CN107565146B - A bipolar plate for a flow battery and its preparation and application - Google Patents
A bipolar plate for a flow battery and its preparation and application Download PDFInfo
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- 238000007731 hot pressing Methods 0.000 claims description 24
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- 238000001125 extrusion Methods 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
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- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 6
- 229910052720 vanadium Inorganic materials 0.000 claims description 6
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 3
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
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- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- ZRXYMHTYEQQBLN-UHFFFAOYSA-N [Br].[Zn] Chemical compound [Br].[Zn] ZRXYMHTYEQQBLN-UHFFFAOYSA-N 0.000 claims description 2
- UKUJCSBWRBWNAV-UHFFFAOYSA-N [Sn].[V] Chemical compound [Sn].[V] UKUJCSBWRBWNAV-UHFFFAOYSA-N 0.000 claims description 2
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims 1
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Classifications
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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
- 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
Description
技术领域technical field
本发明涉及液流电池双极板材料领域，特别涉及全钒液流电池的双极板及其制备方法。The invention relates to the field of bipolar plate materials for flow batteries, in particular to a bipolar plate of an all-vanadium flow battery and a preparation method thereof.
背景技术Background technique
全钒液流电池因其具有输出功率和容量相互独立，系统设计灵活；能量效率高，寿命长，运行稳定性和可靠性高，自放电低；选址自由度大，无污染、维护简单，运营成本低，安全性高等优点，在规模储能方面具有广阔的发展前景，被认为是解决太阳能、风能等可再生能源发电系统随机性和间歇性非稳态特征的有效方法，在可再生能源发电和智能电网建设中有着重大需求。All-vanadium redox flow batteries are flexible in system design due to their independent output power and capacity; high energy efficiency, long life, high operational stability and reliability, and low self-discharge; large degree of freedom in location selection, no pollution, and simple maintenance. It has the advantages of low operating cost and high safety, and has broad development prospects in terms of large-scale energy storage. There is a significant need in power generation and smart grid construction.
双极板作为液流电池的关键部件，起着将单电池串联起来组成电堆的作用，需要具有良好的导电性、阻液性、化学稳定性以及一定的机械强度。As the key component of the flow battery, the bipolar plate plays the role of connecting the single cells in series to form a stack. It needs to have good electrical conductivity, liquid resistance, chemical stability and certain mechanical strength.
目前主要用到的双极板材料为硬质石墨板或碳塑复合材料。硬质石墨板具有电导率高、阻液性和化学稳定性好的特点，但高成本、机械性能差限制了其实际应用。碳塑复合材料是目前广受关注的一种双极板材料，主要优点是加工简单，成本低廉，易于实现大规模生产。然而，这种材料导电性较差，为了提高导电性，需要提高材料中的导电填料含量。然而，导电填料含量过高会使板变脆，不宜于电堆组装。因此，有必要研制高导电性高韧性的碳塑复合双极板。At present, the main bipolar plate materials used are hard graphite plates or carbon-plastic composite materials. Rigid graphite sheets have the characteristics of high electrical conductivity, liquid resistance and chemical stability, but their high cost and poor mechanical properties limit their practical applications. Carbon-plastic composite material is a bipolar plate material that has attracted wide attention. Its main advantages are simple processing, low cost, and easy mass production. However, this material has poor electrical conductivity, and in order to improve the electrical conductivity, it is necessary to increase the content of conductive fillers in the material. However, too high a conductive filler content will make the board brittle and unsuitable for stack assembly. Therefore, it is necessary to develop carbon-plastic composite bipolar plates with high conductivity and high toughness.
全钒液流电池为追求高功率密度，要求低电池内阻，因此对双极板的电导率有较高要求，而要提高电导率，则要提高导电填料的含量。为制备体电导率高于10S/cm的碳塑复合双极板材料，通常导电填料的质量分数要达到60％以上，此时由于聚合物基体中含有大量的导电填料，因此粘度增大，流动性降低，一方面会造成成型加工困难，另一方面制备的双极板较脆，无法满足装堆对机械性能的要求，尤其是韧性方面。In pursuit of high power density, all-vanadium redox flow batteries require low battery internal resistance, so there is a higher requirement for the conductivity of the bipolar plate, and to improve the conductivity, the content of conductive fillers must be increased. In order to prepare carbon-plastic composite bipolar plate materials with bulk conductivity higher than 10S/cm, the mass fraction of conductive fillers should reach more than 60%. On the one hand, it will cause difficulties in forming and processing. On the other hand, the prepared bipolar plate is relatively brittle and cannot meet the requirements for mechanical properties of stacking, especially in terms of toughness.
