ratio.And a large amount of cut-and-try work and theoretical investigationes show to have and analyse the oxygen catalytic activity preferably and can in acidic medium, mainly concentrate on IrO by the oxygen-separating catalyst of stable existence
2, RuO
2On metal oxide containing precious metals.Therefore, need to select suitable preparation technology, analyse the eelctro-catalyst of oxygen excellent performance, control the electrolysis cost effectively, increase its commercial applicability with preparation.
The preparation of membrane electrode Catalytic Layer can adopt methods such as dipping reduction, electrochemical reduction directly that catalyst deposit is surperficial to film, also can be prepared into the powder catalyzer earlier, adopts technology such as spraying, change platen press to be deposited on the film surface indirectly again.The former has been widely used in the preparation of many sizes stable state electrode, but its application at membrane electrode is restricted.In Japanese Patent [J.P.5,538,934], adopt chemical deposition, directly metal-salt is reduced to a side of film.Advantages such as this method has simple to operate, and catalyzer combines with film firmly, and the interface resistance value is little, but its shortcoming is outstanding too, and not high like catalyst utilization, the catalyzer that deposits in the film is prone to cause short circuit.
At present, indirect method prepares membrane electrode and is adopted by numerous scholars.Preparation to the powder oxygen-separating catalyst mainly contains Adams roasting method and sol-gel method two big classes; The Adams roasting method is the method that a kind of technology relatively simply prepares MOX; Propose in nineteen twenty-three by Adams and Shriner etc., use more widely but its harsh and bigger metal oxide particle to roasting condition has limited it.USP [U.S.4,289,519] adopts the Adams roasting method to prepare RuO
2The time, about 10% MgO
2Adding can significantly improve RuO
2Stability.In recent years, along with the broad development of nanotechnology, sol-gel method just like has the trend that replaces the Adams roasting method.In document (Y. Murakami, J. Mater. Chem., 13 (1994) 1773; K.Kameyama, J. Electrochem. Soc., 140 (1993) 1034; M. Ito, J. Electrochem. Soc., 141 (1994) 1234) in, adopt the oxide compound of ethylate hydrolysis method preparation or the colloidal sol of oxyhydroxide, after drying, thermal treatment, obtain RuO
2IrO
2, RuO
2-TiO
2, RuO
2-SnO
2Molecule Deng oxide compound.The preparation method who can be used for analysing the powder MOX of oxygen electrocatalysis also comprises pulverize at low temperature, high-energy ball milling method, hydrothermal method etc.
Summary of the invention
The object of the present invention is to provide a kind of preparation technology of SPE water electrolysis anode oxygen-separating catalyst,, reduce the electrolysis cost to improve electrolytic efficiency.Employing solvability ethanol/water preferably is a solvent, to promote the dissolving and the dispersion of precious metal salt, simultaneously, by the more weak NaHCO of alkalescence
3Regulate its pH value, to reach best crystallization effect.This technological process is simple, suitability is strong, and the MOX of this method preparation has advantages such as analysing oxygen electro catalytic activity, stability preferably.
For realizing above-mentioned purpose, the technical scheme that the present invention adopts is:
A kind of preparation method of SPE water electrolysis anode oxygen-separating catalyst; Adopt sol-gel method; With volume ratio is that the ethanol/water of 1～2:2～1 is a solvent, and the precursor of metal soluble salt is dissolved, and adopts modes such as magnetic agitation or ultra-sonic dispersion that it is fully dissolved; Adopt the more weak NaHCO of alkalescence
3Ethanol/water solution to regulate its pH value be 8-9, the nucleation rate when effectively controlling the colloid crystallization and the speed of grain growth, and NaHCO during roasting
3At high temperature decompose and to discharge CO
2, help the formation of vesicular structure, and can prevent the reunion of powder granule effectively; Filtration, washing, drying, roasting promptly obtain SPE water electrolysis anode and analyse the oxygen eelctro-catalyst;
The precursor of said metal soluble salt is the mixture of solubility precious metal salt or solubility precious metal salt and solubility base metal salt; Precious metal salt is a kind of or soluble salt more than two kinds among Ru, Ir, the Pt; Base metal salt is a kind of or soluble salt more than two kinds among Ta, Sn, Mn, Mo, the Ti.
Its concrete operations step is following:
The precursor that 1) will be used for preparing the metal soluble salt of SPE water electrolysis anode catalyst is dissolved in the ethanol/water solution that volume ratio is 1～2:2～1, is stirred well to evenly; Said metal-salt is generally RuCl
3, H
2IrCl
6, H
2PtCl
6Deng;
2) preparation NaHCO
3Volume ratio be the ethanol/water solution of 1～2:2～1, drop in the solution of step 1) of high-speed stirring, regulate its pH=8～9;
3) leave standstill 0.5～30h under the room temperature after, spinning, deionized water wash is for several times to there not being Cl
-Be detected 60～90 ℃ of vacuum-drying 4～12h;
4) with the pressed powder of step 3) preparation in air or oxygen atmosphere, calcination process 0.5～10h under 400～600 ℃ of conditions, naturally cooling grinds and promptly obtains SPE water electrolysis anode and analyse the oxygen eelctro-catalyst.
