CN101567452B - Preparation method of liquid flow battery composite material bipolar plate - Google Patents
Preparation method of liquid flow battery composite material bipolar plate Download PDFInfo
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- CN101567452B CN101567452B CN2009100822166A CN200910082216A CN101567452B CN 101567452 B CN101567452 B CN 101567452B CN 2009100822166 A CN2009100822166 A CN 2009100822166A CN 200910082216 A CN200910082216 A CN 200910082216A CN 101567452 B CN101567452 B CN 101567452B
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention relates to a preparation method of a liquid flow battery composite material bipolar plate, belonging to the technical field of liquid flow battery bipolar plate preparation. The preparation method of the liquid flow battery bipolar plate comprises three steps of using a solution method for mixing, using a tape casting method for casting and using a compression molding method for molding successively. The weight percentage of graphite powder/(graphite powder plus polyvinylidene fluoride) is 30% to 75%, and the dissolving temperature is 50 DEG C to 110 DEG C. The thin-layer thickness of a solution casted by the tape casting method is 0.2mm to 5mm, the compression molding temperature is 190 DEG C to 250 DEG C, and the pressure is 11MPa to 30MPa. The composite material bipolar plate made by using the method has the thickness of 1.0mm to 2.2mm and the electrical conductivity of 0.13S/cm to 41S/cm. The invention is easy for organizing large-scale and low-cost production processso as to overcome the shortcomings of complex processing and poor electrical conductivity of the prior liquid flow battery bipolar plate, thus laying the foundation for developing the chemical power technology used in large-scale energy conversion and storage.
Description
Technical field
The invention belongs to flow battery bipolar plates preparing technical field.
Technical background
Utilizing renewable energy power generations such as solar energy, wind energy, ocean wave energy can reduce human interdependent to fossil fuel, is one of following important channel that will obtain energy from nature.Yet owing to solar energy, wind energy, ocean wave energy etc. have unstable feature, the electric energy that is difficult to keep stable is exported, and the apparatus for storing electrical energy of needs and certain scale matches, and constitutes complete electric power system, could guarantee continual and steady supply of electrical energy.Therefore, exploitation electric energy conversion efficiency height, storage volume energy-storage system big, that economic performance is good become the important step of development renewable and clean energy resource generating.
(Vanadium Redox Battery VRB) is a kind of mechanism of new electrochemical power sources to all-vanadium flow battery, transforms the storage and the release of realization electric energy mutually by the vanadium ion of different valence state.Owing to use element of the same race to form battery system, avoided from principle that the variety classes active material interpenetrates the cross pollution of producing between positive and negative half-cell.Utilization is dissolved in that the different valence state vanadium ion is as anode and negative electrode active material in the electrolyte, and anodal electrolyte and negative pole electrolyte separate storage are avoided battery storage process self-discharge phenomenon fully, is suitable for extensive thermal energy storage process and uses.When the power of wind energy, device of solar generating surpasses rated output power,, electric energy is converted into chemical energy is stored in the ion of different valence state by to the flow battery charging; When Blast Furnace Top Gas Recovery Turbine Unit (TRT) can not satisfy rated output power, flow battery began discharge, and the chemical energy that stores is converted into electric energy, guaranteed the output of stable electrical power.In various forms of energy storage devices, all-vanadium flow battery has electrical power storage and transformation efficiency height, and the characteristics of long service life, environmental protection, safety are easy to be complementary with wind energy, solar power generation, for renewable energy utilization provides technique guarantee.Be used for the network system energy storage, can avoid the hydroenergy storage station construction period long, the shortcoming of addressing geographical conditions harshness, the uninterrupted power supply that is suitable for medium-scale industrial enterprise, hotel, government department uses, can effectively improve grid supply quality, finish " peak load shifting " effect of electrical network.
Bipolar plates in the flow battery directly connects the anodal half-cell and the negative pole half-cell of adjacent single cells, need possess the electrolyte permeability of prevention and conduction current ability simultaneously, in addition, bipolar plates also should have good chemical stability, anti-electrochemical oxidation and certain mechanical strength.Normal conditions at high temperature with the thermoplastic polymer fusion, add acetylene black or graphite powder or conductive fiber then as conductive filler, are processed into conductive plastics as bipolar plates after fully mixing.This method has successfully been used (CN1515046A in the flow battery research and development; CN1670992A).Complicated in order to overcome the control of high-temperature fusion course of processing temperature, polymeric material decomposes, melt viscosity height, be difficult to and shortcomings such as conductive filler fully mixes, people propose to utilize polymer suspension and conductive filler to mix, dried soak is rolled under 70～80 ℃ of conditions in flakes repeatedly, inject behind the mould technical method (CN101150192A) in the high temperature furnace sinter molding.Because the chemical bond character of DIC cellulosic material and organic high molecular compound is different with structure, cause material cohesive energy, surperficial close and distant water characteristic significant difference, have a strong impact on the even dispersion of carbon element class conductive filler in polymer suspension, be difficult to finish the mixing on molecular scale, influence the bipolar plates electric conductivity and further improve.
