CN104525272B - Preparation method of anode catalyst special for direct alcohol fuel cell - Google Patents
Preparation method of anode catalyst special for direct alcohol fuel cell Download PDFInfo
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- CN104525272B CN104525272B CN201410812332.XA CN201410812332A CN104525272B CN 104525272 B CN104525272 B CN 104525272B CN 201410812332 A CN201410812332 A CN 201410812332A CN 104525272 B CN104525272 B CN 104525272B
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- anode catalyst
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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 of an anode catalyst special for a direct alcohol fuel cell. The method comprises the following steps: by taking graphene as an anode catalyst carrier, dissolving the carrier in a solvent, performing ultrasonic treatment for 30-45 minutes, magnetically stirring for 1-2 hours, adding a high polymer material, and regulating the concentration of a spinning solution, adding one or two metal compounds, controlling the metal atom ratio, stirring and performing reflux condensation at the temperature of 60 DEG C for 3 hours, thereby obtaining an electro-spinning solution; spinning by utilizing an electrostatic spinning technology, performing pre-oxidation and carbonization treatment on the spun film, and finally obtaining the anode catalyst film. The method disclosed by the invention has the advantages that according to the preparation method of the anode catalyst special for the direct alcohol fuel cell disclosed by the invention, the appearance structure of the prepared anode catalyst is film-shaped, the traditional powdery structure is simplified, and the step of preparing a catalytic layer by using a complex coating in the traditional process is simplified. Compared with the conventional anode catalyst for the fuel cell, the anode catalyst disclosed by the invention has obvious advantages, and the battery assembly is simplified.
Description
Technical field
The present invention relates to a kind of preparation method of direct alcohol fuel cell special anode catalyst, belongs to fuel cell and urges
Agent field.
Background technology
Fuel cell (Fuel Cell) is that a kind of fuel that will be present in is converted into electric energy with the chemical energy in oxidant
TRT.Fuel and air are fed separately to fuel cell, and electricity is just rumly produced.It exteriorly has positive and negative
Pole and electrolyte etc., as a battery, but substantially it can not " storing up electricity " but one " power plant ".Fuel cell is with height
The features such as effect, environmental friendliness, is described as the new forms of energy of 21 century, and it is that one kind causes fuel and oxidant in the presence of electrolyte
Between reaction TRT.When battery operated, negative pole is continuously input into fuel, oxidation reaction occurs, and continuously supplies in positive pole
Oxygen supply agent（Oxygen or air）Shi Fasheng reduction reactions.As long as reactant is continually entered in principle, and constantly discharges reaction product
Thing, fuel cell just continuously can generate electricity.
Direct alcohol fuel cell（DAFC）Appearance, a big chunk reason is alcohols abundance, cheap, is deposited
Storage, it is easy to carry, become the focus of research in recent years.But direct alcohol fuel cell（DAFC）Development additionally depend on it is complete to alcohol
The oxidized research and development with high catalytic activity and the elctro-catalyst of high selectivity, therefore, both at home and abroad mainly around raising catalyst
Performance is studied of both expanding.
First aspect：The selection of catalyst carrier.So far, platinum is the best catalysis of generally acknowledged pure electrochemical oxidation
Agent, but the intermediate product of alcohols electrochemical oxidation is easily absorbing on platinum electrode, makes catalyst poisoning, causes catalytic performance very
It is fast to fail.Also platinum expensive, scarcity of resources, improves the cost of fuel cell, ultimately limit the wide of fuel cell
General application.The development of carbon supported platinum catalyst, makes catalyst particle high degree of dispersion, stablizes, substantially increase catalyst platinum utilization,
And strengthen its catalysis activity, it is easy to platinum to recycle.On this basis, researcher is urged in fuel cell to other material with carbon elements
The application in agent field has been also carried out studying and has explored.Graphene becomes one of study hotspot both domestic and external as new material,
Compared with other material with carbon elements, it has higher mechanical strength, bigger theoretical specific surface area；The distribution of electrochemical site is more
It is homogeneous；With extraordinary thermal conductivity and conductance property, catalyst nano-particles can have both been improved in its table as catalyst carrier
The decentralization in face, while also causing motor and electrolyte to have bigger contact area, is conducive to the carrying out of electrochemical reaction, so as to
Improve catalyst catalytic performance.Occur with Graphene as carrier at present or be prepared as carrier with carbon fiber-based merely urging
The method of agent.