It is the powder MOX that the SPE water power of preparation is resolved the oxygen eelctro-catalyst, is monobasic metal oxide containing precious metals PtO
2, RuO
2Or IrO
2Or be binary or polynary precious metal complex metal oxides or binary or polynary precious metal and base metal complex metal oxides.
Monobasic metal oxide containing precious metals PtO
2, RuO
2Or IrO
2Binary or polynary precious metal and base metal complex metal oxides such as RuO2-IrO2, RuO
2-TaO
2, RuO
2-IrO
2-SnO
2
The said solvent that is used to dissolve precious metal salt and NaHCO3 is an ethanol/water, and volume ratio is 1～1.2:1.2～1.
The step 4) roasting is under oxygen or conditions of air, to carry out, and from room temperature temperature programming to 400～600 ℃, temperature rise rate is controlled to be 1～5 ℃/h, then in 400～600 ℃ of roasting 0.5～10h.
In the research of powder MOX, the most significant problems of existence is how effectively the pattern of control catalyst obtains its advantages of high catalytic activity and stability.Because the anode overpotential is to cause the main source of electrolyzer energy loss; This has good electro catalytic activity with regard to the catalyzer that requires to prepare, simultaneously oxygen wash away and the atmosphere of strongly-acid, hyperoxia voltinism requires the catalyzer of preparation need have excellent electrochemical stability.And the pattern of catalyst themselves (like particle size, specific surface area, porosity etc.) is with its catalytic activity of the left and right sides and stability.
The present invention considers the problems referred to above, and the concrete principle of oxygen-separating catalyst preparation technology of the present invention is set forth as follows:
Ethanol and water are the most widely used at present solvents; The ethanol/water that adopts the equal-volume ratio is as solvent; Be the organic properties of materials of the good dissolving of ethanol capable of using, the character of the dissolve inorganic salts that water also capable of using is good has reached the abundant dissolved purpose of metal-salt precursor.Only under alkaline condition, just can help colloidal and form simultaneously.Under weak basic condition, can effectively control the speed of colloidal nucleation and grain growth.Select for use this as weakly alkaline NaHCO
3Ethanol/water solution be easy to regulator solution pH to 8～9, supercarbonate CO when high temperature simultaneously
2Release, will help the formation of vesicular structure, hinder particulate effectively and reunite, thereby realize control the catalyzer pattern.
Beneficial effect of the present invention
1, the present invention can prepare the eelctro-catalyst of high oxygen separated catalytic activity.
2, technological process of the present invention is simple to operation, and each processing parameter is easy to control.Use technology provided by the invention, only need the pH value of regulator solution can reach satisfied effect.
3, the present invention is applicable to the preparation of most of transition metal oxides, and application prospect is good.
Description of drawings
The cyclic voltammetry curve of Fig. 1, oxygen-separating catalyst, sweep rate 50mVs
-1
The linear time base sweep curve of Fig. 2, oxygen-separating catalyst, sweep rate 2mVs
-1
The polarization curve of Fig. 3, electrolyzer, electrode area 5cm
2, probe temperature 60
oC.
Embodiment
Embodiment 1
Take by weighing 1g RuCl
3NH
2O (n=3～5) is dissolved in 50mL ethanol/water (equal-volume ratio, the down together) solution, stirs 30min, drips 0.38M NaHCO
3Ethanol/water solution, make pH=8, continue to stir 30min after, leave standstill 5h, outwell upper solution, centrifuging, deionized water wash repeats AgNO 3 times
3Solution does not have white emulsion when detecting or deposition generates.In 80 ℃ of vacuum-dryings the whole night, respectively 400 ℃ with 500 ℃ of following air in roasting 30min, naturally cooling makes SPE water electrolysis anode oxygen-separating catalyst RuO
2, the about 0.3g of output.
Embodiment 2
Take by weighing the H of 1g
2IrCl
6In (Ir content 37wt%) solution 50mL ethanol/water solution, other step makes SPE water electrolysis anode oxygen-separating catalyst IrO with embodiment 1
2, the about 0.3g of output.
