CN106159282A - Membrane electrode of fuel batter with proton exchange film eelctro-catalyst and preparation method thereof - Google Patents
Membrane electrode of fuel batter with proton exchange film eelctro-catalyst and preparation method thereof Download PDFInfo
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- CN106159282A CN106159282A CN201510145774.8A CN201510145774A CN106159282A CN 106159282 A CN106159282 A CN 106159282A CN 201510145774 A CN201510145774 A CN 201510145774A CN 106159282 A CN106159282 A CN 106159282A
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- eelctro
- catalyst
- proton exchange
- membrane electrode
- exchange film
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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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- 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
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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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- Engineering & Computer Science (AREA)
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- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a kind of membrane electrode of fuel batter with proton exchange film eelctro-catalyst and preparation method thereof, a kind of membrane electrode of fuel batter with proton exchange film eelctro-catalyst, prepared by following preparation method: graphene oxide powder adds in polyhydric alcohol, and ultrasonic disperse obtains graphite oxide enolate solution；Take chloroplatinic acid aqueous solution to be placed in polyhydric alcohol and obtain chloroplatinic acid in alcohol；Above-mentioned prepared graphite oxide enolate solution and chloroplatinic acid in alcohol are mixed；Adding aqueous slkali regulation pH to 8～12 in the mixed solution prepared, be transferred in microwave reaction kettle, 180～250W heats are to 80～180 DEG C of reactions 5～25min；Reactant liquor cools down, and vacuum filters；The alternately washing of filter cake organic solvent and deionized water is neutral to filtrate pH drier to constant weight, obtains Pt/ Graphene eelctro-catalyst.Particle agglomeration avoided by eelctro-catalyst of the present invention, and particle diameter is little, and the catalysis activity of the eelctro-catalyst of high dispersive is high, adds the utilization rate of eelctro-catalyst.
Description
Technical field
The invention belongs to fuel cell field, relate to a kind of membrane electrode of fuel batter with proton exchange film eelctro-catalyst and preparation side thereof
Method, relates to Pt/ Graphene eelctro-catalyst and preparation method thereof.
Background technology
Fuel cell is a kind of electrochemical appliance that the chemical energy in fuel hydrogen is directly translated into electric energy, and energy resource density is high, ring
Border is friendly, has development prospect widely.Conventional fuel cell membrane electrode eelctro-catalyst is Pt/C catalyst, typically uses
H2PtCl6Direct-reduction process is made, and directly uses H2PtCl6During preparation Pt, the response time is long, PtCl6 -2Suction is easily assembled at carbon surface
Attached, the dispersibility of Pt is not high enough so that Pt particle diameter is excessive, up to tens nanometers, and skewness, prepared electro-catalysis
Agent is in electrochemical reaction, and eelctro-catalyst hydraulic performance decline, electrode performance is the best.Therefore, it is necessary to find new preparation method and work
Skill condition, reduces the particle size of Pt in catalyst, increases Pt dispersion on carrier and effective rate of utilization.
Summary of the invention
It is an object of the invention to for deficiency of the prior art, it is provided that a kind of membrane electrode of fuel batter with proton exchange film eelctro-catalyst
Preparation method.
It is an object of the invention to be achieved through the following technical solutions:
A kind of membrane electrode of fuel batter with proton exchange film eelctro-catalyst, is prepared by following preparation method:
(1), graphene oxide powder add in polyhydric alcohol, ultrasonic disperse obtains graphite oxide enolate solution, described oxidation stone
The mass volume ratio of ink alkene powder and polyhydric alcohol is 0.5～1mg:1mL；The chloroplatinic acid aqueous solution taking 0.05～0.06mol/L is put
Chloroplatinic acid in alcohol is obtained in polyhydric alcohol；Above-mentioned prepared graphite oxide enolate solution and chloroplatinic acid in alcohol are mixed, ultrasonic point
Dissipating, in mixed solution, the amount ratio of graphene oxide and chloroplatinic acid is 390～2000g:1mol；
(2), step (1) prepare mixed solution in add aqueous slkali regulation pH to 8～12, be transferred in microwave reaction kettle,
180～250W heats are to 80～180 DEG C of reactions 5～25min；Reactant liquor cools down, and vacuum filters；Filter cake is with having
The alternately washing of machine solvent and deionized water is neutral to filtrate pH, then is dried to constant weight at 60～90 DEG C, obtains with graphene oxide
For carrier, Pt/ Graphene eelctro-catalyst with Pt as active component.