Second aspect：The preparation method of catalyst.General, researcher is by improving the method that tradition prepares catalyst
The activity of catalyst is improved, the catalysis activity of catalyst is subject to noble metal method, metallic catalyst composition, catalyst carrier
Affect etc. several factors.Infusion process is a kind of very traditional common method for preparing noble metal catalyst, Shawn D.Lin etc.
<<Journal of Physical Chemistry B>>The 1st phase " Morphology of cabon of volume 103 in 1999
supported Pt-Ru electrocatalyst and the CO tolerance of anodes for PEM fuel
Introduce during cells " is literary and hydrogen reducing is used at 250 DEG C or so, operate comparatively laborious, metal particle diameter wider range, and there is peace
Full hidden danger.Chemical reduction method is another kind of preparation method for using more support type Pt and Pt multicomponent catalyst, is being prepared
In catalyst process, the formation of metal be in the liquid phase with carry out in carrier surface, the metal crystal nuclei shape on carrier surface at random
Into and grow up to form catalyst granules, cause gained catalyst distribution of particles it is uneven, in addition it is also necessary to substantial amounts of solvent and
Excessive reducing agent, not only increases the cost of post processing, and also results in environmental pollution.
The content of the invention
Present invention aims to deficiency of the prior art, there is provided a kind of direct alcohol fuel cell special anode
The preparation method of catalyst, so as to the catalysis activity and stability that simplify preparation technology flow process, improve catalyst.
To solve above-mentioned technical problem, the technical solution used in the present invention is：A kind of direct alcohol fuel cell anode is special
With the preparation method of catalyst, its innovative point is：By the use of Graphene as the carrier material of catalyst, add metal compound
Thing, under the action of the solvent, hybrid reaction forms electrospinning liquid, has been additionally added macromolecular material, with Graphene in the electrospinning liquid
Mix with metallic compound, it is ensured that electrospinning liquid concentration range is 5-21wt%；The addition of the macromolecular material is 2～3wt%,
Electrostatic spinning technique is recycled to prepare the direct alcohol fuel cell anode catalyst with membrane structure；The Graphene and gold
Category compound is 1 in mass ratio：10～5：17.
Further, the macromolecular material is any one in polyacrylonitrile or Nafion liquid.
Further, the metallic compound be chloroplatinic acid, stannic chloride pentahydrate, the chloroplatinic acid and other two in lead acetate
The composition of any one combination in kind metallic compound or more three kinds of metallic compounds.
Further, when the metallic compound selects the metallic compound of two or three metal composites, control gold
The atomic ratio of category is Pt：Sn or Pt：Pb=（1：1）~（3：1）, Pt：Pb：Sn=（1：1：1）~（3：3：1）.
Further, the solvent is any one in ethylene glycol solution or DMF solution.
Further, the electrospinning liquid is prepared by the way of heating in water bath for reaction, is comprised the following steps that：
（1）Graphene, 30～40min of ultrasonic disperse, by mixed solution 2～3h of magnetic agitation are added in solvent solution；
（2）The macromolecular material of 2～3wt% amounts is added, is continued magnetic agitation, until completely dissolved, is added metal compound
Thing, is placed on magnetic stirrer and continues stirring heating water bath, control bath temperature for 60～100 DEG C, electricity is obtained after 2～3h
Spin liquid.
Beneficial effects of the present invention are as follows：
（1）The preparation method of the direct alcohol fuel cell special anode catalyst of the present invention, the anode for preparing are urged
The contour structures of agent are membranaceous, simplify traditional floury structure, prepared by complicated coating in simplifying traditional handicraft
The step of Catalytic Layer, there is clear advantage with conventional fuel battery anode catalyst, easy battery assembling.
（2）The preparation method of the direct alcohol fuel cell anode special-purpose catalyst of the present invention, changes in the past fine using carbon
The combination of dimension, graphitization additive and metallic particles, directly with Graphene as catalyst carrier, adds metallic compound, passes through
Specific operation and step, are greatly improved activity, stability and the anti-poisoning capability of catalyst oxidation alcohol.