When utilizing thermoplastic polymer to prepare the flow battery bipolar plates, in polymer, evenly disperse and interconnect, form conductive network, realize the bipolar plates electric conductivity by conductive filler.The present invention proposes the flow battery bipolar plates that solwution method is mixed and the die pressing moulding combines and prepares scheme.Select for use suitable solvent that polymeric material is dissolved, be prepared into solution, add acetylene black or graphite powder or conductive fiber then, fully mix as conductive filler.Because the viscosity of polymer solution is far below the viscosity of polymer melt under the high temperature, conductive filler is dispersed in the polymer solution, the solvent of selecting for use all has affinity preferably to polymer and conductive filler, helps polymer and conductive filler to mix.With well-mixed polymer and conductive filler curtain coating straticulation, become sheet-shaped material after removing solvent.Some conducting polymer materials are superimposed together, and with its compression molding, become conductive bipolar plate after the cooling under certain temperature, pressure.Utilize the compression-moulding methods can the disposal molding flow-guiding structure, realize that active material in the electrolyte evenly the flowing of bipolar plate surfaces, increases the electrochemical reaction interfacial area, promote electrochemical redox reaction, improve the flow battery current density.This bipolar plates is used for flow battery, utilizes the elasticity of polymeric material to realize that easily the sealing of flow battery pile and engineering amplify, and avoids fully leaking in the electrolyte and leaking.In addition, solwution method hybrid technique easy realization of large-scale production, the solvent that dry run removes can reclaim usefulness again, realizes the environmental protection and the double benefit that reduces production costs.
Summary of the invention
The object of the invention is to provide a kind of preparation method of composite material bipolar plate, and especially preparation is applicable to the conductive bipolar plate in the flow battery.
The preparation method of composite material bipolar plate of a kind of flow battery of proposition of the present invention, described method contains following steps successively;
Step (1) is dissolved in the macromolecular compound Kynoar in the dimethyl sulfoxide solvent, and the concentration of described Kynoar in solution is 3%～11% when representing with percetage by weight, and course of dissolution stirs in 50 ℃～110 ℃ temperature ranges and finishes;
Step (2) adds conductive filler in the solution that step (1) obtains, and mixes in 50 ℃～110 ℃ temperature ranges, and described conductive filler is a graphite powder, and the percetage by weight of described graphite powder/(graphite powder+Kynoar) is between 30%～75%;
Step (3), use solution that the curtain coating casting method obtains step (2) at level and smooth glass surface curtain coating straticulation, thickness is between 0.2～3 millimeter, place the environment in 50 ℃～110 ℃ temperature ranges to carry out drying, after described dimethyl sulfoxide solvent volatilization, form the chip solid compound, peel off from described glass surface;
Step (4), the described chip solid compound that step (3) is obtained is superimposed together, place the plastic mould pressing processing mold, be warmed up to 190 ℃～250 ℃ temperature ranges gradually, keep after 15 minutes～60 minutes, apply 11MPa～30MPa pressure and continue compression molding in 3 minutes～10 minutes, the cooling back demoulding becomes conductive bipolar plate, and thickness is between 1.0～2.1 millimeters.
In the preparation method of composite material bipolar plate of above-mentioned a kind of flow battery, described graphite powder be crystalline flake graphite, particle size range between 1～2 micron, density is 2.2g/cmw, fixed carbon content is greater than 99.9%.
In the preparation method of composite material bipolar plate of above-mentioned a kind of flow battery, described macromolecular compound is with one or more the mixture in the following material: polyvinyl chloride, polysulfones, polyether sulfone, polyether-ether-ketone replace.
In the preparation method of composite material bipolar plate of above-mentioned a kind of flow battery, described solvent is with one or more the mixture in the following material: dimethyl formamide, and dimethylacetylamide, the N-methyl pyrrolidone replaces.
In the preparation method of composite material bipolar plate of above-mentioned a kind of flow battery, described conductive filler is with one or more the mixture in the following material: expanded graphite, carbon black, acetylene black, long carbon fiber, short carbon fiber, and carbon nano-tube replaces.
