CN105958085A - Preparation method for metal-organic-framework-loaded platinum-based catalyst - Google Patents
Preparation method for metal-organic-framework-loaded platinum-based catalyst Download PDFInfo
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- CN105958085A CN105958085A CN201610302325.4A CN201610302325A CN105958085A CN 105958085 A CN105958085 A CN 105958085A CN 201610302325 A CN201610302325 A CN 201610302325A CN 105958085 A CN105958085 A CN 105958085A
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- preparation
- organic framework
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- metallic organic
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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
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
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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
Abstract
The invention discloses a preparation method for a metal-organic-framework-loaded platinum-based catalyst. The metal organic framework is added to an alcoholic solution and the mixture is subjected to ultrasonic oscillation; then a mixed solution of chloroplatinic acid and cobalt oxide is added in a dropwise manner; next, NaOH is added and stirred, and the mixture is placed in a microwave oven to be heated intermittently; and next, the mixture is subjected to cooling, suction filtration and vacuum drying to obtain the metal-organic-framework-loaded platinum-based catalyst. The catalyst prepared by the invention is small in granules, hard to agglomerate, high in dispersibility and high in electrochemical catalytic activity.
Description
Technical field
The present invention relates to the preparation method of a kind of metallic organic framework load platinum catalyst.
Background technology
Oxygen reduction catalyst agent conventional in fuel cell and lithium-air battery at present is carbon supported platinum-based catalyst, but due to Pt shortage of resources,
Expensive, it is necessary to take suitable preparation method and process conditions, improve the dispersibility of Pt, reduce Pt granular size, reduce Pt at catalyst
In load capacity, reduce catalyst cost.The method preparing unit and multicomponent catalyst at present is a lot, e.g., impregnates a liquid phase reduction: by Pt
Presoma dissolve after, mix with activity carbon carrier, add reducing agent, such as NaBH4, formalin, sodium citrate, sodium formate, hydrazine etc.,
Make Pt reduction, deposit on activated carbon, after drying, obtain Pt/C catalyst.The advantage of this method is that method is easy, and shortcoming is prepared urging
Agent dispersibility is poor, and mean diameter is bigger.But preparation has one more scabrous problem of Pt base catalyst of polymolecularity.
Summary of the invention
The invention provides the preparation method of platinum based catalyst of a kind of metallic organic framework load, the active component high degree of dispersion of the catalyst of preparation,
It is difficult to reunite, overcomes prior art defect.
The preparation method of the platinum based catalyst of a kind of metallic organic framework load is carried out in the steps below:
Being added by metallic organic framework in alcoholic solution, with sonic oscillation to forming uniform dispersion, the most dropwise dropping chloroplatinic acid and cobaltous chloride mixing are molten
Liquid, stirs 30 minutes, is subsequently placed in intermittent-heating in microwave oven, cools down sucking filtration, vacuum drying 10 hours, obtains metallic organic framework supporting Pt
Base nano-catalyst.
The preparation method of the platinum based catalyst of a kind of metallic organic framework load, described Pt element and Co elemental mole ratios are 1:1.
The preparation method of the platinum based catalyst of a kind of metallic organic framework load, described metallic organic framework ratio in the catalyst is 85-99.5%.
The preparation method of the platinum based catalyst of a kind of metallic organic framework load, described alcohol is: ethylene glycol, ethanol and glycerol.
A kind of preparation method of the platinum based catalyst of metallic organic framework load, the metal ion of described metallic organic framework is: Cr, Mn, Fe,
One or both and the mixture of above element arbitrary proportion in Co, Ni, Ti, Zr, Mo, Sn, Se, Ca.
The present invention provides a kind of simple and quick preparation method, applied microwave control technique and the relatively mild reducing agent of reducing property, by the work of catalyst
Property composition reverts to the surface of carrier quickly and evenly.The catalyst granules that the inventive method prepares is little, be difficult to reunite, be evenly distributed, electrification
Learn catalysis activity high.The present invention uses the selection of microwave heating, reducing agent and dispersant product particle size to be controlled between 1.5～l0nm.This
Invention is suitable for preparing metallic organic framework and carries unitary and polynary nanometer metal material eelctro-catalyst, can be used for alcohol fuel battery, lithium-air battery and electricity
The nano-catalytic of the high dispersive of chemical sensor electrode.
