CN116905027A - Supported nano iridium catalyst, preparation method and application - Google Patents
Supported nano iridium catalyst, preparation method and application Download PDFInfo
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- CN116905027A CN116905027A CN202310752619.7A CN202310752619A CN116905027A CN 116905027 A CN116905027 A CN 116905027A CN 202310752619 A CN202310752619 A CN 202310752619A CN 116905027 A CN116905027 A CN 116905027A
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- iridium
- antimony oxide
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- nano iridium
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- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910052741 iridium Inorganic materials 0.000 title claims abstract description 63
- 239000003054 catalyst Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XXLJGBGJDROPKW-UHFFFAOYSA-N antimony;oxotin Chemical compound [Sb].[Sn]=O XXLJGBGJDROPKW-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000002131 composite material Substances 0.000 claims abstract description 16
- 239000002105 nanoparticle Substances 0.000 claims abstract description 12
- 239000011148 porous material Substances 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000005868 electrolysis reaction Methods 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 abstract description 5
- 229910000457 iridium oxide Inorganic materials 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000007772 electrode material Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000012528 membrane Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 230000010287 polarization Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- LYCAIKOWRPUZTN-NMQOAUCRSA-N 1,2-dideuteriooxyethane Chemical compound [2H]OCCO[2H] LYCAIKOWRPUZTN-NMQOAUCRSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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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
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
- C25B11/081—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound the element being a noble metal
-
- 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
-
- 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
- C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
-
- 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
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
- C25B11/067—Inorganic compound e.g. ITO, silica or titania
-
- 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
- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
- C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
- C25B9/19—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The application discloses a supported nano iridium catalyst and a preparation method thereof, wherein the catalyst prepared by the application is of a tin antimony oxide supported nano iridium-based composite structure, and the mass content of iridium in the catalyst is 9-40%; the specific surface area of tin antimony oxide is not less than 95m 2 /g; according to the method, the tin antimony oxide is directly used as the basal pore mesoporous nano iridium to prepare the tin antimony oxide/iridium composite nano particles, so that the method is simple and controllable, and the problem that harmful gas is generated in the existing catalyst preparation process is solved; solves the problem of large iridium or iridium oxide consumption in the existing catalyst preparation process, and greatly reduces the production costThe electrode material is suitable for large-scale industrial production and is popularized to more novel electrode materials.
Description
Technical Field
The application relates to the technical field of electrolyzed water catalysis, in particular to a metal oxide supported nano iridium catalyst, a preparation method and application thereof.
Background
With the increasing demand for renewable energy sources in recent years, hydrogen energy has received increasing attention as a green renewable energy source. PEM (proton exchange membrane) technology for producing hydrogen by electrolysis of water can efficiently convert electric energy into hydrogen energy for storage. While MEA (membrane electrode) acts as a key component of the cell, its performance determines the electrolysis efficiency. The catalytic efficiency of OER (oxygen evolution reaction) catalysts directly affects OER reaction rate and determines MEA performance, and therefore, high performance OER catalysts are critical for PEM water electrolysis hydrogen production. The OER catalysts on the market at present are mainly nano iridium oxide and iridium black, but the preparation process is relatively complex and the cost is high, so that the OER catalyst with simple process and low cost needs to be designed and prepared.
Disclosure of Invention
The first aim of the application is to provide a supported nano iridium catalyst which has higher catalytic activity and chemical stability and can be applied to the technical field of electrolytic water catalysis.
In order to achieve the first object, the present application provides the following technical solutions:
a supported nano iridium catalyst is of a tin antimony oxide supported nano iridium-based composite structure; wherein the mass content of iridium in the catalyst is 9-40%; the specific surface area of the tin antimony oxide is not less than 95m 2 /g。
Optionally, the specific surface area of the tin antimony oxide is 95-200 m 2 /g, preferably 95m 2 /g。
Optionally, the supported nano iridium catalyst has a porous structure, and the average pore diameter is 2 nm-8 nm.
Optionally, the particle size of the nano iridium is 2-4nm, and the particle size range of the tin antimony oxide is 20-40nm.
The second purpose of the application is to provide a preparation method of the supported nano iridium catalyst, which has simple process and low cost.
In order to achieve the second object, the method specifically comprises the following steps:
s1: carrying out ultrasonic dispersion on 60-90 parts by weight of tin antimony oxide particles in an organic solvent for 5-10 min;
s2: adding 10-40 parts by mass of nano iridium particles into the dispersion liquid obtained in the step S1, continuing to ultrasonically disperse for 20-30 min, and fully stirring to obtain a mixed solution of tin antimony oxide/iridium composite nano particles;
s3: centrifuging the mixed solution obtained in the step S2 for 3-5 times, and performing ultrasonic cleaning to obtain black solid particles;
s4: and (3) fully drying the black solid particles obtained in the step (S3) for 6-8 hours to obtain the tin antimony oxide/iridium composite nano particles.
Optionally, in S1, the organic solvent used is ethanol, ethylene glycol or a mixture of ethanol and ethylene glycol.