This bipolar plates is used for flow battery, performance graphite material good conductivity, the speciality that electrochemical corrosion resistant is strong, and in conjunction with the easy machine-shaping of macromolecule polymer material, and good pliability characteristics, preparation flow battery composite material double pole plate.Adopt the flow battery bipolar plates preparation technology that solwution method is mixed and the die pressing moulding combines, effectively overcome problems such as original high-temperature fusion course of processing polymeric material decomposes, conductive filler mixing difficulty, avoid in raw material, adding small-molecular weight processing aids such as lubricant, antioxidant simultaneously, improve the chemical stability of composite material double pole plate use.By at composite material double pole plate surface pressure system flow-guiding structure, realize that the active material in the electrolyte flows at the even of bipolar plate surfaces, increase the electrochemical reaction interfacial area, promote electrochemical redox reaction, improve the flow battery current density.Composite material double pole plate preparation technology method proposed by the invention, process realize the mass preparation of conductive bipolar plate simply, easily, for further industrial production lays the foundation.
Description of drawings
Fig. 1. the composite material double pole plate preparation technology flow chart of flow battery
Embodiment
The present invention contains following steps successively;
Step (1) is dissolved in the macromolecular compound Kynoar in the dimethyl sulfoxide solvent, and the concentration of described Kynoar in solution is 3%～11% when representing with percetage by weight, and course of dissolution stirs in 50 ℃～110 ℃ temperature ranges and finishes;
Step (2) adds conductive filler in the solution that step (1) obtains, and mixes in 50 ℃～110 ℃ temperature ranges, and described conductive filler is a graphite powder, and the percetage by weight of described graphite powder/(graphite powder+Kynoar) is between 30%～75%;
Step (3), use solution that the curtain coating casting method obtains step (2) at level and smooth glass surface curtain coating straticulation, thickness is between 0.2～3 millimeter, place the environment in 50 ℃～110 ℃ temperature ranges to carry out drying, after described dimethyl sulfoxide solvent volatilization, form the chip solid compound, peel off from described glass surface;
Step (4), the described chip solid compound that step (3) is obtained is superimposed together, place the plastic mould pressing processing mold, be warmed up to 190 ℃～250 ℃ temperature ranges gradually, keep after 15 minutes～60 minutes, apply 11MPa～30MPa pressure and continue compression molding in 3 minutes～10 minutes, the cooling back demoulding becomes described conductive bipolar plate, and thickness is between 1.0～2.2 millimeters.
Described macromolecular compound is one or more the mixture in the following material: polyvinyl chloride, polysulfones, polyether sulfone, polyether-ether-ketone.
Described solvent is one or more the mixture in the following material: dimethyl formamide, dimethylacetylamide, N-methyl pyrrolidone.
Described conductive filler is one or more the mixture in the following material: expanded graphite, carbon black, acetylene black, long carbon fiber, short carbon fiber, and carbon nano-tube.
Further specific implementation method of the present invention is as follows.
1) use chemical solvent that a kind of macromolecule resin is dissolved, add conductive filler then, abundant stirring and dissolving in 50～110 ℃ of temperature ranges is used casting method to form thin layer at level and smooth glass surface and is carried out drying, forms the solid flaky composite material after removing solvent; Flaky composite material is superimposed together, inserts in the plastic processing process mould commonly used, be warmed up to 190～250 ℃ of scopes gradually and keep after 30 minutes, apply 11～30MPa pressure die forming and kept 5 minutes, the cooling back demoulding becomes conductive bipolar plate;
2) chemical solvent 1) is dimethyl sulfoxide (DMSO) or dimethyl formamide;
3) macromolecular compound 1) is the fluoro containing polymers compound, preferentially selects Kynoar, and the concentration of macromolecule resin in solution is 3～11% (percetages by weight);
4) conductive filler 1) is a graphite powder, preferentially selects crystalline flake graphite, and granule size is 1～2 micron, density 2.2g/cm
3, fixed carbon content is greater than 99.9%, and the concentration of described conductive filler in Kynoar and conductive filler mixture is 30%～75% when representing with percetage by weight;
5) the composite material conductive bipolar plates 1), the thickness behind the cooling forming is between 1.0～2.2 millimeters.
The Kynoar of certain mass is added the back stirring and dissolving of heating in the dimethyl sulfoxide (DMSO), the crystalline flake graphite of certain mass is sneaked in the solution, fully mix.Cast in that the curtain coating straticulation carries out drying on the glass plate of cleaning, become the sheet composite conducting material after removing solvent.Some are superimposed together, put into mould die forming under the condition of heating, the insulation certain hour obtains the composite conducting bipolar plates after the demoulding.Utilize common electric conducting material method of testing, use electrochemical workstation to measure the conductivity of composite material double pole plate.Actual conditions sees Table one.