（3）The preparation method of the direct alcohol fuel cell anode special-purpose catalyst of the present invention, using conventional electrostatic spinning
Technology is prepared in catalyst process, and water-bath mode is adopted when prepared by electrospinning liquid, and reaction temperature is relatively low, and the reaction time is short, behaviour
Make easy, reducing agent recycling, energy-conservation environmental protection again.
（4）The preparation method of the direct alcohol fuel cell anode special-purpose catalyst of the present invention, using electrostatic spinning skill
On the basis of art prepares anode catalyst, directly anode catalyst is modified and is modified using Graphene.Break through tradition
The anode catalyst with Graphene as carrier preparation method, prepared with membrane structure using electrostatic spinning technique with stone
Anode catalyst of the black alkene for carrier.
Specific embodiment
Technical scheme is elaborated with reference to specific embodiment.
Embodiment 1
Without the preparation method of macromolecular material：
25mg Graphenes are weighed, is added in the ethylene glycol solution of 13.5ml, ultrasonic disperse 30min is added thereto to
The chloroplatinic acid of 96mg, is placed on magnetic stirrer and stirs to whole dissolvings, that is, obtain electrospun solution.
Electrospinning liquid is loaded into electrostatic spinning apparatus, technological parameter is set, spinning is carried out, the film for obtaining is placed in vacuum drying
Case, is dried 12h, finally gives anode catalyst Pt/Gr.
The solution concentration of the present embodiment is too small, it is impossible to spin silk, and solution is projected in pearl.
Embodiment 2
Addition macromolecular material forms the preparation method of Graphene 0.3wt%：
The PAN for taking 0.68g is dissolved in 7.5gN, dinethylformamide solution（DMF）In, condensing reflux stirring in water bath
3h, bath temperature obtain the colloidal sol clarified at 90 DEG C.The chloroplatinic acid of 48mg is added after stirring cooling, is placed on magnetic stirrer
2h is to whole dissolvings for stirring.25mg graphene powders are added in mixed solution again, continues ultrasonic vibration 1h, you can make Graphene
Powder is dispersed in spinning solution.Electrostatic spinning technique is recycled, the carbon fiber-based anode that Graphene was modified is finally given
Catalyst.
Embodiment 3
Addition macromolecular material forms the preparation method of Graphene 0.2wt%：
The PAN for taking 0.5g is dissolved in 7.5gN, dinethylformamide solution（DMF）In, condensing reflux stirring in water bath 4h,
Bath temperature obtains the colloidal sol clarified at 90 DEG C.The chloroplatinic acid of 34mg is added after stirring cooling, is placed on magnetic stirrer and is stirred
2h is to whole dissolvings.20mg graphene powders are added in mixed solution again, continues ultrasonic vibration 30min, you can make Graphene
Powder is dispersed in spinning solution.Conventional electrostatic spinning technique is recycled, the carbon fiber-based that Graphene was modified is finally given
Anode catalyst.
Embodiment 4
Addition macromolecular material forms the preparation method of Graphene 0.1wt%：
The PAN for taking 1g is dissolved in 15gN, dinethylformamide solution（DMF）In, condensing reflux stirring in water bath 3h, water
Bath temperature obtains the colloidal sol clarified at 90 DEG C.Stirring cooling after add 96mg chloroplatinic acid, be placed on magnetic stirrer stir to
All dissolve.20mg graphene powders are added in mixed solution again, continues ultrasonic vibration 30min, you can make graphene powder
It is dispersed in spinning solution.Conventional electrostatic spinning technique is recycled, the carbon fiber-based anode that Graphene was modified is finally given
Catalyst.
The anode catalyst of embodiment 2～4 is in spinning process：
（1）Spinning phenomenon is good.
（2）SEM is tested：100～600nm of radius, mean radius 450nm.
（3）XRD analysis：As the addition of Graphene, diffraction peak intensity are reduced, degree of crystallinity declines, the addition of Graphene
For mass fraction 0.1% when, best results.
Embodiment 5
Addition macromolecular material ensures preparation method of the macromolecular material weight ratio for PAN 3wt%：
30mg Graphenes are weighed, is added in the DMF of 15g, ultrasonic disperse 30min, then magnetic agitation is carried out, add after 2h again
Enter the polyacrylonitrile of 0.5g, after magnetic agitation 2h, add 96mg chloroplatinic acids, mixed solution condensing reflux 2h to be stirred at 60 DEG C and obtained
Electrospun solution.Electrospinning liquid loads electrostatic spinning apparatus, arranges technological parameter, carries out spinning, and the film for obtaining is placed in vacuum drying chamber,
It is dried 12h.The product for obtaining is cut into appropriately sized, is laid in crucible, be placed in vacuum tube furnace and heat, product is carried out
Conventional pre-oxidation and carbonization treatment, finally give anode catalyst Pt/Gr.
