CN106450353A - Rare earth-iridium composite catalyst and preparation method thereof - Google Patents
Rare earth-iridium composite catalyst and preparation method thereof Download PDFInfo
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- CN106450353A CN106450353A CN201610813919.1A CN201610813919A CN106450353A CN 106450353 A CN106450353 A CN 106450353A CN 201610813919 A CN201610813919 A CN 201610813919A CN 106450353 A CN106450353 A CN 106450353A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9041—Metals or alloys
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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
- Y02E60/50—Fuel cells
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Abstract
The invention discloses preparation of rare earth-iridium composite catalyst of a non-platinum catalytic system built by rare earth and platinum, is mainly used in electrooxidation of alcohol in an acid medium, and belongs to the technical field of a fuel cell. A carbon-loaded rare earth oxide is firstly obtained by precipitation reaction and thermal treatment, and then the rare earth-iridium composite catalyst is obtained by reaction of the carbon-loaded rare earth oxide, a non-platinum precious metal precursor and a transition metal precursor. In the catalyst, element iridium is used as an active constituent, rare earth element is used as a catalytic-promotion constituent, transition metal element is used as an auxiliary constituent, the three constituents act with one another and are synergetic in activity, thus, the catalyst has relatively high activity and stability, is relatively rich in raw material source and low in cost, and an effective path is provided for designing the non-platinum catalytic system of the fuel cell.
Description
Technical field
The present invention relates to a kind of non-platinum System Catalyst, more particularly to a kind of rare earth-iridium for being built by rare earth, iridium is compound urges
The preparation of agent, is mainly used in, in acid medium in ethanol electrooxidation reaction, belonging to field of fuel cell technology.
Background technology
Direct Ethanol Fuel Cell due to the naturally occurring property of ethanol, nontoxic, energy density high the advantages of, start to cause
The research interest of people, and be with a wide range of applications.The at present directly anode catalyst used by alcohol fuel with Pt and
Based on its alloy catalyst, but this kind of catalyst faces resource scarcity, expensive, the problems such as easily being poisoned by intermediate product, from
And limit to its development and application.Therefore, finding a kind of non-platinum catalysis system has become the task of top priority of fuel cell.
In alkaline medium, the activity of palladium-based catalyst is higher, good stability, it is considered to be a kind of very promising platinum
Replace material.However, in acid medium, developing high performance non-platinum system and still suffering from very big challenge.There is document report
Road, iridium price is less than platinum, good stability, and resisting CO poisoning ability is good, therefore can alternatively platinum catalyst extensive
Be applied in some electrocatalytic reactions.But, with regard to iridium as main active component, for anode of fuel cell oxidation of ethanol
The report of reaction is but very few.Additionally, rare earth element has abundant d orbital electron, rare earth oxide resists in acid medium
Corrosivity are good, can improve the dispersibility of noble metal, and produce strong synergism with noble metal, therefore, to your gold improved
The activity of category component has very big facilitation.Furthermore, there are some researches show, some relatively cheap metals are added in noble metal
Such as：Ferrum, copper, nickel, cobalt, stannum etc. can change the electronic structure of catalyst component metal and the structure of nano-particle as helper component
Composition, to improve the electro-chemical activity of noble metal and reduce the consumption of noble metal.
Content of the invention
The purpose of the present invention is for above-mentioned problems of the prior art, provides a kind of activity height, good stability, becomes
The preparation method of this low rare earth-iridium composite catalyst, is the non-platinum catalysis system of designing fuel cell there is provided effective
Approach.
（One）The preparation of rare earth-iridium composite catalyst
The preparation method of rare earth-iridium composite catalyst of the present invention, comprises the following steps that：
（1）Carbon carries the preparation of rare earth oxide：By rare earth metal salt with carbon carrier ultrasonic disperse in distilled water, dilute ammonia is added
Water adjusts pH to 9～11, stirs 0.5～3h, washes, and dries, and products therefrom processes 1～5h at 600～1100 DEG C, obtains carbon
Carry rare earth oxide.Wherein, rare earth metal salt be cerous nitrate, Lanthanum (III) nitrate, praseodymium nitrate, europium nitrate, at least one in rubidium nitrate；
Carrier is carbon dust, mesoporous carbon, carbosphere, Graphene, CNT or carbon nano-fiber；The amount of carbon carrier is rare earth metal salt matter
1～5 times of amount.