In described membrane electrode of fuel batter with proton exchange film eelctro-catalyst, the weight/mass percentage composition of Pt is 9～50%.
Preferably, in described graphite oxide enolate solution, the amount ratio of graphene oxide powder and polyhydric alcohol is 0.6～0.9
Mg:1mL.
Preferably, mixed solution microwave power in microwave reaction kettle is 180～200W, reaction temperature be 120～
180 DEG C, the response time is 5～10min.
Described polyhydric alcohol is the one in ethylene glycol, propylene glycol or Polyethylene Glycol；Described aqueous slkali is NaOH or KOH
Solution, specifically can use the NaOH solution of mass fraction 5% or the KOH solution of 5%；Having of described washing filter cake
Machine solvent is the one in dehydrated alcohol, acetone.
It is a further object to provide the preparation method of membrane electrode of fuel batter with proton exchange film eelctro-catalyst, including following
Step:
(1), graphene oxide powder add in polyhydric alcohol, ultrasonic disperse obtains graphite oxide enolate solution, described oxidation stone
The mass volume ratio of ink alkene powder and polyhydric alcohol is 0.5～1mg:1mL；The chloroplatinic acid aqueous solution taking 0.05～0.06mol/L is put
Chloroplatinic acid in alcohol is obtained in polyhydric alcohol；Above-mentioned prepared graphite oxide enolate solution and chloroplatinic acid in alcohol are mixed, ultrasonic point
Dissipating, in mixed solution, the amount ratio of graphene oxide and chloroplatinic acid is 390～2000g:1mol；
(2), step (1) prepare mixed solution in add aqueous slkali regulation pH to 8～12, be transferred in microwave reaction kettle,
180～250W heats are to 80～180 DEG C of reactions 5～25min；Reactant liquor cools down, and vacuum filters；Filter cake is with having
The alternately washing of machine solvent and deionized water is neutral to filtrate pH, then is dried to constant weight at 60～90 DEG C, obtains with graphene oxide
For carrier, Pt/ Graphene eelctro-catalyst with Pt as active component.
In step (1), in described graphite oxide enolate solution the amount ratio of graphene oxide powder and polyhydric alcohol be preferably 0.6～
0.9mg:1mL.Described polyhydric alcohol is the one in ethylene glycol, propylene glycol or Polyethylene Glycol.
In step (2), described aqueous slkali is NaOH or KOH solution, specifically can use the NaOH of mass fraction 5%
Solution or the KOH solution of 5%.
Mixed solution microwave power in microwave reaction kettle is preferably 180～200W, reaction temperature be preferably 120～
180 DEG C, the response time is preferably 5～10min.
The organic solvent of described washing filter cake is the one in dehydrated alcohol, acetone.
Beneficial effects of the present invention:
The eelctro-catalyst electrode activity that the present invention prepares is good, electrochemical reaction is active good.Graphene oxide is used to carry as Pt
Body, graphene oxide has amphiphilic character, has good dispersion, prevent PtCl in water and alcoholic solution6 -2Assemble absorption raw
Become bulky grain platinum crystal grain, it is to avoid particle agglomeration, beneficially eelctro-catalyst particle size dispersion, particle diameter is little, it is possible to play excellent catalysis
Performance, improves platinum utilization, thus improves the utilization rate of eelctro-catalyst, makes catalyst have higher activity, significantly drops
The consumption of low platinum.Polyhydric alcohol can be with stable metal nanoparticle as reaction solution and dispersant simultaneously, and reactant liquor is steady under alkalescence
Fixed, graphene oxide and chloroplatinic acid can make eelctro-catalyst particle diameter be in Nano Particle by microwave process for synthesizing.