The macromolecular material of above-mentioned adjustable solution concentration is not limited only to polyacrylonitrile macromolecular material, can also be 5wt%
Nafion liquid.
Embodiment 6
Addition macromolecular material ensures preparation method of the macromolecular material weight ratio for PAN 2wt%：
20mg Graphenes are weighed, is added in the DMF of 10g, ultrasonic disperse 30min, then magnetic agitation is carried out, add after 1h again
Enter the PAN of 0.2g, after magnetic agitation 2h, add 100mg chloroplatinic acids, mixed solution condensing reflux 1h to be stirred at 60 DEG C and obtain electrospinning
Solution.Electrospinning liquid loads electrostatic spinning apparatus, arranges technological parameter, carries out spinning, and the film for obtaining is placed in vacuum drying chamber, is dried
12h.The product for obtaining is cut into appropriately sized, is laid in crucible, be placed in vacuum tube furnace and heat, routine is carried out to product
Pre-oxidation and carbonization treatment, finally give anode catalyst Pt/Gr.
Embodiment 7
Addition macromolecular material ensures preparation method of the macromolecular material weight ratio for PAN2.5wt%：
20mg Graphenes are weighed, is added in the DMF of 10g, ultrasonic disperse 30min, then magnetic agitation is carried out, add after 1h again
Enter the PAN of 0.259g, after magnetic agitation 1h, add 100mg chloroplatinic acids, mixed solution condensing reflux 1h to be stirred at 60 DEG C and obtain electricity
Spin solution.Electrospinning liquid loads electrostatic spinning apparatus, arranges technological parameter, carries out spinning, and the film for obtaining is placed in vacuum drying chamber, does
Dry 12h.The product for obtaining is cut into appropriately sized, is laid in crucible, be placed in vacuum tube furnace and heat, product is carried out often
Rule pre-oxidation and carbonization treatment, finally give anode catalyst Pt/Gr.
The anode catalyst spinning effect of embodiment 5～7 is as shown in table 1 below：
| Embodiment 5 | PAN 3wt% | During electrostatic spinning, present and float cotton-shaped, effect is relatively good. |
| Embodiment 6 | PAN 2wt% | Concentration is too small, it is impossible to spin silk, water-drop sputtering. |
| Embodiment 7 | PAN 2.5wt% | Moderate concentration, fibre diameter are thinner, substantially all in below 300nm. |
Conclusion：For the technical process that can reduce pre-oxidation and be carbonized, the content of PAN is reduced as far as possible, minimum content is
2.5%。
Embodiment 8
Metallic compound selects the preparation method of the metal mixture of stannic chloride pentahydrate and chloroplatinic acid：
20mg Graphenes are weighed, is added in the DMF of 15g, ultrasonic disperse 45min；Add appropriate SnCl4.5H2O, magnetic
Power stirs 2h, adds chloroplatinic acid after fully dissolving, and makes Pt/Sn atomic ratios for 3, then by 110 DEG C under nitrogen atmosphere of mixed solution
Stirring condensing reflux 3h；Again by mixed liquor 30～45min of ultrasonic disperse, electrospun solution is obtained.Electrospinning liquid loads electrostatic spinning dress
Put, technological parameter is set, spinning is carried out, the film for obtaining is placed in vacuum drying chamber, is dried 24h, product is pre-oxidized and carbon
Change is processed, and finally gives anode catalyst PtSn/Gr.
The spun fiber surface of the present embodiment is smooth, and even thickness, average diameter reach 200nm.
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel it should be appreciated that the present invention is not restricted to the described embodiments, the simply explanation described in above-described embodiment and specification this
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, these changes
Change and improvement is both fallen within scope of the claimed invention.The claimed scope of the invention by appending claims and its
Equivalent thereof.