（2）The preparation of rare earth-iridium composite catalyst：By the presoma of metal iridium, transition metal precursor and dispersant
Ultrasonic disperse stirs 0.5～2h in ethylene glycol；Carbon is added to carry rare earth oxide after adjusting pH=7～10, anti-in 100～200 DEG C
2～8 h are answered, washing, dry, that is, obtain rare earth-iridium composite catalyst.Wherein, the presoma of metal iridium is IrCl3；Transition gold
Category presoma is stannic chloride, iron chloride, Nickel dichloride., cobaltous chloride, at least one of cobalt nitrate, and the presoma of metal iridium and transition are golden
The mol ratio of category presoma is 1:0.25～1:4；Carbon carries 1～5 times of forerunner's weight that the amount of rare earth oxide is metal iridium.
Dispersant be sodium citrate, sodium tartrate, sodium pyrophosphate, sodium hexameta phosphate, sodium tripolyphosphate, sodium alginate,
EDTA etc..The consumption of dispersant is metal iridium presoma mol ratio 1:1～1:4.
Ethylene glycol is both solvent in the reaction, and reducing agent, and its consumption should be excessive（Make metal iridium presoma,
It is fully dispersed that transition metal precursor and the carbon for adding afterwards carry rare earth oxide）.
Rare earth-iridium composite catalyst prepared by the present invention, with iridium as active component, rare earth element is co-catalysis group
Point, transition metal is iridium, rare earth element, transition metal phase helper component, through be combined in the catalyst for obtaining
Interaction, activity collaboration so as to higher activity and stability.
2nd, the sign of rare earth-iridium composite catalyst prepared by the present invention
Below by XPS, EDX and TEM test, the rare earth-iridium composite catalyst of above-mentioned preparation is characterized.
1. XPS is characterized
Rare earth-iridium composite catalyst that Fig. 1 is prepared for the present invention（Ir3Sn-CeO2/C）The full spectrogram of XPS.Can from Fig. 1
Going out, iridium, stannum, cerium, oxygen, carbon all successfully be detected, illustrates Ir can be obtained by the preparation method of the present invention3Sn-CeO2/ C is catalyzed
Agent.
2. EDX test
The rare earth that Fig. 2 is prepared for the present invention-iridium structure composite catalyst（Ir3Sn-CeO2/C）EDX test chart.Can from Fig. 2
Go out, in catalyst prepared by the present invention, there are iridium, stannum, cerium, oxygen, five kinds of elements of carbon, prove further to be successfully prepared rare earth-iridium
Composite catalyst.
3. TEM test
Rare earth-iridium composite catalyst that Fig. 3 is prepared for the present invention（Ir3Sn-CeO2/C）TEM test chart.Can from Fig. 3 a
Go out, catalyst prepared by the present invention presents the typical face-centered cubic polycrystalline structure of iridium.From Fig. 3 b it is observed that, nano-particle
Can be evenly dispersed on carbon carrier.Corresponding 0.23 nm of spacing of lattice and 0.31 nm of Fig. 3 b is respectively iridium tin alloy
（111）Crystal face and ceria（111）Crystal face.
3rd, rare earth-performance of the iridium structure composite catalyst in ethanol electrooxidation
Below rare earth-iridium composite catalyst prepared by the present invention is examined to the activity of ethanol electrocatalytic oxidation and stability
Examine.
Fig. 4 prepares rare earth-iridium composite catalyst Ir for the present invention3Sn-CeO2/ C, carbon supported noble metal catalyst Pt/C and Ir/
C is in 0.5 M H2SO4+ 0.5 M C2H5Cyclic voltammogram in OH solution.From figure 5 it can be seen that catalyst of the present invention
（Ir3Sn-CeO2/C）There are more negative spike potential and bigger electric current density, its peak point current is about noble metal catalyst（Pt/C and
Ir/C）4.53 and 2.20 times, illustrate that the catalyst shows excellent electrochemistry in ethanol electrocatalysis oxidation reaction and lives
Property.
The catalyst that Fig. 5 is prepared for the present invention is in 0.5 M H2SO4+ 0.5 M C2H5Chrono-amperometric in OH solution is surveyed
Examination curve.Through the test of 3000 s, rare earth-iridium composite catalyst Ir3Sn-CeO2/ C is always maintained at higher electric current density.