Detailed description of the invention
Embodiment 1
Weigh 200mg graphene oxide powder, be placed in supersonic oscillations in 300mL propylene glycol, obtain the oxidation stone of mix homogeneously
Ink enolate solution；Measure 0.05mol/L chloroplatinic acid 2mL, be placed in 30mL propylene glycol, be uniformly mixed and obtain chloroplatinic acid
Alcoholic solution；Mixing above two solution, stirring is lower adds mass fraction 5%NaOH solution, regulates pH=10, stirs 30
Min, puts in microwave reaction kettle, microwave power 200W, temperature 180 DEG C, heats 5min, reacts complete, be cooled to room
Temperature；Reactant liquor vacuum filters, the alternately washing of filter cake dehydrated alcohol and deionized water, and washing 3 times is to filtrate pH=7 respectively,
Then in vacuum drying oven at a temperature of 80 DEG C be dried 3 hours to constant weight, be able to graphene oxide be carrier, with Pt as activity
The Pt/ Graphene eelctro-catalyst of composition, the weight/mass percentage composition of Pt about 10%.The Pt/ Graphene eelctro-catalyst that the present embodiment prepares
Particle diameter is in 1～3 nanometers, and eelctro-catalyst particle size dispersion is uniform.
Embodiment 2
Weigh 200mg graphene oxide powder, be placed in supersonic oscillations in 300mL propylene glycol, obtain the oxidation stone of mix homogeneously
Ink enolate solution；Measure 0.05mol/L chloroplatinic acid 3mL, be placed in 30mL propylene glycol, be uniformly mixed and obtain chloroplatinic acid
Alcoholic solution；Mixing above two solution, stirring is lower adds mass fraction 5%NaOH solution, regulates pH=10, stirs 30
Min, puts in microwave reaction kettle, microwave power 200W, temperature 180 DEG C, heats 5min, reacts complete, be cooled to room
Temperature；Reactant liquor vacuum filters, the alternately washing of filter cake dehydrated alcohol and deionized water, and washing 3 times is to filtrate pH=7 respectively,
Then in vacuum drying oven at a temperature of 80 DEG C be dried 3 hours to constant weight, be able to graphene oxide be carrier, with Pt as activity
The Pt/ Graphene eelctro-catalyst of composition, the weight/mass percentage composition of Pt about 15%.The Pt/ Graphene eelctro-catalyst that the present embodiment prepares
Particle diameter is in 1～3 nanometers, and eelctro-catalyst particle size dispersion is uniform.
Embodiment 3
Weigh 350mg graphene oxide powder, be placed in supersonic oscillations in 400mL ethylene glycol, obtain the oxidation stone of mix homogeneously
Ink enolate solution；Measure 0.06mol/L chloroplatinic acid 6mL, be placed in the ethylene glycol of 20mL, be uniformly mixing to obtain chloroplatinic acid alcohol
Solution；Mixing above two solution, stirring is lower adds 5%KOH solution, regulates pH=12, stirs 20min, be then placed in
In microwave reaction kettle, microwave power 180W, temperature 120 DEG C, heats 8min, reacts complete, be cooled to room temperature；Reactant liquor
Vacuum filters, the alternately washing of filter cake acetone and deionized water, and washing 5 times is to filtrate pH=7 respectively, then in vacuum drying
In case 60 DEG C be dried 5 hours to constant weight, be able to graphene oxide be carrier, Pt/ graphene nano electricity with Pt as active component
Catalyst；The weight/mass percentage composition of Pt about 20%.The Pt/ Graphene eelctro-catalyst particle diameter that the present embodiment prepares is 3～5 nanometers,
Eelctro-catalyst particle size dispersion is uniform.
Embodiment 4
Weigh 150mg graphene oxide powder, be placed in supersonic oscillations in 300mL propylene glycol, obtain the oxidation stone of mix homogeneously
Ink enolate solution；Measure 0.05mol/L chloroplatinic acid 3mL, be placed in 30mL propylene glycol, be uniformly mixed；Mix above-mentioned
Two kinds of solution, the pH=5 of regulation mixed solution, stir 30min, put in microwave reaction kettle, microwave power 200W, temperature
Spend 180 DEG C, heat 5min, react complete, be cooled to room temperature；Reactant liquor vacuum filters, filter cake dehydrated alcohol and deionization
Water alternately washing, respectively washing 3 times, to filtrate PH=7, are then dried 3 hours to permanent in vacuum drying oven at a temperature of 80 DEG C
Weight, be able to graphene oxide be carrier, Pt/ Graphene eelctro-catalyst with Pt as active component, the weight/mass percentage composition of Pt is about
20%.The Pt/ Graphene eelctro-catalyst particle diameter that the present embodiment prepares is 15～20 nanometers, eelctro-catalyst particle diameter skewness.