Claims (5)
1. a kind of preparation method of direct alcohol fuel cell special anode catalyst, it is characterised in that：By the use of Graphene as
The carrier material of catalyst, adds metallic compound, and under the action of the solvent, hybrid reaction forms electrospinning liquid, the electrospinning liquid
In be additionally added macromolecular material, mix with Graphene and metallic compound, it is ensured that electrospinning liquid concentration range be 5～21wt%；It is described
The addition of macromolecular material is 2～3wt%, recycles electrostatic spinning technique to prepare the direct Aalcohols fuel with membrane structure
Cell anode catalyst；The Graphene and metallic compound are 1～10 5～17 in mass ratio;
Above-mentioned metallic compound is chloroplatinic acid, stannic chloride pentahydrate, the chloroplatinic acid in lead acetate and other two kinds of metallic compounds
In any one combination or more three kinds of metallic compounds composition.
2. the preparation method of direct alcohol fuel cell special anode catalyst according to claim 1, it is characterised in that：
The macromolecular material is any one in polyacrylonitrile or Nafion liquid.
3. the preparation method of direct alcohol fuel cell special anode catalyst according to claim 1, it is characterised in that：
When the metallic compound selects the metallic compound of two or three metal composites, the atomic ratio for controlling metal is Pt Sn
Or Pt Pb=1 3～1, Pt Pb Sn=1 1 1～3 31.
4. the preparation method of direct alcohol fuel cell special anode catalyst according to claim 1, it is characterised in that：
The solvent is any one in ethylene glycol solution or N,N-dimethylformamide solution.
5. the preparation method of direct alcohol fuel cell special anode catalyst according to claim 1, it is characterised in that：
The electrospinning liquid is prepared by the way of heating in water bath for reaction, is comprised the following steps that：
(1) Graphene, 30～40min of ultrasonic disperse, by mixed solution 2～3h of magnetic agitation are added in solvent solution；
(2) macromolecular material of 2～3wt% amounts is added, is continued magnetic agitation, until completely dissolved, is added metallic compound,
Be placed on magnetic stirrer and continue stirring heating water bath, bath temperature is controlled for 60～100 DEG C, electrospinning is obtained after 2～3h
Liquid.
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| US20170200940A1 (en) * | 2016-01-12 | 2017-07-13 | Hk Graphene Technology Corporation | Nannoparticle/porous graphene composite, synthesizing methods and applications of same |
| CN107673307A (en) * | 2016-08-01 | 2018-02-09 | 福建新峰二维材料科技有限公司 | Germanium/graphene/titanium dioxide nanofiber composite material and preparation method thereof and battery |
| CN106784894A (en) * | 2016-12-26 | 2017-05-31 | 南通大学 | A kind of method for preparing the graphene-based anode electrocatalyst of direct alcohol fuel cell |
| CN106784874A (en) * | 2016-12-26 | 2017-05-31 | 南通大学 | A kind of method for preparing direct alcohol fuel cell anode electrocatalyst |
| CN110112424B (en) * | 2019-04-18 | 2022-05-03 | 电子科技大学 | Anode of ethanol fuel cell and preparation method thereof |
| CN112701300A (en) * | 2019-10-23 | 2021-04-23 | 中国科学院大连化学物理研究所 | High-stability carbon skeleton nanofiber membrane electrode and preparation method and application thereof |
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| CN101733094B (en) * | 2009-12-14 | 2012-01-25 | 浙江大学 | Pt-CeO2/graphene electro-catalyst and preparation method thereof |
| CN102054990A (en) * | 2010-12-06 | 2011-05-11 | 常熟理工学院 | Method for preparing nano electro-catalyst for anode of ethanol fuel cell |
| US9388513B2 (en) * | 2011-07-01 | 2016-07-12 | The University Of Kentucky Research Foundation | Crystallographically-oriented carbon nanotubes grown on few-layer graphene films |
| KR20130015719A (en) * | 2011-08-04 | 2013-02-14 | 연세대학교 산학협력단 | A complex comprising a mesoporous silicon oxide and a graphene, and method for preparing the same |
| CN103227334B (en) * | 2013-04-03 | 2015-05-20 | 上海交通大学 | Carbon-containing metal catalyst, preparation method and application thereof |
| CN103441287B (en) * | 2013-08-09 | 2016-06-01 | 中国科学院上海高等研究院 | The preparation method of a kind of direct methanol fuel cell membrane electrode |
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