发明内容SUMMARY OF THE INVENTION
为解决上述技术问题，本发明旨在提供一种具有高导电性高韧性的液流电池用双极板及其制备方法，以降低电池内阻。In order to solve the above technical problems, the present invention aims to provide a bipolar plate for a flow battery with high conductivity and high toughness and a preparation method thereof, so as to reduce the internal resistance of the battery.
为实现上述目的，本发明采用的技术方案为：To achieve the above object, the technical scheme adopted in the present invention is:
本发明提供的双极板是由熔融指数为2-10的聚丙烯、导电填料以及润滑剂组成的碳塑复合板，或是由熔融指数为2-10的聚丙烯、导电填料组成的碳塑复合板，聚丙烯的质量分数为15-35％，导电填料的质量分数为65-85％，润滑剂的质量分数为0-2％。The bipolar plate provided by the invention is a carbon-plastic composite plate composed of polypropylene with a melt index of 2-10, conductive fillers and lubricants, or a carbon-plastic composite plate composed of polypropylene with a melt index of 2-10 and conductive fillers For the composite plate, the mass fraction of polypropylene is 15-35%, the mass fraction of conductive filler is 65-85%, and the mass fraction of lubricant is 0-2%.
其中，所述聚丙烯为挤出级聚丙烯，熔融指数优选2-5；Wherein, the polypropylene is extrusion grade polypropylene, and the melt index is preferably 2-5;
所述导电填料为石墨、碳黑、碳纤维、石墨纤维、乙炔黑、碳纳米管中的一种或几种；The conductive filler is one or more of graphite, carbon black, carbon fiber, graphite fiber, acetylene black, and carbon nanotube;
所述润滑剂为聚乙烯蜡、硬脂酸、硬酯酸钙、硬酯酸锌、石蜡、乙烯基双硬脂酰胺中的一种或几种。The lubricant is one or more selected from polyethylene wax, stearic acid, calcium stearate, zinc stearate, paraffin wax and vinyl bis-stearamide.
所述熔融指数为采用ASTM D1238标准测试方法在230℃/2.16kg条件下测得。The melt index is measured under the condition of 230°C/2.16kg using the ASTM D1238 standard test method.
所述碳塑复合板通过将原料共混后采用模压工艺或挤出压延成型工艺制备而成。The carbon-plastic composite board is prepared by blending the raw materials and then adopting a molding process or an extrusion calendering process.
本发明提供的制备该种双极板的方法包括如下步骤：The method for preparing the bipolar plate provided by the present invention comprises the following steps:
1.采用密炼的方式按所需比例将聚合物、导电填料和润滑剂，或聚合物和导电填料混合均匀，密炼温度为200-240℃，转子转速为40-60r/min；1. Mix the polymer, the conductive filler and the lubricant, or the polymer and the conductive filler evenly in the required proportion by the banburying method, the banburying temperature is 200-240℃, and the rotor speed is 40-60r/min;
2.将混合均匀的密炼料放入模具中，采用热压的方式将密炼料压制成双极板，热压温度为180～220℃，热压压力为5～50MPa，热压时间为1～30min。2. Put the mixed mixed material into the mold, and press the mixed material into a bipolar plate by hot pressing. The hot pressing temperature is 180～220℃, the hot pressing pressure is 5～50MPa, and the hot pressing time is 1 to 30 minutes.