Embodiment 5
Weigh the Vulcan XC-72 hydrocarbon black powder of 150mg Cabot company, be placed in supersonic oscillations in 300mL propylene glycol,
Obtain the white carbon black alcoholic solution of mix homogeneously；Measuring 0.05mol/L chloroplatinic acid 3mL, be placed in 30mL propylene glycol, stirring mixing is all
Even；Mixing above two solution, the pH=5 of regulation mixed solution, stirs 30min, puts in microwave reaction kettle, microwave merit
Rate 200W, temperature 180 DEG C, heats 5min, reacts complete, be cooled to room temperature；Reactant liquor vacuum filters, and filter cake is with anhydrous
The alternately washing of ethanol and deionized water, respectively washing 3 times are to filtrate PH=7, then dry at a temperature of 80 DEG C in vacuum drying oven
Dry 3 hours to constant weight, be able to white carbon black be carrier, Pt/C eelctro-catalyst with Pt as active component, the weight/mass percentage composition of Pt
About 20%.The Pt/C eelctro-catalyst particle diameter that the present embodiment prepares is 1～3 nanometers, eelctro-catalyst particle diameter skewness.
The electrification of the Pt/ Graphene eelctro-catalyst that embodiment 1-3 prepares is investigated by SUN-FTP500 fuel battery test platform
Learn reactivity.
The Pt/ Graphene eelctro-catalyst battery performance that table 1 embodiment 1-4 prepares
As shown in Table 1: in Pt/ Graphene eelctro-catalyst, the weight/mass percentage composition of Pt is different, eelctro-catalyst electrical property is different, with
The weight/mass percentage composition Pt in eelctro-catalyst improves, and battery performance improves.
The eelctro-catalyst prepared according to commonsense method (embodiment 4) and the inventive method (embodiment 1-3) is contrasted, embodiment
The 4 Pt/ Graphene eelctro-catalysts (Pt of 20%) prepared reach voltage 0.4～0.6V, current intensity 600mA, and embodiment 1
The Pt/ Graphene eelctro-catalyst (Pt of 10%) prepared i.e. can reach effect same.
Material (embodiment 3) will be made with graphene oxide and make the eelctro-catalyst of material (embodiment 5) with white carbon black and contrast, at Pt
Under conditions of identical, the electric current density of Pt/ Graphene eelctro-catalyst of embodiment 3, voltage are substantially better than the Pt/C of embodiment 5
Eelctro-catalyst.
Claims (10)
1. a membrane electrode of fuel batter with proton exchange film eelctro-catalyst, it is characterised in that this eelctro-catalyst is by following preparation side
Method prepares:
(1), graphene oxide powder add in polyhydric alcohol, ultrasonic disperse obtains graphite oxide enolate solution, described oxidation stone
The mass volume ratio of ink alkene powder and polyhydric alcohol is 0.5～1mg:1mL；The chloroplatinic acid aqueous solution taking 0.05～0.06mol/L is put
Chloroplatinic acid in alcohol is obtained in polyhydric alcohol；Above-mentioned prepared graphite oxide enolate solution and hydrogen platinic acid alcoholic solution are mixed, ultrasonic point
Dissipating, in mixed solution, the amount ratio of graphene oxide and chloroplatinic acid is 390～2000g:1mol；
(2), step (1) prepare mixed solution in add aqueous slkali regulation pH to 8～12, be transferred in microwave reaction kettle,
180～250W heats are to 80～180 DEG C of reactions 5～25min；Reactant liquor cools down, and vacuum filters；Filter cake is with having
The alternately washing of machine solvent and deionized water is neutral to filtrate pH, then is dried to constant weight at 60～90 DEG C, obtains with graphene oxide
For carrier, Pt/ Graphene eelctro-catalyst with Pt as active component.
Membrane electrode of fuel batter with proton exchange film eelctro-catalyst the most according to claim 1, it is characterised in that described matter
In proton exchange film fuel cell film pole eelctro-catalyst, the weight/mass percentage composition of Pt is 9～50%.
Membrane electrode of fuel batter with proton exchange film eelctro-catalyst the most according to claim 1, it is characterised in that described oxygen
In functionalized graphene alcoholic solution, the amount ratio of graphene oxide powder and polyhydric alcohol is 0.6～0.9mg:1mL.
Membrane electrode of fuel batter with proton exchange film eelctro-catalyst the most according to claim 1, it is characterised in that mixed solution
Microwave power in microwave reaction kettle is 180～200W, and reaction temperature is 120～180 DEG C, the response time be 5～
10min。
Membrane electrode of fuel batter with proton exchange film eelctro-catalyst the most according to claim 1, it is characterised in that described many
Unit's alcohol is the one in ethylene glycol, propylene glycol or Polyethylene Glycol；The organic solvent of described washing filter cake be dehydrated alcohol, third
One in ketone.