Optionally, in S2, the stirring period is 48-72 hours.
Optionally, in S3, the centrifugation speed of the mixed solution is 10000-12000 rpm, and optionally, the centrifugation speed is 10000rpm.
Alternatively, in S4, the drying temperature of the black solid particles is 50 to 70 ℃.
Compared with the prior art, the application has the following beneficial effects:
1. the method directly utilizes the tin antimony oxide as the basal pore mesoporous nano iridium to prepare the tin antimony oxide/iridium composite nano particles, is simple and controllable, and solves the problem of harmful gas generated by the existing catalyst preparation process.
2. The preparation process solves the problem of large iridium or iridium oxide consumption of the existing catalyst preparation process, greatly reduces the production cost, is suitable for large-scale industrial production, and is popularized to more novel electrode materials.
3. The application utilizes the composite structure of tin antimony oxide and iridium, can improve the electrocatalytic active surface area in the electrolysis process, so that the catalyst shows extremely high electrocatalytic hydrogen production activity in practical application, ensures the hydrogen evolution efficiency of electrocatalytic decomposed water under extremely low use level of metallic iridium, and fully plays the effective catalytic capability of nano iridium.
Drawings
FIG. 1 is a comparison of polarization curves for examples of the present application and comparative examples;
FIG. 2 is a standard test membrane electrode sprayed with a catalyst sample;
FIG. 3 is a comparison of polarization curves for different BET embodiments.
Detailed Description
The following description of the embodiments of the present application will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Example 1
The preparation method of the supported nano iridium catalyst comprises the following steps:
s1: 1g of tin antimony oxide particles (BET 95m in 35ml of ethylene glycol 2 Carrying out ultrasonic dispersion for 10min;
s2: adding 0.1g of nano iridium particles into the dispersion liquid obtained in the step S1, continuing ultrasonic dispersion for 20min, and fully stirring at 500rpm at room temperature of 25 ℃ for 48h to ensure that nano iridium particles are carried on the tin antimony oxide, so as to obtain a mixed solution of the tin antimony oxide/iridium composite nano particles;
s3: centrifuging the mixed solution obtained in the step S2 at 10000rpm, and repeating the steps for 3 times by using isopropanol to carry out ultrasonic treatment for 5min to obtain black solid particles;
s4: and (3) fully drying the black solid particles obtained in the step (S3) for 6 hours at the temperature of 70 ℃ under the vacuum condition to obtain the tin antimony oxide/iridium composite nano particles.
In the present example, the specific surface area of the tin antimony oxide was 95m 2 /g; the grain diameter of the nano iridium is 2-4nm; the grain diameter of the tin antimony oxide is 20-40nm.
Example 2
The preparation method of the supported nano iridium catalyst comprises the following steps:
s1: 1g of tin antimony oxide (BET 95 m) was treated in 35ml of ethanol 2 Carrying out ultrasonic dispersion on the particles for 10min;
s2: adding 0.15g of nano iridium particles into the dispersion liquid obtained in the step S1, continuing ultrasonic dispersion for 25min, and fully stirring at 600rpm for 48h at the room temperature of 25 ℃ to ensure that nano iridium particles are carried on the tin antimony oxide, so as to obtain a mixed solution of the tin antimony oxide/iridium composite nano particles;
s3: centrifuging the mixed solution obtained in the step S2 at 11000rpm, and repeating the steps for 3 times by using isopropanol to carry out ultrasonic treatment for 5min to obtain black solid particles;
s4: and (3) fully drying the black solid particles obtained in the step (S3) for 7 hours at the temperature of 70 ℃ under the vacuum condition to obtain the tin antimony oxide/iridium composite nano particles.
In the present example, the specific surface area of the tin antimony oxide was 95m 2 /g; the grain diameter of the nano iridium is 2-4nm; the grain diameter of the tin antimony oxide is 20-40nm.
Example 3
The preparation method of the supported nano iridium catalyst comprises the following steps:
s1: at a ratio of 1:1 in 35ml ethanol: for 1g of tin antimony oxide (BET 95 m) 2 Carrying out ultrasonic dispersion on the particles for 10min;
s2: adding 0.2g of nano iridium particles into the dispersion liquid obtained in the step S1, continuing ultrasonic dispersion for 25min, and fully stirring at 600rpm for 48h at the room temperature of 25 ℃ to ensure that nano iridium particles are carried on the tin antimony oxide, so as to obtain a mixed solution of the tin antimony oxide/iridium composite nano particles;
s3: centrifuging the mixed solution obtained in the step S2 at 11000rpm, and repeating the steps for 3 times by using isopropanol to carry out ultrasonic treatment for 5min to obtain black solid particles;
s4: and (3) fully drying the black solid particles obtained in the step (S3) for 7 hours at the temperature of 70 ℃ under the vacuum condition to obtain the tin antimony oxide/iridium composite nano particles.
In the present example, the specific surface area of the tin antimony oxide was 95m 2 /g; the grain diameter of the nano iridium is 2-4nm; the grain diameter of the tin antimony oxide is 20-40nm.