或，将混合均匀的密炼料用粉碎机粉碎，采用挤出压延成型工艺，使用单螺杆挤出机或者双螺杆挤出机制成碳塑复合双极板，料筒温度为180～220℃，口模温度为160～200℃，主机转速为5～15rpm。Or, pulverize the evenly mixed banbury material with a pulverizer, use an extrusion calendering process, and use a single-screw extruder or a twin-screw extruder to form a carbon-plastic composite bipolar plate, and the barrel temperature is 180-220 ℃, The die temperature is 160～200℃, and the main engine speed is 5～15rpm.
本发明所述双极板可应用于全钒液流电池、锌溴液流电池、多硫化钠溴液流电池或锡钒液流电池中。The bipolar plate of the invention can be applied to an all-vanadium flow battery, a zinc-bromine flow battery, a sodium-bromine polysulfide flow battery or a tin-vanadium flow battery.
与现有技术相比，本发明具有如下优点：Compared with the prior art, the present invention has the following advantages:
(1)采用本发明的双极板，与现有的碳塑复合材料双极板相比，由于导电填料含量的提高，具有更高的体电导率，从而能够降低双极板的本体电阻和接触电阻，继而减小电池内阻。(1) Using the bipolar plate of the present invention, compared with the existing carbon-plastic composite bipolar plate, due to the increase of the conductive filler content, it has higher bulk conductivity, so that the body resistance and the resistance of the bipolar plate can be reduced. Contact resistance, thereby reducing the internal resistance of the battery.
(2)采用本发明的双极板，与硬石墨板相比，具有较高的韧性，可以改善液流电池的组装条件。(2) Compared with the hard graphite plate, the bipolar plate of the present invention has higher toughness and can improve the assembly conditions of the flow battery.
(3)本发明提出的双极板制备方法简单，生产过程容易控制，易于批量化制备，且所用原料价格低廉，可全部实现国产化。(3) The preparation method of the bipolar plate proposed by the present invention is simple, the production process is easy to control, and it is easy to be prepared in batches, and the raw materials used are cheap, and all of them can be localized.
具体实施方式Detailed ways
下面通过具体实施例详述本发明。The present invention will be described in detail below through specific embodiments.
实施例1Example 1
分别称取聚丙烯(熔融指数为5)0.5kg，石墨粉0.8kg，碳黑0.7kg，聚乙烯蜡10g，硬酯酸锌10g，加入到密炼机中，密炼温度为220℃，转子转速为50r/min，密炼时间20分钟。然后将混合均匀的密炼料经粉碎机粉碎后送入单螺杆挤出机中，挤出机料筒温度为200℃，主机转速为10rpm，口模温度为190℃，挤出片材并压延成型制得1mm厚碳塑复合双极板。Take by weighing 0.5kg of polypropylene (melt index is 5), 0.8kg of graphite powder, 0.7kg of carbon black, 10g of polyethylene wax, and 10g of zinc stearate, and add them to the mixer, the mixing temperature is 220°C, and the rotor The rotating speed is 50r/min, and the mixing time is 20 minutes. Then, the uniformly mixed banbury material is crushed by a pulverizer and sent to a single-screw extruder. The temperature of the extruder barrel is 200 ° C, the speed of the main engine is 10 rpm, and the die temperature is 190 ° C. Extrude the sheet and calender A 1mm thick carbon-plastic composite bipolar plate was obtained by molding.
分别测试本实施例双极板和各对比例中碳塑复合板的电导率、接触电阻和力学性能，结果列于表1，相对于对比例1和2，本实施例双极板的电导率大幅提高，接触电阻降低了60％左右，而弯曲形变基本不变，仍然保持了较高的韧性，而相对于对比例3，本实施例双极板的抗弯形变得到了大幅提升。The electrical conductivity, contact resistance and mechanical properties of the carbon-plastic composite plates in the bipolar plate of this embodiment and each comparative example were tested respectively. The results are listed in Table 1. Compared with Comparative Examples 1 and 2, the electrical conductivity of the bipolar plate in this embodiment It is greatly improved, the contact resistance is reduced by about 60%, and the bending deformation is basically unchanged, and the high toughness is still maintained. Compared with Comparative Example 3, the bending resistance of the bipolar plate in this embodiment has been greatly improved.