Detailed description of the invention
Embodiment 1
By 1g metallic organic framework, (central ion is Co, and specific surface area is 534.3m2/ g) add in 20mL ethylene glycol, with sonic oscillation to shape
Uniformly dispersion liquid, the most dropwise dropping 2mL contains 0.01M chloroplatinic acid and 0.01M cobaltous chloride mixed solution, adds formic acid 25 DEG C of conditions
Lower stirring 30 minutes, the mode being subsequently placed in microwave oven under 1000W power heating 10s interval 50s heats 10min, cools down sucking filtration, very
Empty drying 10 hours, obtains metallic organic framework supporting Pt base nano-catalyst, and the efficiency for charge-discharge for lithium-air battery is 89.7%.
Embodiment 2
By 0.5g metallic organic framework, (central ion is Mn, and specific surface area is 3981.2m2/ g) add in 20mL ethylene glycol, use sonic oscillation
To forming uniform dispersion, the most dropwise dropping 5mL contains 0.2M chloroplatinic acid and 0.2M cobaltous chloride mixed solution, adds formic acid at 25 DEG C of bars
Stirring 30 minutes under part, the mode being subsequently placed in microwave oven under 700W power heating 10s interval 50s heats 10min, cools down sucking filtration, very
Empty drying 10 hours, prepares metallic organic framework and carries Pt base nano-catalyst, and the efficiency for charge-discharge for lithium-air battery is 83.6%.
Embodiment 3
By 0.7g metallic organic framework, (central ion is Fe, and specific surface area is 2353.8m2/ g) add in 20mL ethylene glycol, with sonic oscillation extremely
Forming uniform dispersion, the most dropwise dropping 4mL contains 0.2M chloroplatinic acid and 0.2M cobaltous chloride mixed solution, adds formic acid 25 DEG C of conditions
Lower stirring 30 minutes, the mode being subsequently placed in microwave oven under 1500W power heating 10s interval 50s heats 10min, cools down sucking filtration, very
Empty drying 10 hours, prepares metallic organic framework and carries Pt base nano-catalyst, and the efficiency for charge-discharge for lithium-air battery is 84.1%.
Claims (5)
1. the preparation method of the platinum based catalyst of a metallic organic framework load, it is characterised in that preparation method is as follows:
Being added by metallic organic framework in alcoholic solution, with sonic oscillation to forming uniform dispersion, the most dropwise dropping chloroplatinic acid and cobaltous chloride mixing are molten
Liquid, adds formic acid and stirs 30 minutes, be subsequently placed in intermittent-heating in microwave oven, cool down sucking filtration, vacuum drying 10 hours, obtain metal organic
The platinum based catalyst of skeleton adulteration.
2. according to the preparation method of the platinum based catalyst of a kind of metallic organic framework load described in claim l, it is characterised in that Pt element and Co
Elemental mole ratios is 1:1.
3. according to the preparation method of the platinum based catalyst of a kind of metallic organic framework load described in claim l, it is characterised in that metallic organic framework
Part by weight in the catalyst is 85-99.5%.
4. according to the preparation method of the platinum based catalyst of a kind of metallic organic framework load described in claim l, it is characterised in that the alcohol in alcoholic solution
For: ethylene glycol, ethanol and glycerol.
5. according to the preparation method of the Pt base catalyst of a kind of metallic organic framework load described in claim l, it is characterised in that the organic bone of metal
The metal ion of frame is: one or both and the above element arbitrary proportion in Cr, Mn, Fe, Co, Ni, Ti, Zr, Mo, Sn, Se, Ca
Mixture.