Comparative example 1
The difference to example 1 is that: the iridium content of comparative example 1 was higher depending on the kind of catalyst used and the iridium content.
The comparative example used a commercial iridium oxide catalyst as the Ningbo department innovative energy technology iridium oxide.
Test example 1 catalyst polarization comparison
The experimental steps are as follows:
the catalyst was ultrasonically dispersed and uniformly sprayed on a 5X 5cm Nafion-115 proton exchange membrane, the catalyst loading was 35mg for both examples and comparative examples and the membrane electrode was assembled using an electrolytic cell, and the current density was set at 0-2.5A/cm 2 And (3) testing and data acquisition using a battery detection system. The collected voltage and current data were plotted as a curve for comparison using the data processing software Origin.
As shown in FIG. 1, which is a comparative graph of polarization curves of examples 1, 2 and 3 of the present application and comparative example 1, it can be seen that the performances of examples 1, 2 and 3 are better than those of comparative example 1 under the same conditions, and it is proved that the catalyst prepared by the method of the present application has better application performance.
Test example 2 preparation of Standard Membrane electrode to be tested for catalyst sample spraying
The difficulty of dispersing the catalyst can be roughly judged by spraying the catalyst prepared in example 1 onto a proton exchange membrane, and as can be seen from fig. 2, the catalyst coated part is uniform and compact, no obvious defect is caused, and the catalyst is uniform and no hard-to-disperse agglomerate is caused.
Test example 3 comparison of polarization curves of tin antimony oxide catalysts of different BET
The prepared tin antimony oxide catalysts of different BET were ultrasonically dispersed and uniformly sprayed on Nafion-115 proton exchange membranes of 5X 5cm according to the method of example 1, the catalyst loadings were all 35mg and the membrane electrodes were assembled using an electrolytic cell, and the current densities were set to 0-2.5A/cm 2 And (3) testing and data acquisition using a battery detection system. Collected BET was 95m using data processing software Origin 2 /g、45m 2 /g and 5m 2 Catalyst sample voltage and current data per gram are plotted as curves for comparison.
As can be seen from the polarization curve of FIG. 3, the catalyst samples with higher BET perform better, so BET95m is preferred in this patent 2 Samples were prepared with above/g of tin antimony oxide particles.
It will be evident to those skilled in the art that the application is not limited to the details of the foregoing illustrative embodiments, and that the present application may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the application being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (9)
1. A supported nano iridium catalyst is characterized in that: the nano iridium catalyst is of a tin antimony oxide loaded nano iridium-based composite structure; wherein the mass content of iridium in the catalyst is 9-40%; the specific surface area of the tin antimony oxide is not less than 95m 2 /g。
2. The supported nano iridium catalyst according to claim 1, wherein: the supported nano iridium catalyst has a porous structure, and the average pore diameter is 2 nm-8 nm.
3. The supported nano iridium catalyst according to claim 2, wherein: the particle size of the nano iridium is 2 nm-4 nm, and the particle size range of the tin antimony oxide is 20 nm-40 nm.
4. The preparation method of the supported nano iridium catalyst is characterized by comprising the following steps of:
s1: carrying out ultrasonic dispersion on 60-90 parts by weight of tin antimony oxide particles in an organic solvent for 5-10 min;
s2: adding 10-40 parts by mass of nano iridium particles into the dispersion liquid obtained in the step S1, continuing ultrasonic dispersion for 20-30 min, and fully stirring to obtain a mixed solution of tin antimony oxide/iridium composite nano particles;
s3: centrifuging the mixed solution obtained in the step S2 for 3-5 times, and performing ultrasonic cleaning to obtain black solid particles;
s4: and (3) fully drying the black solid particles obtained in the step (S3) for 6-8 hours to obtain the tin antimony oxide/iridium composite nano particles.
5. The method for preparing the supported nano iridium catalyst according to claim 4, wherein the method comprises the following steps: in S1, the organic solvent used is ethanol, ethylene glycol or a mixture of ethanol and ethylene glycol.
6. The method for preparing the supported nano iridium catalyst according to claim 4, wherein the method comprises the following steps: in S2, stirring time is 48-72 h.
7. The method for preparing the supported nano iridium catalyst according to claim 4, wherein the method comprises the following steps: in S3, the centrifugation speed of the mixed solution is 10000-12000 rpm, and optionally, 10000rpm.
8. The method for preparing the supported nano iridium catalyst according to claim 4, wherein the method comprises the following steps: in S4, the drying temperature of the black solid particles is 50 to 70 ℃.
9. The use of the supported nano iridium catalyst according to claim 1-3 in water electrolysis catalysis,
the method is characterized in that: the supported nano iridium catalyst can be used for preparing hydrogen by cathode electrolysis water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202310752619.7A CN116905027A (en) | 2023-06-25 | 2023-06-25 | Supported nano iridium catalyst, preparation method and application |
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| CN202310752619.7A CN116905027A (en) | 2023-06-25 | 2023-06-25 | Supported nano iridium catalyst, preparation method and application |
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