CN104332641A - Preparation method of composite bipolar plate - Google Patents
Preparation method of composite bipolar plate Download PDFInfo
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- CN104332641A CN104332641A CN201410432555.3A CN201410432555A CN104332641A CN 104332641 A CN104332641 A CN 104332641A CN 201410432555 A CN201410432555 A CN 201410432555A CN 104332641 A CN104332641 A CN 104332641A
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/18—Regenerative fuel cells, e.g. redox flow batteries or secondary fuel cells
- H01M8/184—Regeneration by electrochemical means
- H01M8/188—Regeneration by electrochemical means by recharging of redox couples containing fluids; Redox flow type batteries
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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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Abstract
The invention relates to a preparation method of a composite bipolar plate. The preparation method comprises the following steps: preparing a matrix polymer, a conductive filling material, and a compatilizer, wherein the compatilizer comprises inorganic groups and organic groups; mixing the matrix polymer, conductive filling material, and compatilizer so as to obtain a mixture; and finally moulding the mixture so as to obtain the composite bipolar plate.
Description
Technical field
The present invention relates to a kind of preparation method of bipolar plates, particularly relate to a kind of preparation of composite dual-electrode plates used for all-vanadium redox flow battery.
Background technology
Vanadium redox battery (VFB) is a kind of emerging large-scale energy-storage system, is also that a kind of efficient, environmental protection and Large Copacity can the energy-storage batteries of degree of depth discharge and recharge.VFB not only as the supporting energy storage device of the electricity generation system of the regenerative resource such as solar energy, wind energy, and as the peak adjusting device of electrical network, can improve transmission of electricity quality, ensures power grid security.VFB is using the vanadium ion solution of different valence state as the active material of positive pole and negative pole, and positive active material is V
+ 4/ V
+ 5electricity is right, and negative electrode active material is V
+ 2/ V
+ 3electricity is to being stored in respective electrolyte storage tank respectively, by external pump, electrolyte is pumped in cell stack, it is made to circulate in the closed-loop path of different fluid reservoirs and half-cell, adopt amberplex as the barrier film of battery pack, electrolyte is parallel to be flow through electrode surface and electrochemical reaction occurs, and is collected and conduction current by bipolar plates, makes storage chemical energy in the electrolytic solution convert electric energy to.This reversible course of reaction makes VFB can complete charging, discharges and recharge.
Conductive bipolar plate, as one of the critical piece of VFB, has and collects the electric current that electrochemical reaction produces and the effect of separating both positive and negative polarity electrolyte.In VFB, electrolyte is generally the sulfuric acid solution of vanadium ion, has very strong corrosivity; Meanwhile, V
5+have stronger oxidizability, therefore, bipolar plates, except need having good conductivity, also must have enough strong chemically-resistant and electrochemical corrosion.Composite dual-electrode plates be a kind of by conductive carbon material as conductive filler and the macromolecular material bipolar plates as matrix.Composite dual-electrode plates is than the good corrosion resistance of metal double polar plates, compared with pure graphite bi-polar plate, composite dual-electrode plates preparation technology is simple, and cost is lower, conductive filler can be helped the adding of macromolecular material to form conductive network skeleton, and improve the resistance to compression of bipolar plates, bending resistance and decay resistance.
But, the dispersiveness of the material with carbon element in composite dual-electrode plates of the prior art is poor, and between material with carbon element and macromolecular material in conjunction with price differential, thus the active oxygen atom that VFB produces in electrochemical reaction process is easy to corrode material with carbon element, thus cause the loss of material with carbon element, and then reduce the electric conductivity of bipolar plates and the decay resistance of VFB.
Summary of the invention
In view of this, necessaryly a kind of conductivity is provided and all good composite dual-electrode plates of corrosion resistance.
A preparation method for composite dual-electrode plates, comprises the following steps: provide matrix polymer, conductive filler and compatilizer, and described compatilizer has inorganic group and organic group simultaneously; Mix this matrix polymer, conductive filler and compatilizer and form a mixture, and with this mixture for material forming is formed described composite dual-electrode plates.
Compared with prior art, the embodiment of the present invention utilizes the compatilizer simultaneously with described inorganic group and organic group to come to mix with matrix polymer and conductive filler to prepare described composite dual-electrode plates, effectively improve the compatibility of described conductive filler and described matrix polymer, thus improve the dispersiveness of described conductive filler in described matrix polymer and and described matrix polymer between adhesion, and then improve the electric conductivity of this composite dual-electrode plates, decay resistance and the mechanical performance such as stretching, impact strength.
Embodiment
The preparation method of the composite dual-electrode plates of the embodiment of the present invention will be described in detail below.
