CN107768689A - A kind of preparation method of the compound platinum catalyst of pyridine ion liquid polyoxometallate - Google Patents
A kind of preparation method of the compound platinum catalyst of pyridine ion liquid polyoxometallate Download PDFInfo
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- CN107768689A CN107768689A CN201711025049.2A CN201711025049A CN107768689A CN 107768689 A CN107768689 A CN 107768689A CN 201711025049 A CN201711025049 A CN 201711025049A CN 107768689 A CN107768689 A CN 107768689A
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- Prior art keywords
- polyoxometallate
- ion liquid
- rgo
- pyridine ion
- epy
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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
- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
-
- 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
- H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1009—Fuel cells with solid electrolytes with one of the reactants being liquid, solid or liquid-charged
- H01M8/1011—Direct alcohol fuel cells [DAFC], e.g. direct methanol fuel cells [DMFC]
-
- 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 present invention provides a kind of preparation method of the compound platinum catalyst of pyridine ion liquid polyoxometallate, and this method is with redox graphene（rGO）For carrier, while pyridine ion liquid polyoxometallate is introduced, using chloroplatinic acid as platinum source, ethylene glycol is that reducing agent prepares the compound platinum catalyst Pt/ (epy) of pyridine ion liquid polyoxometallate3PMo12O40/rGO.Obtained composite catalyst has good Electrocatalytic Oxidation of Methanol activity and resisting CO poisoning performance, thus has potential application prospect in terms of fuel cell.
Description
Technical field
The present invention relates to a kind of preparation method of the compound platinum catalyst of pyridine ion liquid polyoxometallate.
Background technology
DMFC（DMFC）It is a kind of new fuel cell, there is efficient, safety, energy density height, make
The advantages that with recyclable fuel, it is that other type fuel cells are incomparable, has a extensive future.Electrocatalytic Oxidation of Methanol
Agent is the critical material in DMFC, and now widely used is platinum base（Pt bases）Elctro-catalyst, but Pt scarcity of resources, price are held high
It is expensive, meanwhile, the intermediate product carbon monoxide that Pt catalyst is easily aoxidized by methanol（CO）Poison, so as to reduce Pt catalytic activity,
Cause Pt usage amounts high, DMFC costs remain high.Therefore, activity, the stability of Pt catalyst are improved, enhancing Pt catalyst
CO tolerance catalysts performance, it is the key issue for realizing DMFC commercial applications.
On the one hand, the selection of DMFC catalyst carriers has a major impact for its catalytic activity, stability.Preferable electricity is urged
Agent carrier must be provided simultaneously with high-specific surface area, satisfactory electrical conductivity, corrosion resistance, suitable pore structure and surface group etc..Cause
And most common DMFC catalyst carriers are carbon material, such as carbon black, CNT, activated carbon, porous carbon, carbon fiber.Graphite
Alkene is a kind of tightly packed carbonaceous new material into bi-dimensional cellular shape lattice structure of single layer of carbon atom, compared with other carbon materials,
Graphene is combined by most stable of benzene hexatomic ring, has bigger theoretical specific surface area（About 2630 m2·g-1）More
Good electronic conduction ability (about 2 × 105 cm2·V-1·s-1), thus be considered as optimal catalyst carrier material it
One.
On the other hand, the CO tolerance catalysts performance for strengthening Pt catalyst is also the key of DMFC development.Polyoxometallate
（POM）It is a kind of multinuclear mixed valence compound containing oxygen bridge with unique texture and performance, complex is had concurrently in structure
With the feature of metal oxide, have acid and oxidation-reduction quality concurrently in performance, be widely used in catalysis, electrochemistry, optics,
The numerous areas such as functional material.As a kind of inorganic electroactive material, it is mainly characterized by that one can be undergone polyoxometallate
Reversible, multistep the multielectron transfer process of series, has good redox reversible, can receive and discharge electronics,
The relay station of electronics can be served as, this electrocatalytic properties to polyoxometallate is highly beneficial.There are some researches show DMFC's
Polyoxometallate is introduced in anode electrocatalyst, may act as oxidant, intermediate product CO is changed into nontoxic CO2, so as to
Prevent catalyst CO poisoning and deactivations.Moreover, the polyoxometallate of reduction can also reoxidize, and recycle.
Therefore, graphene and polyoxometallate are introduced into DMFC catalyst simultaneously, construct new Pt/ polyoxometallic acids
Salt/graphene composite catalyst material, it is expected to the catalytic activity, stability and CO tolerance catalysts performance of Pt catalyst are effectively improved,
Theoretical direction is provided for the research of new fuel cell catalyst material, development and application, establishes application foundation.