用本实施例双极板组装成全钒液流单电池，正极电解液为1.5M VO2+的3M H2SO4溶液40ml，负极电解液为1.5M V3+的3M H2SO4溶液40ml。采用本实施例双极板的单电池，电流密度为80mA/cm2时，电压效率和能量效率分别为88.2％和83.6％；电流密度为100mA/cm2时，电压效率和能量效率也分别达到了85.6％和81.3％。The bipolar plate of this example was used to assemble an all-vanadium flow single cell, the positive electrolyte was 40ml of 1.5M VO 2+ 3M H 2 SO 4 solution, and the negative electrolyte was 1.5MV 3+ 3M H 2 SO 4 solution 40ml. For the single cell using the bipolar plate of this embodiment, when the current density is 80mA/cm 2 , the voltage efficiency and energy efficiency are 88.2% and 83.6% respectively; when the current density is 100mA/cm 2 , the voltage efficiency and energy efficiency also reach up 85.6% and 81.3%.
实施例2Example 2
分别称取聚丙烯(熔融指数为3)0.4kg，石墨粉1.0kg，碳黑0.6kg，石蜡15g，硬酯酸5g，加入到密炼机中，密炼温度为230℃，转子转速为50r/min，密炼时间20分钟。然后将混合均匀的密炼料放入模具中，送入热压机，热压温度为210℃，热压压力为50MPa，热压时间为3min。最终热压成型制得1mm厚碳塑复合双极板。Weigh out 0.4kg of polypropylene (with a melt index of 3), 1.0kg of graphite powder, 0.6kg of carbon black, 15g of paraffin wax, and 5g of stearic acid, and add them to the mixer. The mixing temperature is 230°C, and the rotor speed is 50r. /min, the mixing time is 20 minutes. Then put the evenly mixed Banbury into the mold and send it to the hot press, the hot pressing temperature is 210℃, the hot pressing pressure is 50MPa, and the hot pressing time is 3min. Finally, a 1mm thick carbon-plastic composite bipolar plate was obtained by hot pressing.
实施例3Example 3
分别称取聚丙烯(熔融指数为10)0.6kg，石墨粉1kg，碳黑0.4kg，聚乙烯蜡5g，硬酯酸锌5g，加入到密炼机中，密炼温度为220℃，转子转速为50r/min，密炼时间20分钟。然后将混合均匀的密炼料放入模具中，送入热压机，热压温度为200℃，热压压力为30MPa，热压时间为10min。最终热压成型制得1mm厚碳塑复合双极板。Take by weighing polypropylene (melt index is 10) 0.6kg, graphite powder 1kg, carbon black 0.4kg, polyethylene wax 5g, zinc stearate 5g, join in Banbury mixer, Banbury temperature is 220 ℃, rotor speed It is 50r/min, and the mixing time is 20 minutes. Then put the evenly mixed banbury into the mold and send it to the hot press, the hot pressing temperature is 200℃, the hot pressing pressure is 30MPa, and the hot pressing time is 10min. Finally, a 1mm thick carbon-plastic composite bipolar plate was obtained by hot pressing.
实施例4Example 4
分别称取聚丙烯(熔融指数为2)0.7kg，石墨粉0.9kg，碳纳米管0.4kg，聚乙烯蜡10g，硬酯酸钙10g，加入到密炼机中，密炼温度为220℃，转子转速为50r/min，密炼时间20分钟。然后将混合均匀的密炼料经粉碎机粉碎后送入单螺杆挤出机中，挤出机料筒温度为210℃，主机转速为8rpm，口模温度为200℃，挤出片材并压延成型制得1mm厚碳塑复合双极板。Take by weighing 0.7kg of polypropylene (melt index is 2), 0.9kg of graphite powder, 0.4kg of carbon nanotubes, 10g of polyethylene wax, and 10g of calcium stearate, and add them to the mixer, and the mixing temperature is 220°C. The rotor speed is 50r/min, and the mixing time is 20 minutes. Then the uniformly mixed banbury material is crushed by a pulverizer and sent to a single-screw extruder. The temperature of the extruder barrel is 210 ° C, the speed of the main machine is 8 rpm, and the temperature of the die is 200 ° C. The sheet is extruded and calendered. A 1mm thick carbon-plastic composite bipolar plate was obtained by molding.