The embodiment of the present invention provides a kind of preparation method of composite dual-electrode plates, comprises the following steps:
S1, provides matrix polymer, conductive filler and compatilizer, and described compatilizer has inorganic group and organic group simultaneously;
S2, mixes this matrix polymer, conductive filler and compatilizer and forms a mixture, and
S3, with this mixture for material forming is formed described composite dual-electrode plates.
In above-mentioned steps S1, the effect of described matrix polymer is the bearing substrate as described conductive filler.Preferably, described matrix polymer is thermoplastic resin, described matrix polymer can for but be not limited in polyethylene (PE), polypropylene (PP), polyvinyl chloride (PVC), polystyrene (PS) and acrylonitrile-butadiene-styrene copolymer (ABS) one or more.
Described conductive filler is inorganic conductive filler, is preferably material with carbon element, and this conductive filler can be, but not limited to one or more in graphite, carbon black, MCMB, carbon fiber, carbon nano-tube and Graphene.
Described compatilizer has inorganic group and organic group simultaneously, thus can effectively improve inorganic described conductive filler and organically between matrix polymer interface performance to improve compatibility or the dispersiveness of described conductive filler in this matrix polymer.Effectively can improve the adhesion between described conductive filler and described matrix polymer in addition.Described compatilizer can be maleic anhydride grafted polymer.Preferably, described compatilizer is maleic anhydride grafted polymer.This maleic anhydride grafted polymer has stronger polar reaction group, greatly can improve the dispersiveness of compatibility between base polymer and inorganic conductive material and conductive filler, and active oxygen atom owing to producing in electrochemical reaction process can be reduced and corrode material with carbon element, thus the mechanical strength of the composite dual-electrode plates of follow-up formation, hot strength and impact strength can be improved.In addition, while realizing described conductive filler high filler loading capacity, make described mixture have good rheological performance, thus reach the object of conductivity, corrosion resistance and the mechanical strength improving composite dual-electrode plates.
Described maleic anhydride grafted polymer is that maleic anhydride monomer graft polymers group is formed.This maleic anhydride grafted polymer can for but be not limited in maleic anhydride grafted polyethylene (PE-g-MAH), maleic anhydride inoculated polypropylene (PP-g-MAH), maleic anhydride graft polyvinyl chloride (PVC-g-MAH), maleic anhydride grafted polystyrene (PS-g-MAH) and maleic anhydride grafted acrylonitrile-butadiene-styrene copolymer (ABS-g-MAH) one or more.Preferably, described polymeric groups is identical with the material of described matrix polymer, thus increases the compatibility between matrix polymer, conductive filler and maleic anhydride grafted polymer, the dispersiveness of described conductive filler and the adhesion with described matrix polymer further.Such as, when described matrix polymer is PE, described maleic anhydride grafted polymer is PE-g-MAH, when described matrix polymer is PP, described maleic anhydride grafted polymer is PP-g-MAH, and when described matrix polymer is PVC, described maleic anhydride grafted polymer is PVC-g-MAH.When described matrix polymer is PS, described maleic anhydride grafted polymer is PS-g-MAH, and when described matrix polymer is ABS, described maleic anhydride grafted polymer is ABS-g-MAH.
Mass ratio between described matrix polymer, conductive filler and compatilizer can be (10%-30%): (50%-70%): (10%-40%).Preferably, described mass ratio can be 10%:80%:10%.
In above-mentioned steps S2, as long as the mode of described mixing is not limit can make Homogeneous phase mixing between described matrix polymer, conductive filler and compatilizer.Preferably, the mode by stirring makes Homogeneous phase mixing between described matrix polymer, conductive filler and compatilizer.The speed of described stirring can be 600 revs/min to 1000 revs/min.Preferably, the speed of described stirring can be 800 revs/min.The uniformity coefficient mixed between matrix polymer, conductive filler and compatilizer in mixture described in the basis of time of described stirring is determined, preferably, the time of described stirring is greater than 20 minutes.In the process of described mixing, due to the existence of described compatilizer, thus make to be connected by chemical bond between described conductive filler with described matrix polymer.
In above-mentioned steps S3, described shaping mode can be compression molding or roll-forming.Described compression molding specifically comprises the following steps:
S31, forms composite material by described mixture extrusion molding, and this Laminated Shear Deformable is become pellet, and
S32, is placed in the described composite dual-electrode plates of the compressing formation of mould by described pellet.
Described roll-forming specifically comprises the following steps:
S31 ', forms described composite material by described mixture extrusion molding, and
S32 ', the direct roll-forming of the composite material this extruded forms described composite dual-electrode plates.