Fig. 6 is rare earth-iridium composite catalyst Ir3Sn-CeO2/ C, carbon supported noble metal catalyst Pt/C and Ir/C difference 3000
Electric current density block diagram during s.From fig. 6 it can be seen that in 3000 s, the catalyst Ir of the present invention3Sn-CeO2/ C is still
The electric current density of maximum is maintained, illustrates that it has preferable stability and durability.
In sum, rare earth-iridium structure that prepared by the present invention is combined non-platinum System Catalyst activity height, good stability, is combustion
Material battery platinum based catalyst substitution studies provide effective approach.
Description of the drawings
Rare earth-iridium composite catalyst that Fig. 1 is prepared for the present invention（Ir3Sn-CeO2/C）The full spectrogram of XPS.
Rare earth-iridium composite catalyst that Fig. 2 is prepared for the present invention（Ir3Sn-CeO2/C）EDX test chart.
Rare earth-iridium composite catalyst that Fig. 3 is prepared for the present invention（Ir3Sn-CeO2/C）TEM test chart.
The rare earth that Fig. 4 is prepared for the present invention-iridium composite catalyst Ir3Sn-CeO2/ C, carbon supported noble metal catalyst Pt/C and
Ir/C is in 0.5 M H2SO4+ 0.5 M C2H5Cyclic voltammogram in OH solution.
Fig. 5 is rare earth-iridium composite catalyst Ir3Sn-CeO2/ C, carbon supported noble metal catalyst Pt/C and tri- kinds of catalysis of Ir/C
Agent is in 0.5 M H2SO4+ 0.5 M C2H5Chrono-amperometric test curve in OH solution.
Fig. 6 is rare earth-iridium composite catalyst Ir3Sn-CeO2/ C, carbon supported noble metal catalyst Pt/C and Ir/C are in 3000 s
When electric current density block diagram.
Specific embodiment
Below by specific embodiment, the preparation of non-platinum System Catalyst is combined to rare earth-iridium of the present invention and performance is made into one
Step explanation.
Embodiment 1, catalyst Ir3Sn-CeO2The preparation of/C
CeO2The preparation of/C：By 500.00 mg carbon dusts and 387.30 mg Ce (NO3)3·6H2O is dissolved into 30 mL distilled water
In, 30 mL weak ammonia are added dropwise over, until pH=10 or so, stirs 3 hours, sucking filtration, washing, drying, gained sample is 800
Heat treatment 4 hours at DEG C（Heating rate is 5 DEG C/min）, obtain CeO2/C.
Ir3Sn-CeO2The preparation of/C：By 1.7 mL IrCl3With 5.61 mg SnCl4·5H2O is added in round-bottomed flask,
30 mL ethylene glycol are added as reducing agent, after ultrasonic disperse, continue stirring 0.5 hour；Then add in mixed solution
35.29 mg sodium citrates, stirring adjusts pH value of solution=8 or so with 5% KOH/ ethylene glycol solution after making its dissolving；Add 100
mg CeO2/ C, is further continued for after ultrasonic disperse stirring 0.5 hour；Finally in N2Protection, at 180 DEG C react 4 hours, sucking filtration, washing,
Dry, obtain final product rare earth-iridium composite catalyst（Ir3Sn-CeO2/C）.
Rare earth-iridium composite catalyst is compared to the platinum carbon catalyst of business（Pt/C）, its peak current density is Pt/C catalysis
4.53 times of agent.
Embodiment 2, catalyst IrFe2-Sm2O3The preparation of/G
Sm2O3The preparation of/G：Using the sedimentation method, first by 300.00 mg Graphenes and 369.50 mg Sm (NO3)3·6H2O is molten
Solution is in 30 mL distilled water, then is added dropwise over 30 mL weak ammonia, until pH=10 or so, stirs 3 hours so as to which mixing is equal
Even, sucking filtration, washing, drying, gained sample heat treatment 2 hours at 800 DEG C（Heating rate is 5 DEG C/min）, obtain
Sm2O3/G.
IrFe2-Sm2O3The preparation of/G：By 1.5 mL IrCl3With 14.10 mg FeCl3·6H2O is added to round-bottomed flask
In, 30 mL ethylene glycol being added as reducing agent, continues stirring 0.5 hour after ultrasonic disperse；Then add in mixed solution
60.37 mg sodium hexameta phosphate, stirring adjusts pH value of solution=9 or so with 5% KOH/ ethylene glycol solution after making its dissolving, adds 200 mg
Sm2O3/ G, is further continued for after ultrasonic disperse stirring 0.5 hour；Finally in N2Protection, at 160 DEG C react 6 hours, sucking filtration, washing, do
Dry, obtain final product rare earth-iridium composite catalyst（IrFe2-Sm2O3/G）.