By the mode that the foregoing description provides, can make the flow battery bipolar plates of arbitrary dimension shape.Performance graphite material good conductivity, the speciality that electrochemical corrosion resistant is strong, in conjunction with the easy machine-shaping of macromolecule polymer material, and good pliability characteristics, preparation flow battery composite material double pole plate.This bipolar plates shows good chemical stability and anti-electrochemical oxidation characteristic in the medium-term and long-term immersion of the electrolyte of all-vanadium flow battery.The process route that the present invention proposes organizes on a large scale easily, production process cheaply, overcomes flow battery bipolar plates processed complex in the past, and the shortcoming of poorly conductive lays the foundation for development is used for the chemical power source technology that large-scale electric energy transforms and store.
Claims (5)
1. the preparation method of composite material bipolar plate of a flow battery is characterized in that, described method contains following steps successively;
Step (1) is dissolved in the macromolecular compound Kynoar in the dimethyl sulfoxide solvent, and the concentration of described Kynoar in solution is 3%～11% when representing with percetage by weight, and course of dissolution stirs in 50 ℃～110 ℃ temperature ranges and finishes;
Step (2) adds conductive filler in the solution that step (1) obtains, and mixes in 50 ℃～110 ℃ temperature ranges, and described conductive filler is a graphite powder, and the percetage by weight of described graphite powder/(graphite powder+Kynoar) is between 30%～75%;
Step (3), use solution that the curtain coating casting method obtains step (2) at level and smooth glass surface curtain coating straticulation, thickness is between 0.2～3 millimeter, place the environment in 50 ℃～110 ℃ temperature ranges to carry out drying, after described dimethyl sulfoxide solvent volatilization, form the chip solid compound, peel off from described glass surface;
Step (4), the described chip solid compound that step (3) is obtained is superimposed together, place the plastic mould pressing processing mold, be warmed up to 190 ℃～250 ℃ temperature ranges gradually, keep after 15 minutes～60 minutes, apply 11MPa～30MPa pressure and continue compression molding in 3 minutes～10 minutes, the cooling back demoulding becomes conductive bipolar plate, and thickness is between 1.0～2.1 millimeters.
2. the preparation method of composite material bipolar plate of a kind of flow battery according to claim 1 is characterized in that, described graphite powder be crystalline flake graphite, particle size range between 1～2 micron, density is 2.2g/cm
3, fixed carbon content is greater than 99.9%.
3. the preparation method of composite material bipolar plate of a kind of flow battery according to claim 1, it is characterized in that described macromolecular compound is with one or more the mixture in the following material: polyvinyl chloride, polysulfones, polyether sulfone, polyether-ether-ketone replace.
4. the preparation method of composite material bipolar plate of a kind of flow battery according to claim 1, it is characterized in that, described solvent is with one or more the mixture in the following material: dimethyl formamide, and dimethylacetylamide, the N-methyl pyrrolidone replaces.
5. the preparation method of composite material bipolar plate of a kind of flow battery according to claim 1, it is characterized in that, described conductive filler is with one or more the mixture in the following material: expanded graphite, carbon black, acetylene black, long carbon fiber, short carbon fiber, and carbon nano-tube replaces.
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| CN101814605B (en) * | 2010-03-19 | 2012-07-25 | 清华大学 | Preparation method of fluororesin-containing conductive plastic bi-polar plate |
| JP2011228059A (en) * | 2010-04-16 | 2011-11-10 | Sumitomo Electric Ind Ltd | Dipole plate for redox flow battery |
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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 |
| CN110257738B (en) * | 2019-01-15 | 2020-08-04 | 中南大学 | Preparation method of superfine carbon particle reinforced metal matrix composite material |
| CN111092231B (en) * | 2020-03-24 | 2020-08-04 | 杭州德海艾科能源科技有限公司 | Vanadium battery integrated electrode prepared from high-molecular resin emulsion |
| CN112157931A (en) * | 2020-09-17 | 2021-01-01 | 大连博融新材料有限公司 | Carbon bipolar plate with high carbon content, preparation process and application thereof |
| CN113745559B (en) * | 2021-09-22 | 2023-06-30 | 宁波信远材料科技股份有限公司 | Ultrathin carbon/carbon composite bipolar plate and preparation method thereof |
| CN116914172A (en) * | 2023-07-31 | 2023-10-20 | 浙江华熔科技有限公司 | High-performance composite bipolar plate and preparation method thereof |
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