对比例1Comparative Example 1
分别称取聚丙烯(熔融指数为0.7)0.5kg，石墨粉0.8kg，碳黑0.7kg，聚乙烯蜡10g，硬酯酸锌10g，加入到密炼机中，密炼温度为220℃，转子转速为50r/min，密炼时间20分钟。然后将混合均匀的密炼料经粉碎机粉碎后送入单螺杆挤出机中，挤出机料筒温度为210℃，主机转速为10rpm，口模温度为190℃，挤出片材并压延成型制得1mm厚碳塑复合双极板。Take by weighing 0.5kg of polypropylene (melt index is 0.7), 0.8kg of graphite powder, 0.7kg of carbon black, 10g of polyethylene wax, and 10g of zinc stearate, and add them to the mixer. The mixing temperature is 220°C. The rotating speed is 50r/min, and the mixing time is 20 minutes. Then, the uniformly mixed banbury material is crushed by a pulverizer and sent to a single-screw extruder. The temperature of the extruder barrel is 210 ° C, the speed of the main machine is 10 rpm, and the die temperature is 190 ° C. The extruded sheet is extruded and rolled. A 1mm thick carbon-plastic composite bipolar plate was obtained by molding.
对比例2Comparative Example 2
分别称取聚丙烯(熔融指数为30)0.8kg，石墨粉0.6kg，碳黑0.6kg，聚乙烯蜡10g，硬酯酸锌10g，加入到密炼机中，密炼温度为200℃，转子转速为50r/min，密炼时间20分钟。然后将混合均匀的密炼料经粉碎机粉碎后送入单螺杆挤出机中，挤出机料筒温度为215℃，主机转速为10rpm，口模温度为200℃，挤出片材并压延成型制得1mm厚碳塑复合双极板。Take by weighing 0.8kg of polypropylene (melt index is 30), 0.6kg of graphite powder, 0.6kg of carbon black, 10g of polyethylene wax, 10g of zinc stearate, and add them to the mixer, the mixing temperature is 200 ℃, the rotor The rotating speed is 50r/min, and the mixing time is 20 minutes. Then, the uniformly mixed banbury material is crushed by a pulverizer and sent to a single-screw extruder. The temperature of the extruder barrel is 215°C, the speed of the main machine is 10rpm, and the die temperature is 200°C. The sheet is extruded and calendered. A 1mm thick carbon-plastic composite bipolar plate was obtained by molding.
对比例3Comparative Example 3
分别称取聚丙烯(熔融指数为30)0.5kg，石墨粉0.8kg，碳黑0.7kg，聚乙烯蜡10g，硬酯酸锌10g，加入到密炼机中，密炼温度为200℃，转子转速为50r/min，密炼时间20分钟。然后将混合均匀的密炼料放入模具中，送入热压机，热压温度为210℃，热压压力为50MPa，热压时间为3min。最终热压成型制得1mm厚碳塑复合双极板。Take by weighing 0.5kg of polypropylene (melt index is 30), 0.8kg of graphite powder, 0.7kg of carbon black, 10g of polyethylene wax, and 10g of zinc stearate, and add them to the mixer, the mixing temperature is 200°C, and the rotor The rotating speed is 50r/min, and the mixing time is 20 minutes. Then put the evenly mixed Banbury into the mold and send it to the hot press, the hot pressing temperature is 210℃, the hot pressing pressure is 50MPa, and the hot pressing time is 3min. Finally, a 1mm thick carbon-plastic composite bipolar plate was obtained by hot pressing.
表1Table 1
该双极板解决了高含量导电填料碳塑复合双极板韧性差的问题，从而具有高导电性和良好的韧性，能够在保证电堆组装的前提下降低双极板的本体电阻和接触电阻，从而降低流储能电池的欧姆内阻。The bipolar plate solves the problem of poor toughness of the high-content conductive filler carbon-plastic composite bipolar plate, so it has high conductivity and good toughness, and can reduce the body resistance and contact resistance of the bipolar plate on the premise of ensuring the assembly of the stack , thereby reducing the ohmic internal resistance of the current energy storage battery.
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