In above-mentioned steps S31 and S31 ', described mixture can carry out extrusion molding in an extrusion device.Described extrusion device can be the one in single screw extrusion machine, double screw extruder, mill and banbury.The embodiment of the present invention adopts double screw extruder to carry out extrusion molding to described mixture.The temperature-controllable of described extrusion molding built in 190 DEG C within the scope of 260 DEG C.The rotating speed of screw rod in described screw extruder in described mixture extrusion molding process is 200 revs/min to 300 revs/min.
Above-mentioned steps S31 can comprise further:
S311, pellet described in Homogeneous phase mixing;
S312, by the extrusion molding formation secondary composite material again of the pellet after Homogeneous phase mixing, and becomes secondary pellet by this secondary Laminated Shear Deformable, and
S313, repeats above-mentioned steps S311-S312.
Described conductive filler and the dispersed and described pellet that is each other good bonding strength of matrix polymer can be obtained by above-mentioned steps S311-313, thus conductive filler can be made in the composite dual-electrode plates of follow-up formation dispersed and have stronger adhesion for described matrix polymer in described matrix polymer.
In above-mentioned steps S32, described compressing mode is preferably hot-forming.Described mould has the shape of bipolar plates.Describedly hot-formingly to come by a hot press.Described hot-forming temperature can be 190 DEG C to 260 DEG C.Described hot-forming pressure controllable is built in 10Mpa to 30Mpa.The described hot-forming time can be controlled in 10 minutes to 60 minutes.
Above-mentioned preparation method can comprise further shaping described in a pair after composite dual-electrode plates surface carry out the step of blasting treatment.
The process of described blasting treatment is that material spray high velocity jet is surperficial to described composite dual-electrode plates, makes the surface of described composite dual-electrode plates produce frosted finish effect.By can improve the surface area of this bipolar plates to the process of described composite dual-electrode plates surface sand-blasting, thus after assembled battery, just can increase the contact area of this bipolar plates and electrode surface with less assembly force, thus the contact resistance between electrode can be reduced.Because battery can adopt the assembly force between less electrode and bipolar plates when assembling, thus effectively can avoid the change that the pore structure of electrode occurs, and then avoid cause electrolyte in hole due to the change of the pore structure of electrode resistance to mass tranfer increase, concentration polarization.
Described blasting treatment can adopt dry abrasive blasting technique also can adopt vapour blasting technique.Dry abrasive blasting technique is adopted to carry out blasting treatment to described bipolar plate surfaces in the embodiment of the present invention.Described material spray can for but be not limited in white fused alumina sand, resin sand and glass sand one or more.
In the composite dual-electrode plates that the embodiment of the present invention is prepared by said method, described conductive filler is dispersed in described matrix polymer, and due to the inorganic group of described compatilizer and the effect of organic group, be connected by chemical bond between described conductive filler with described matrix polymer, thus the adhesion that improve between them, and form conductive network.When described composite dual-electrode plates is after described frosted process, this composite dual-electrode plates has the surface of frosted.
The embodiment of the present invention utilizes the compatilizer simultaneously with described inorganic group and organic group to come to mix with matrix polymer and conductive filler to prepare described composite dual-electrode plates, effectively improve the compatibility of described conductive filler and described matrix polymer, thus improve the dispersiveness of described conductive filler in described matrix polymer and and described matrix polymer between adhesion, and then improve the electric conductivity of this composite dual-electrode plates, decay resistance and the mechanical performance such as stretching, impact strength.
Embodiment 1
(1) PE-g-MAH of the PE resin of 30g, 210g conductive carbon black, 60g is put in high mixer, mixing speed 800r/min, stir 30min, fully mix formation one mixture.
(2) described mixture is injected double screw extruder and carry out extrusion molding, the temperature of described extrusion molding controls at 190 DEG C ~ 220 DEG C, and screw speed is 40r/min ~ 80r/min, extrudes pellet.
(3) described pellet is dropped into described high mixer again, mixing speed 800r/min, stir 20min, re-inject described double screw extruder afterwards and again carry out extrusion molding, the temperature of extrusion molding controls at 190 DEG C, screw speed is 200r/min, extrudes pellet, repeats this operation twice.
(4) pellet that produces after above-mentioned repeatedly mixing and extrusion molding is put in hot pressing die, then by this hot pressing die as hot-forming on hot press, hot press temperature control 190 DEG C, Stress control at 10MPa, hot pressing time 30min.