Embodiment 3
Take by weighing each 5mg of anode catalyst of embodiment 1 and embodiment 2, be dissolved in the absolute ethyl alcohol of 1mL ultra-sonic dispersion 15min respectively; The Nafion solution of the 5wt% of Dropwise 50 μ L continues ultra-sonic dispersion 30min, gets 25 μ L and is coated on the glass carbon working electrode; And be reference electrode with the SCE; The platinized platinum electrode is a counter electrode, forms classical three-electrode system, at 0.5M H
2SO
4In the solution, under the logical nitrogen condition, the oxygen-separating catalyst that embodiment 1 and embodiment 2 are prepared carries out cyclic voltammetric test and linear time base sweep (Fig. 1 and Fig. 2).
Test result: Ru (III)/Ru (IV), Ru (IV)/Ru (VI) and the Ir (III) that characteristic redox peak is corresponding/Ir (IV) is electric to fairly obvious, RuO
2, IrO
2Have bigger electrostatic double layer charging current, and, show to have the good oxygen activity of analysing.Initial oxygen evolution potential RuO
2<irO
2, its oxygen summit current of analysing at 1.2V (vs SCE) has also reflected same trend, and RuO is described
2The oxygen activity of analysing be better than IrO
2
Embodiment 4
The metal oxide containing precious metals of embodiment 1 or the embodiment 2 preparations anode catalyst as the SPE water electrolytic cell is sprayed on Nafion 115 films, and the load amount is 2 mgcm
-2, negative electrode is Pt/C, Pt load amount is 0.4 mg cm
-2, the cathode and anode diffusion layer is selected the Torry carbon paper for use, at 140 ℃, under the 10atm, is pressed into membrane electrode, is assembled into electrolyzer, and it is carried out electrochemical property test (Fig. 3).
The electrolyzer evaluating is following: cell operation temperature 60
OC, atmospheric operation, zero(ppm) water flow 25mL min
-1, single pool area 5cm
2, adopt the D.C. regulated power supply power supply.
Test result: also reflected the experimental result that embodiment 3 obtains basically, but under high electric density, because RuO
2Poor stability is by anode catalyst IrO
2The electrolyzer polarization performance of assembling is better than RuO
2, at 1.8V be close 650 mAcm that reach of electricity
-2
Claims (6)
1. a method for preparing SPE water electrolysis anode oxygen-separating catalyst adopts sol-gel method, and it is characterized in that: the employing volume ratio is the precursor of the ethanol/water solution dissolution of metals soluble salt of 1～2:2～1, adopts NaHCO
3Ethanol/water solution to regulate its pH value be 8～9; It is dry that ageing, solid leach the thing washing, and roasting promptly obtains SPE water electrolysis anode and analyses the oxygen eelctro-catalyst;
The precursor of metal soluble salt is the mixture of solubility precious metal salt or solubility precious metal salt and solubility base metal salt;
Precious metal salt is a kind of or soluble salt more than two kinds among Ru, Ir, the Pt;
Base metal salt is a kind of or soluble salt more than two kinds among Ta, Sn, Mn, Mo, the Ti.
2. according to the described method of claim 1, it is characterized in that:
The concrete operations step is following:
The precursor that will be used for preparing the metal soluble salt of SPE water electrolysis anode catalyst is dissolved in the ethanol/water solution that volume ratio is 1～2:2～1, is stirred well to evenly;
Preparation NaHCO
3Volume ratio be the ethanol/water solution of 1～2:2～1, drop in the solution of step 1) of high-speed stirring, regulate its pH=8～9;
After leaving standstill 0.5～30h under the room temperature, spinning, deionized water wash is to there not being Cl
- Be detected 60～90 ℃ of vacuum-drying 4～12h;
With the pressed powder of step 3) preparation in air or oxygen atmosphere, calcination process 0.5～10h under 400～600 ℃ of conditions, naturally cooling grinds and promptly obtains SPE water electrolysis anode and analyse the oxygen eelctro-catalyst.
3. according to claim 1 or 2 described methods, it is characterized in that: it is the powder MOX that the SPE water power of preparation is resolved the oxygen eelctro-catalyst, is monobasic metal oxide containing precious metals PtO
2, RuO
2Or IrO
2Or be binary or polynary precious metal complex metal oxides or binary or polynary precious metal and base metal complex metal oxides.
4. according to the described method of claim 3, it is characterized in that: monobasic metal oxide containing precious metals PtO
2, RuO
2Or IrO
2Binary or polynary precious metal and base metal complex metal oxides RuO
2-IrO
2, RuO
2-TaO
2Or RuO
2-IrO
2-SnO
2
5. according to claim 1 or 2 described methods, it is characterized in that: the said solvent that is used to dissolve precious metal salt is an ethanol/water, and its volume ratio is 1～1.2:1.2～1.
6. according to the described method of claim 2, it is characterized in that: the step 4) roasting is under oxygen or conditions of air, to carry out, and from room temperature temperature programming to 400～600 ℃, temperature rise rate is controlled to be 1～5 ℃/h, then in 400～600 ℃ of roasting 0.5～10h.
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