The content of the invention
A kind of preparation method of the compound platinum catalyst of pyridine ion liquid polyoxometallate.
The present invention relates to a kind of compound platinum catalyst of pyridine ion liquid polyoxometallate, its composition is Pt/ (epy)3PMo12O40/ redox graphene（Pt/(epy)3PMo12O40/rGO）, synthesis step includes the following steps.
(1) by 0.02 gN- ethylpyridine molybdophosphate (epy)3PMo12O40It is placed in round-bottomed flask, adds 1 mLN,N- dimethylformamide（DMF）Dissolving.
(2) 25 mL ethylene glycol are added, ultrasonic 5min is well mixed.
(3) 0.04 g reduction-oxidation graphite, ultrasonic disperse 30min are added.
(4) the mol L of 1 mL 0.05 are sequentially added-1Chloroplatinic acid（H2PtCl6•6H2O）Ethylene glycol solution and 0.4 mL
0.4 mol•L-1Potassium hydroxide（KOH）The aqueous solution, then more than magnetic agitation 3h, it is sufficiently mixed it.
(5) will be heated to reflux naturally cooling to room temperature after 3 h under the conditions of 160 DEG C of the mixed solution normal pressure of step (4),
Continue to stir 12h.
(6) product made from step (5) is fully washed with high purity water and acetone, 60 DEG C of 12 h of vacuum drying, pyrrole is made
The compound platinum catalyst Pt/ (epy) of pyridine ionic liquid polyoxometallate3PMo12O40/rGO。
Brief description of the drawings
Fig. 1 is the compound platinum catalyst Pt/ (epy) of pyridine ion liquid polyoxometallate produced by the present invention3PMo12O40/
RGO high-resolution-ration transmission electric-lens photo, it can be seen that introduce the Pt of the compound platinum catalyst of pyridine ion liquid polyoxometallate
Particle diameter very little, about 2.8 nanometers, and be uniformly dispersed on the big catalyst carrier rGO of specific surface area.
Fig. 2 is the compound platinum catalyst Pt/ (epy) of pyridine ion liquid polyoxometallate prepared by the present invention3PMo12O40/
RGO and 20% business platinum carbon（Pt/C）The methanol oxidation cycle volt-ampere comparison diagram of catalyst, Pt/rGO, as seen from Figure 2, Pt/
(epy)3PMo12O40/ rGO Electrocatalytic Oxidation of Methanol activity is significantly larger than 20% business Pt/C catalyst and Pt/rGO, illustrates pyrrole
Pyridine ionic liquid polyoxometallate (epy)3PMo12O40Introducing effectively increase the catalytic activity of Pt catalyst.
Fig. 3 is the compound platinum catalyst Pt/ (epy) of pyridine ion liquid polyoxometallate prepared by the present invention3PMo12O40/
RGO and Pt/rGO carbon monoxide（CO）Dissolution cyclic voltammetry curve figure, as seen from Figure 3, Pt/ (epy)3PMo12O40/rGO
CO stripping curve starting platforms current potential be less than Pt/rGO, illustrate Pt/ (epy)3PMo12O40/ rGO has more preferable than Pt/rGO
CO tolerance catalysts performance, it was demonstrated that pyridine ion liquid polyoxometallate (epy)3PMo12O40Introducing can be effectively improved Pt catalyst
CO tolerance catalysts performance.