(5) take out bipolar plates by after described hot pressing die cooling, adopt dry abrasive blasting technique to carry out blasting treatment to bipolar plate surfaces, select hardness 4, bulk density 0.93g/cm
3, granularity is the resin sand of 0.1mm to 0.2mm, uses air pressure sand-blasting machine, compressed air pressure control 0.1Mpa to 0.2Mpa.
Surface after testing, the specific insulation of described bipolar plates prepared by the present embodiment 1 is: 1 Ω cm.As all-vanadium flow battery both positive and negative polarity collector plate, battery charging and discharging performance parameter is: coulombic efficiency 96%, energy efficiency 83.5%, voltage efficiency 87%.
Embodiment 2
(1) PP-g-MAH of the PP resin of 60g, 150g graphite, 90g is put in high mixer, mixing speed 800r/min, stir 30min, fully mix formation mixture.
(2) described mixture is injected double screw extruder and carry out extrusion molding, the temperature of described extrusion molding controls at 200 DEG C, and screw speed is 250r/min, extrudes pellet.
(3) described pellet is dropped into high mixer again, mixing speed 800r/min, stir 20min, inject double screw extruder afterwards, the temperature of extrusion molding controls at 200 DEG C, and screw speed is 250r/min, repeats this operation twice.
(4) described pellet is put in hot pressing die, by described hot pressing die as hot-forming on hot press, hot press temperature control 200 DEG C, Stress control at 15MPa, hot pressing time 30min.
(5) take out bipolar plates by after described hot pressing die cooling, adopt dry abrasive blasting technique to carry out blasting treatment to this bipolar plate surfaces, select Mohs' hardness 9, bulk density 1.6g/cm
3, granularity is the white fused alumina sand of 0.1mm to 0.2mm, uses air pressure sand-blasting machine, compressed air pressure control 0.1Mpa to 0.2Mpa.
Surface after testing, the specific insulation of described bipolar plates prepared by embodiment 2 is: 1 Ω cm.As all-vanadium flow battery both positive and negative polarity collector plate, battery charging and discharging performance parameter is: coulombic efficiency 94%, energy efficiency 84%, voltage efficiency 89%.
Embodiment 3
(1) ABS-g-MAH of the ABS resin of 60g, 180g Graphene, 60g is put in high mixer, mixing speed 800r/min, stir 30min, fully mix formation mixture.
(2) described mixture is injected double screw extruder and carry out extrusion molding, the temperature of extrusion molding controls at 200 DEG C, and screw speed is 200r/min, extrudes pellet.
(3) described pellet is dropped into high mixer again, mixing speed 800r/min, stir 20min, inject double screw extruder afterwards, the temperature of extrusion molding controls at 200 DEG C, and screw speed is 250r/min, repeats this operation twice.
(4) described pellet is put in hot pressing die, by described mold heat as hot-forming on hot press, hot press temperature control 200 DEG C, Stress control at 15MPa, hot pressing time 30min.
(5) take out bipolar plates by after described hot pressing die cooling, adopt dry abrasive blasting technique to carry out blasting treatment to bipolar plate surfaces, select hardness 6-7, bulk density 1.5g/cm
3, granularity is the glass sand of 0.1mm to 0.2mm, uses air pressure sand-blasting machine, compressed air pressure control 0.1Mpa to 0.2Mpa.
Show after testing, the specific insulation of bipolar plates prepared by embodiment 3 is: 1 Ω cm.As all-vanadium flow battery both positive and negative polarity collector plate, battery charging and discharging performance parameter is: coulombic efficiency 96%, energy efficiency 85%, voltage efficiency 89%.
In addition, those skilled in the art can also do other change in spirit of the present invention, and certainly, these changes done according to the present invention's spirit, all should be included within the present invention's scope required for protection.
Claims (12)
1. a preparation method for composite dual-electrode plates, comprises the following steps:
There is provided matrix polymer, conductive filler and compatilizer, described compatilizer has inorganic group and organic group simultaneously;
Mix this matrix polymer, conductive filler and compatilizer and form a mixture, and
With this mixture for material forming is formed described composite dual-electrode plates.
2. the preparation method of composite dual-electrode plates as claimed in claim 1, it is characterized in that, described compatilizer is maleic anhydride grafted polymer.
3. the preparation method of composite dual-electrode plates as claimed in claim 2, it is characterized in that, maleic anhydride grafted polymer is one or more in maleic anhydride grafted polyethylene, maleic anhydride inoculated polypropylene, maleic anhydride graft polyvinyl chloride, maleic anhydride grafted polystyrene and maleic anhydride grafted acrylonitrile-butadiene-styrene copolymer.
4. the preparation method of composite dual-electrode plates as claimed in claim 2, is characterized in that, described maleic anhydride grafted polymer is that maleic anhydride monomer graft polymers group is formed, and described polymeric groups is identical with described matrix polymer.