Rare earth-iridium composite catalyst is compared to the platinum carbon catalyst of business（Pt/C）, its peak current density is Pt/C catalysis
1.41 times of agent.
Embodiment 3, catalyst Ir3Ni-Eu2O3The preparation of/CNT
Eu2O3The preparation of/CNT：By 500.00 mg CNTs and 366.92 mg Eu (NO3)3·6H2O is dissolved into 30 mL
In distilled water, then 30 mL weak ammonia are added dropwise over, until pH=10 or so, stirs 3 hours, sucking filtration, washing, drying, gained
Sample heat treatment 3 hours at 1000 DEG C（Heating rate is 5 DEG C/min）, obtain Eu2O3/CNT.
Ir3Ni-Eu2O3The preparation of/CNT：By 1.9 mL IrCl3With 4.42 mg NiCl2·6H2O is added to round-bottomed flask
In, 30 mL ethylene glycol being added as reducing agent, continues stirring 0.5 hour after ultrasonic disperse；Then add in mixed solution
35.29 mg sodium citrates, stirring adjusts pH value of solution=8 or so with 5% KOH/ ethylene glycol solution after making its dissolving, adds 100mg
Eu2O3/ CNT, continues stirring 0.5 hour after ultrasonic disperse；Finally in N2Protection, at 150 DEG C react 6 hours, sucking filtration, washing,
Dry, obtain final product rare earth-iridium composite catalyst（Ir3Ni-Eu2O3/CNT）.
Rare earth-iridium composite catalyst is compared to business platinum carbon catalyst（Pt/C）, its peak current density is Pt/C catalyst
2.10 times.
Embodiment 4, catalyst IrNi-LaCeOxThe preparation of/C
LaCeOxThe preparation of/C：By 500.00mg carbon dust, 194.05mg La (NO3)3·6H2O and 194.38mg Ce (NO3)3·
6H2O is dissolved in 30 mL distilled water, then is added dropwise over 30 mL weak ammonia, until pH=10 or so, stirs 3 hours, take out
Filter, washing, dry, gained sample heat treatment 3 hours at 900 DEG C（Heating rate is 5 DEG C/min）, obtain LaCeOx/C.
IrNi-LaCeOxThe preparation of/C：By 1.6 mL IrCl3With 10.53 mg NiCl2·6H2O is added to round-bottomed flask
In, 30 mL ethylene glycol being added as reducing agent, continues stirring 0.5 hour after ultrasonic disperse；Then add in mixed solution
40.24 mg sodium alginates, stirring adjusts pH value of solution=8 or so with 5% KOH/ ethylene glycol solution after making its dissolving；Add 100
mg LaCeOx/ C, is further continued for after ultrasonic disperse stirring 0.5 hour；Finally in N2Protection, reacts 3 hours at 180 DEG C, sucking filtration, water
Wash, dry, obtain final product rare earth-iridium composite catalyst（IrNi-LaCeOx/C）.
Rare earth-iridium composite catalyst is compared to business platinum carbon catalyst（Pt/C）, its peak current density is Pt/C catalyst
2.10 times.
Embodiment 5, catalyst LaCeOxThe preparation of/C
Using the sedimentation method, first by 500.00 mg carbon dusts and 389.68 mg La (NO3)3·6H2O is dissolved into 30 mL distilled water
In, then 30 mL weak ammonia are added dropwise over, until pH=10 or so, stirs 3 hours so as to mix homogeneously, sucking filtration, washing, do
Dry, gained sample heat treatment 2 hours at 1100 DEG C（Heating rate is 5 DEG C/min）Obtain La2O3/C.
LaCeOxThe preparation of/C：By 1.6 mL IrCl3With 12.87 mg Co (NO3)2·6H2O is added in round-bottomed flask,
30 mL ethylene glycol are added as reducing agent, continue stirring 0.5 hour after ultrasonic disperse, then add in mixed solution
35.29 mg sodium citrates, stirring adjusts pH value of solution=10 or so with 5% KOH/ ethylene glycol solution after making its dissolving, adds 50
mg La2O3/ C, is further continued for after ultrasonic disperse stirring 0.5 hour；Finally in N2Protection, reacts 4 hours at 180 DEG C, sucking filtration, water
Wash, dry, obtain final product rare earth-iridium composite catalyst LaCeOx/C.