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| CN201610302325.4A CN105958085A (en) | 2016-05-09 | 2016-05-09 | Preparation method for metal-organic-framework-loaded platinum-based catalyst |
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| CN201610302325.4A CN105958085A (en) | 2016-05-09 | 2016-05-09 | Preparation method for metal-organic-framework-loaded platinum-based catalyst |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106582857A (en) * | 2016-12-16 | 2017-04-26 | 昆明理工大学 | Preparation method of metal organic framework for loading nano silver |
| CN108110260A (en) * | 2017-12-29 | 2018-06-01 | 成都新柯力化工科技有限公司 | A kind of fuel-cell catalyst and preparation method of metal-organic framework modification |
| CN109065901A (en) * | 2018-07-12 | 2018-12-21 | 扬州大学 | Transition metal phosphide-noble metal phosphide composite fuel cell catalyst and its preparation method and application |
| CN109904472A (en) * | 2017-12-11 | 2019-06-18 | 中国科学院大连化学物理研究所 | A kind of amorphous PtSe elctro-catalyst and its preparation and application |
| CN112675913A (en) * | 2019-10-18 | 2021-04-20 | 南京理工大学 | Palladium-loaded titanium-based metal organic framework catalyst, preparation method and application |
| CN113130923A (en) * | 2021-04-15 | 2021-07-16 | 北京师范大学 | Preparation method and application of two-dimensional porous carbon supported catalyst |
| CN113363516A (en) * | 2020-03-04 | 2021-09-07 | 香港科技大学 | Catalyst carrier, composite catalyst, preparation method thereof, fuel cell and application thereof |
| CN113659164A (en) * | 2021-08-11 | 2021-11-16 | 南京大学 | Preparation method of fuel cell platinum-based alloy catalyst |
| WO2022111008A1 (en) * | 2020-11-26 | 2022-06-02 | 中国科学院大连化学物理研究所 | Platinum-and-cobalt-based alloy encapsulated with nitrogen-and-phosphorus-co-doped metal organic framework, preparation method therefor and use thereof |
| CN115888831A (en) * | 2022-09-30 | 2023-04-04 | 云南大学 | Preparation method and application of platinum-loaded tin-iron bimetallic organic framework material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103191778A (en) * | 2013-02-28 | 2013-07-10 | 北京化工大学常州先进材料研究院 | Preparation method of metal organic framework loaded Pt-base catalyst |
-
2016
- 2016-05-09 CN CN201610302325.4A patent/CN105958085A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103191778A (en) * | 2013-02-28 | 2013-07-10 | 北京化工大学常州先进材料研究院 | Preparation method of metal organic framework loaded Pt-base catalyst |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106582857A (en) * | 2016-12-16 | 2017-04-26 | 昆明理工大学 | Preparation method of metal organic framework for loading nano silver |
| CN109904472B (en) * | 2017-12-11 | 2021-08-31 | 中国科学院大连化学物理研究所 | Amorphous PtSe electrocatalyst and preparation and application thereof |
| CN109904472A (en) * | 2017-12-11 | 2019-06-18 | 中国科学院大连化学物理研究所 | A kind of amorphous PtSe elctro-catalyst and its preparation and application |
| CN108110260A (en) * | 2017-12-29 | 2018-06-01 | 成都新柯力化工科技有限公司 | A kind of fuel-cell catalyst and preparation method of metal-organic framework modification |
| CN109065901A (en) * | 2018-07-12 | 2018-12-21 | 扬州大学 | Transition metal phosphide-noble metal phosphide composite fuel cell catalyst and its preparation method and application |
| CN109065901B (en) * | 2018-07-12 | 2021-09-03 | 扬州大学 | Transition metal phosphide-noble metal phosphide composite fuel cell catalyst and preparation method and application thereof |
| CN112675913A (en) * | 2019-10-18 | 2021-04-20 | 南京理工大学 | Palladium-loaded titanium-based metal organic framework catalyst, preparation method and application |
| CN113363516A (en) * | 2020-03-04 | 2021-09-07 | 香港科技大学 | Catalyst carrier, composite catalyst, preparation method thereof, fuel cell and application thereof |
| WO2022111008A1 (en) * | 2020-11-26 | 2022-06-02 | 中国科学院大连化学物理研究所 | Platinum-and-cobalt-based alloy encapsulated with nitrogen-and-phosphorus-co-doped metal organic framework, preparation method therefor and use thereof |
| CN113130923A (en) * | 2021-04-15 | 2021-07-16 | 北京师范大学 | Preparation method and application of two-dimensional porous carbon supported catalyst |
| CN113659164A (en) * | 2021-08-11 | 2021-11-16 | 南京大学 | Preparation method of fuel cell platinum-based alloy catalyst |
| CN113659164B (en) * | 2021-08-11 | 2022-11-11 | 南京大学 | Preparation method of fuel cell platinum-based alloy catalyst |
| CN115888831A (en) * | 2022-09-30 | 2023-04-04 | 云南大学 | Preparation method and application of platinum-loaded tin-iron bimetallic organic framework material |
| CN115888831B (en) * | 2022-09-30 | 2024-02-20 | 云南大学 | Preparation method and application of platinum-loaded tin-iron bimetallic organic frame material |
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