5. the preparation method of composite dual-electrode plates as claimed in claim 1, it is characterized in that, the mass percent of described matrix polymer, conductive filler and compatilizer is 10%-30%:50%-70%:10%-40%.
6. the preparation method of composite dual-electrode plates as claimed in claim 1, is characterized in that, described matrix polymer, conductive filler and compatilizer mix in the mode stirred, and the speed of described stirring is 600 revs/min to 1000 revs/min.
7. the preparation method of composite dual-electrode plates as claimed in claim 1, it is characterized in that, described shaping mode is compression molding, specifically comprises the following steps:
Described mixture extrusion molding is formed composite material, and this Laminated Shear Deformable is become pellet, and described pellet is placed in the described composite dual-electrode plates of the compressing formation of mould.
8. the preparation method of composite dual-electrode plates as claimed in claim 7, it is characterized in that, the temperature of described extrusion molding controls at 190 DEG C within the scope of 260 DEG C, and the mixing speed in described extrusion molding process is 200 revs/min to 300 revs/min.
9. the preparation method of composite dual-electrode plates as claimed in claim 7, it is characterized in that, described compressing mode is hot-forming, and described hot-forming temperature is 190 DEG C to 260 DEG C, and described hot-forming Stress control is at 10Mpa to 30Mpa.
10. the preparation method of composite dual-electrode plates as claimed in claim 1, it is characterized in that, described shaping mode is roll-forming, comprises the following steps:
Described mixture extrusion molding is formed described composite material, and
The direct roll-forming of the composite material this extruded forms described composite dual-electrode plates.
The preparation method of 11. composite dual-electrode plates as claimed in claim 1, is characterized in that, comprise further a pair shaping after the surface of described composite dual-electrode plates carry out the step of blasting treatment.
The preparation method of 12. composite dual-electrode plates as claimed in claim 1, it is characterized in that, described matrix polymer is thermoplastic resin, and described thermoplastic resin is one or more in polyethylene, polypropylene, polyvinyl chloride, polystyrene and acrylonitrile-butadiene-styrene copolymer.
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| JP2018529204A (en) * | 2015-09-25 | 2018-10-04 | ロッテ ケミカル コーポレーション | Slurry composition for electrode production of redox flow battery and electrode of redox flow battery containing the same |
| CN109921053A (en) * | 2017-12-13 | 2019-06-21 | 中国科学院大连化学物理研究所 | A kind of preparation method and applications of bipolar plates |
| CN110137506A (en) * | 2018-02-09 | 2019-08-16 | 上海电气集团股份有限公司 | Bipolar plate of redox flow battery, preparation method and its material microballoon |
| CN110289429A (en) * | 2019-06-21 | 2019-09-27 | 山东大学 | A kind of flexibility proton exchange membrane fuel cell plate and preparation method thereof |
| CN110492122A (en) * | 2019-08-19 | 2019-11-22 | 保定百能汇通新能源科技有限公司 | A kind of compound bipolar plates conductive plastic plate and preparation method thereof Preparation equipment |
| CN110854401A (en) * | 2018-08-21 | 2020-02-28 | 北京普能世纪科技有限公司 | Integrated collector plate, and preparation method and application thereof |
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| JP2018529204A (en) * | 2015-09-25 | 2018-10-04 | ロッテ ケミカル コーポレーション | Slurry composition for electrode production of redox flow battery and electrode of redox flow battery containing the same |
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| CN110137506B (en) * | 2018-02-09 | 2022-05-03 | 上海电气集团股份有限公司 | Flow battery bipolar plate, preparation method and material microspheres thereof |
| CN110854401A (en) * | 2018-08-21 | 2020-02-28 | 北京普能世纪科技有限公司 | Integrated collector plate, and preparation method and application thereof |
| CN110854401B (en) * | 2018-08-21 | 2022-08-19 | 北京普能世纪科技有限公司 | Integrated collector plate, and preparation method and application thereof |
| CN110289429A (en) * | 2019-06-21 | 2019-09-27 | 山东大学 | A kind of flexibility proton exchange membrane fuel cell plate and preparation method thereof |
| CN110289429B (en) * | 2019-06-21 | 2020-09-25 | 山东大学 | Flexible proton exchange membrane fuel cell polar plate and preparation method thereof |
| CN110492122A (en) * | 2019-08-19 | 2019-11-22 | 保定百能汇通新能源科技有限公司 | A kind of compound bipolar plates conductive plastic plate and preparation method thereof Preparation equipment |
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Application publication date: 20150204 |