6. the preparation method of the membrane electrode of fuel batter with proton exchange film eelctro-catalyst described in claim 1, it is characterised in that it
Comprise the following steps:
(1), graphene oxide powder add in polyhydric alcohol, ultrasonic disperse obtains graphite oxide enolate solution, described oxidation stone
The mass volume ratio of ink alkene powder and polyhydric alcohol is 0.5～1mg:1mL；The chloroplatinic acid aqueous solution taking 0.05～0.06mol/L is put
Chloroplatinic acid in alcohol is obtained in polyhydric alcohol；Above-mentioned prepared graphite oxide enolate solution and chloroplatinic acid in alcohol are mixed, ultrasonic point
Dissipating, in mixed solution, the amount ratio of graphene oxide and chloroplatinic acid is 390～2000g:1mol；
(2), step (1) prepare mixed solution in add aqueous slkali regulation pH to 8～12, be transferred in microwave reaction kettle,
180～250W heats are to 80～180 DEG C of reactions 5～25min；Reactant liquor cools down, and vacuum filters；Filter cake is with having
The alternately washing of machine solvent and deionized water is neutral to filtrate pH, then is dried to constant weight at 60～90 DEG C, obtains with graphene oxide
For carrier, Pt/ Graphene eelctro-catalyst with Pt as active component.
The preparation method of membrane electrode of fuel batter with proton exchange film eelctro-catalyst the most according to claim 6, its feature exists
In step (1), in described graphite oxide enolate solution the amount ratio of graphene oxide powder and polyhydric alcohol be 0.6～
0.9mg:1mL.
The preparation method of membrane electrode of fuel batter with proton exchange film eelctro-catalyst the most according to claim 6, its feature exists
In step (1), described polyhydric alcohol is the one in ethylene glycol, propylene glycol or Polyethylene Glycol.
The preparation method of membrane electrode of fuel batter with proton exchange film eelctro-catalyst the most according to claim 6, its feature exists
In step (2), mixed solution microwave power in microwave reaction kettle is 180～200W, reaction temperature be 120～
180 DEG C, the response time is 5～10min.
The preparation method of membrane electrode of fuel batter with proton exchange film eelctro-catalyst the most according to claim 6, its feature exists
In step (2), the organic solvent of described washing filter cake is the one in dehydrated alcohol, acetone.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107275646A (en) * | 2017-06-16 | 2017-10-20 | 福州大学 | A kind of catalyst of fuel batter with proton exchange film of core shell structure and preparation method thereof |
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|---|---|---|---|---|
| CN102151565A (en) * | 2011-03-04 | 2011-08-17 | 南京师范大学 | Method for synthesizing PdPt/graphene nano electrical catalyst in one step by microwave process |
| CN103372429A (en) * | 2013-07-04 | 2013-10-30 | 南京大学昆山创新研究院 | Preparation method of Pt/C (platinum/carbon) catalyst for fuel cell |
| CN103894187A (en) * | 2014-03-20 | 2014-07-02 | 哈尔滨工业大学 | Preparation method of fuel cell Pt/Graphene catalyst |
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2015
- 2015-03-30 CN CN201510145774.8A patent/CN106159282A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102151565A (en) * | 2011-03-04 | 2011-08-17 | 南京师范大学 | Method for synthesizing PdPt/graphene nano electrical catalyst in one step by microwave process |
| CN103372429A (en) * | 2013-07-04 | 2013-10-30 | 南京大学昆山创新研究院 | Preparation method of Pt/C (platinum/carbon) catalyst for fuel cell |
| CN103894187A (en) * | 2014-03-20 | 2014-07-02 | 哈尔滨工业大学 | Preparation method of fuel cell Pt/Graphene catalyst |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107275646A (en) * | 2017-06-16 | 2017-10-20 | 福州大学 | A kind of catalyst of fuel batter with proton exchange film of core shell structure and preparation method thereof |
| CN107275646B (en) * | 2017-06-16 | 2020-03-10 | 福州大学 | Proton exchange membrane fuel cell catalyst with core-shell structure and preparation method thereof |
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Application publication date: 20161123 |