Rare earth-iridium composite catalyst is compared to business platinum carbon catalyst（Pt/C）, its peak current density is Pt/C catalyst
1.56 times.
Claims (10)
1. the preparation method of rare earth-iridium composite catalyst, comprises the following steps that：
（1）Carbon carries the preparation of rare earth oxide：By rare earth metal salt with carbon carrier ultrasonic disperse in distilled water, dilute ammonia is added
Water adjusts pH to 9～11, stirs 0.5～3h, washes, and dries, and products therefrom processes 1～5h at 600～1100 DEG C, obtains carbon
Carry rare earth oxide；
（2）The preparation of rare earth-iridium composite catalyst：By the presoma of metal iridium, transition metal precursor and dispersant are ultrasonic
It is scattered in ethylene glycol, stirs 0.5～2h；Adding carbon to carry rare earth oxide after adjusting pH=7～10,2 is reacted in 100～200 DEG C
～8h, washing, dry, that is, obtain rare earth-iridium composite catalyst.
2. the preparation method of rare earth-iridium composite catalyst as claimed in claim 1, it is characterised in that：Step（1）In, rare earth gold
Category salt is cerous nitrate, Lanthanum (III) nitrate, praseodymium nitrate, europium nitrate, at least one in rubidium nitrate.
3. the preparation method of rare earth-iridium composite catalyst as claimed in claim 1, it is characterised in that：Step（1）In, carbon carrier
For carbon dust, mesoporous carbon, carbosphere, Graphene, CNT or carbon nano-fiber.
4. the preparation method of rare earth-iridium composite catalyst as claimed in claim 1, it is characterised in that：Step（1）In, carbon carrier
Amount be 1～5 times of rare earth metal salt quality.
5. the preparation method of rare earth-iridium composite catalyst as claimed in claim 1, it is characterised in that：Step（2）In, metal iridium
Presoma be IrCl3.
6. the preparation method of rare earth-iridium composite catalyst as claimed in claim 1, it is characterised in that：Step（2）In, transition gold
Category presoma is stannic chloride, iron chloride, Nickel dichloride., cobaltous chloride, at least one of cobalt nitrate.
7. the preparation method of rare earth-iridium composite catalyst as claimed in claim 1, it is characterised in that：Step（2）In, metal iridium
The mol ratio of presoma and transition metal precursor be 1:0.25～1:4.
8. the preparation method of rare earth-iridium composite catalyst as claimed in claim 1, it is characterised in that：Step（2）In, carbon carries dilute
The amount of native oxide is 1～5 times of forerunner's weight of metal iridium.
9. the preparation method of rare earth-iridium composite catalyst as claimed in claim 1, it is characterised in that：Step（2）In, dispersant
For sodium citrate, sodium tartrate, sodium pyrophosphate, sodium hexameta phosphate, sodium tripolyphosphate, sodium alginate or EDTA.
10. the preparation method of rare earth-iridium composite catalyst as claimed in claim 1, it is characterised in that：Step（2）In, dispersant
Consumption for metal iridium presoma mol ratio 1:1～1:4.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114583189A (en) * | 2022-03-08 | 2022-06-03 | 中南大学 | Preparation method of efficient precious metal-rare earth alloy methanol poisoning resistant oxygen reduction catalyst |
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| CN102593473A (en) * | 2012-02-14 | 2012-07-18 | 中国科学院长春应用化学研究所 | Fuel cell catalyst and preparation method thereof |
| CN104307535A (en) * | 2014-09-12 | 2015-01-28 | 西北师范大学 | Preparation method of amorphous nano-oxide-precious metal heterostructure catalyst |
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| CN101362094A (en) * | 2008-09-25 | 2009-02-11 | 同济大学 | No-Pt catalyst for fuel cell, preparation method and use thereof |
| CN102593473A (en) * | 2012-02-14 | 2012-07-18 | 中国科学院长春应用化学研究所 | Fuel cell catalyst and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114583189A (en) * | 2022-03-08 | 2022-06-03 | 中南大学 | Preparation method of efficient precious metal-rare earth alloy methanol poisoning resistant oxygen reduction catalyst |
| CN114583189B (en) * | 2022-03-08 | 2024-02-06 | 中南大学 | Preparation method of efficient noble metal-rare earth alloy methanol poisoning resistant oxygen reduction catalyst |
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