Embodiment
Embodiment 1
Weigh 0.02 g N- ethylpyridines molybdophosphates (epy)3PMo12O40It is placed in round-bottomed flask, adds 1 mL N, N- bis-
NMF（DMF）Dissolving, 25 mL ethylene glycol are added, ultrasonic 5min is well mixed, and adds 0.04 g graphite oxides, ultrasound
Scattered 30min, then sequentially adds the mol L of 1 mL 0.05-1Chloroplatinic acid（H2PtCl6）Ethylene glycol solution and 0.4 mL 0.4
mol•L-1Potassium hydroxide（KOH）The aqueous solution, more than magnetic agitation 3h, be sufficiently mixed it, under the conditions of 160 DEG C of normal pressure plus
Room temperature is naturally cooled to after 3 h of heat backflow, continues to stir 12h, then is fully washed with high purity water and acetone, 60 DEG C of vacuum drying
12 h, the compound platinum catalyst Pt/ (epy) of pyridine ion liquid polyoxometallate is made3PMo12O40/rGO。
Claims (2)
1. a kind of preparation method of the compound platinum catalyst of pyridine ion liquid polyoxometallate, it is characterised in that follow these steps
Carry out：It is by compositionN- ethylpyridine molybdophosphate [(epy)3PMo12O40] the g of pyridine ion liquid polyoxometallate 0.02
It is placed in round-bottomed flask, adds 1 mLN,N- dimethylformamide（DMF）Dissolving, adds 25 mL ethylene glycol, and ultrasonic 5min is mixed
0.04 g reduction-oxidation graphite is added after closing uniformly（rGO）, ultrasonic disperse 30min, then sequentially add 1 mL 0.05
mol•L-1Chloroplatinic acid（H2PtCl6•6H2O）Ethylene glycol solution and the mol L of 0.4 mL 0.4-1The KOH aqueous solution, magnetic agitation
More than 3h, it is sufficiently mixed, is heated to reflux naturally cooling to room temperature after 3 h under the conditions of 160 DEG C of normal pressure, continues to stir 12h,
Fully washed with high purity water and acetone, 60 DEG C of 12 h of vacuum drying, produce the compound platinum of pyridine ion liquid polyoxometallate and urge
Agent Pt/ (epy)3PMo12O40/rGO。
2. preparation method according to claim 1, the compound platinum catalyst of pyridine ion liquid polyoxometallate of gained
Pt/(epy)3PMo12O40/ rGO has good Electrocatalytic Oxidation of Methanol activity and anti-carbon monoxide（CO）Poisoning performance.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108435252A (en) * | 2018-04-10 | 2018-08-24 | 新疆大学 | A kind of preparation method of the compound platinum catalyst of conducting polymer polyoxometallate |
| CN112366329A (en) * | 2020-11-20 | 2021-02-12 | 新疆大学 | Preparation method of three-dimensional coal-based graphene supported platinum catalyst |
| CN114628706A (en) * | 2022-04-11 | 2022-06-14 | 西安凯立新材料股份有限公司 | Catalyst for proton exchange membrane fuel cell and preparation method thereof |
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| US7488699B2 (en) * | 2004-12-30 | 2009-02-10 | Industrial Technology Research Institute | Hollow mesoporous carbon electrode-catalyst for direct methanol fuel cell and preparation thereof |
| CN102664276A (en) * | 2012-04-24 | 2012-09-12 | 北京化工大学 | Titanium dioxide-modified (TiO2-modified) carbon-loaded platinum (Pt)-based electric catalyst and preparation method thereof |
| CN102824910A (en) * | 2012-08-23 | 2012-12-19 | 南京理工大学 | Ternary composite catalyst containing platinum, transition metal oxide and graphene and preparation method thereof |
| CN104810530A (en) * | 2015-03-26 | 2015-07-29 | 桂林电子科技大学 | Preparation method and application of graphene-Pt (platinum) nanoparticle-polypyrrole composite material |
| CN104953138A (en) * | 2015-06-17 | 2015-09-30 | 江苏大学 | Pd-CoSi2/graphene compound electrocatalyst as well as preparation method and application thereof |
| CN106622364A (en) * | 2016-12-21 | 2017-05-10 | 新疆大学 | Solid phase preparation method of ionic liquid polyoxometallate nano electrocatalyst |
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2017
- 2017-10-27 CN CN201711025049.2A patent/CN107768689A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US7488699B2 (en) * | 2004-12-30 | 2009-02-10 | Industrial Technology Research Institute | Hollow mesoporous carbon electrode-catalyst for direct methanol fuel cell and preparation thereof |
| CN102664276A (en) * | 2012-04-24 | 2012-09-12 | 北京化工大学 | Titanium dioxide-modified (TiO2-modified) carbon-loaded platinum (Pt)-based electric catalyst and preparation method thereof |
| CN102824910A (en) * | 2012-08-23 | 2012-12-19 | 南京理工大学 | Ternary composite catalyst containing platinum, transition metal oxide and graphene and preparation method thereof |
| CN104810530A (en) * | 2015-03-26 | 2015-07-29 | 桂林电子科技大学 | Preparation method and application of graphene-Pt (platinum) nanoparticle-polypyrrole composite material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108435252A (en) * | 2018-04-10 | 2018-08-24 | 新疆大学 | A kind of preparation method of the compound platinum catalyst of conducting polymer polyoxometallate |
| CN112366329A (en) * | 2020-11-20 | 2021-02-12 | 新疆大学 | Preparation method of three-dimensional coal-based graphene supported platinum catalyst |
| CN114628706A (en) * | 2022-04-11 | 2022-06-14 | 西安凯立新材料股份有限公司 | Catalyst for proton exchange membrane fuel cell and preparation method thereof |
| CN114628706B (en) * | 2022-04-11 | 2024-02-13 | 西安凯立新材料股份有限公司 | Catalyst for proton exchange membrane fuel cell and preparation method thereof |
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