CN103415950A - 到平坦多孔基材的两面的两种乙烯基单体混合物的同时聚合 - Google Patents
到平坦多孔基材的两面的两种乙烯基单体混合物的同时聚合 Download PDFInfo
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Abstract
采用了下述方法在多孔基材的两面上形成具有多种离子交换聚合物的双极电极，所述方法包括：在电极基材的两面上为电极基材提供活性碳层，其中所述两面具有没有活性碳层的外部周边带。将电极基材放置在由一对聚乙烯薄膜形成的热塑性封套中。在靠着电极基材的封套各侧放入Mylar薄片，将封套热封到电极基材的没有活性碳的外部周边带上以在电极基材的一侧上形成第一口袋且在电极基材的对侧上形成第二口袋。所述方法还包括将具有阴离子交换基团的第一可聚合单体混合物插入封套的第一口袋中和将具有阳离子交换基团的第二可聚合单体混合物插入封套的第二口袋中。随后使第一可聚合单体混合物和第二可聚合单体混合物在烘箱中聚合。
Description
发明背景。
发明领域
本发明涉及双极电极，且更详细地讲，涉及同时施用两种不同的离子交换聚合物到电极基材的两面的方法。
相关技术描述
越来越需要使用被动去离子来纯化水。被动去离子使用双极电极，例如具有由具有阳离子交换功能的材料形成的第一侧或第一面和具有阴离子交换功能的第二侧或第二面的两个薄片。两种不同的离子交换材料层各自为多孔的或要不然根据其化学、物理结构和交联程度而稍微能渗透中性流体，且各层具有离子交换功能，运行离子交换功能以在电场下传输一种类型的离子通过所述材料，同时基本上或有效地阻断大多数相反极性的离子。利用在相邻层中面对面布置的两种不同交换类型的材料，离子被一层或另一层有效地“阻断”且因此不能通过该薄片。
施用离子交换单体到电极的单独各侧且使它们聚合产生双极电极，与具有压在其上的离子交换膜的一系列单极(monoplanar)电极相比，所述双极电极更有效地起作用。在这方面，希望提供用于制造双极电极的新方法。
发明概述
一方面，本发明涉及在多孔基材的两面上形成具有多种离子交换聚合物的双极电极的方法。所述方法包括：在电极基材的两面上为电极基材提供活性碳层，其中所述两面具有没有活性碳层的外部周边带。将电极基材放置在由一对聚乙烯薄膜形成的热塑性封套中。在靠着电极基材的封套各侧放入Mylar薄片，将封套热封到电极基材的没有活性碳的外部周边带上以在电极基材的一侧上形成第一口袋且在电极基材的对侧上形成第二口袋。所述方法还包括将具有阴离子交换基团的第一可聚合单体混合物插入封套的第一口袋中和将具有阳离子交换基团的第二可聚合单体混合物插入封套的第二口袋中。随后使第一可聚合单体混合物和第二可聚合单体混合物在烘箱中聚合。
在参考附图阅读以下发明详述和所附权利要求书时将显而易见本发明及其优于现有技术的优势。
附图简述
通过结合附图进行参考本发明实施方案的以下描述，将更加显而易见本发明的上述及其他特征且将更透彻地理解本发明本身，其中：
图1示出了根据本发明的一个实施方案制造的双极电极的示意图。
相应的参考符号表示在整个附图视图中的相应部分。
发明详述
现在将参考附图在以下发明详述中描述本发明，其中详细描述优选的实施方案以便能够实施本发明。虽然参考这些特定优选的实施方案描述了本发明，但是应当理解的是，本发明不受这些优选实施方案限制。相反地，本发明包括如在考虑以下发明详述时将显而易见的许多供选物、改进及等价物。
参考图1，示出了包括在其两侧上具有不同的离子交换聚合物涂层的基本平坦的电极基材12的双极电极10。基材12为具有中间导电薄膜的多孔载体。理想地，电极基材12由热塑性聚乙烯薄膜制成，活性碳层结合到所述薄膜的各个面12A、12B上以形成多孔载体。所述电极基材的两面12A、12B用不同的离子交换聚合物涂布。根据本发明，电极基材12的两面12A、12B用两种乙烯基单体混合物同时涂布且经历同时聚合。因此，如下所述的方法特别适合在电极基材的两面上同时形成两种不同的离子交换聚合物涂层。
电极基材12由热塑性薄膜形成，活性碳层14结合在所述薄膜的各个面12A、12B上。技术人员应理解，可使用大量的其他材料来形成电极基材。例如，可以提到含有活性碳的填料，诸如树脂和粘合剂如TFE和PVDF。在一个合乎需要的实施方案中，基材12通常为边长为约10英寸×21.5英寸的矩形。然而，本领域技术人员应理解这些尺寸仅用于举例说明，且在不偏离本发明的范围的情况下可使用其他尺寸。所述基材的外部周边具有保持没有活性碳层14的区带18。
双口袋封套20围绕电极基材形成。通过用封套20覆盖多孔电极基材12，防止聚合受氧气阻碍且获得表面平滑度。在一个实施方案中，封套20用两个具有三个结合在一起的侧面和一个开口的侧面的通常矩形的聚乙烯薄膜22形成，以使得电极基材12可放置到封套中。封套20的聚乙烯薄膜22围绕所述基材的周长热封到电极基材12的没有活性碳14的区带18，由此围绕活性碳14在电极基材12的一侧上形成第一口袋且在电极12的对侧上形成第二口袋。塑料或Mylar薄片30 (即，聚对苯二甲酸乙二醇酯)插入在聚乙烯薄膜22与电极基材12之间的封套20的各个口袋中。在一个实施方案中，含有电极基材12的封套20随后放置在两块刚性板之间且将所述板夹牢在一起。
将第一乙烯基单体溶液加到在所述基材的第一面12A上形成的第一口袋中且将第二乙烯基单体溶液加到围绕所述基材的第二面12B形成的第二口袋中。第一单体溶液与第二单体溶液不同。液体单体置换在所述活性碳中的空气。在一个实施方案中，抽吸真空以从所述活性碳中除去空气。
理想地，第一口袋用包含具有阴离子交换基团或可转化成阴离子交换基团的基团的可聚合单体的第一可聚合单体混合物填充。用于将第一可聚合单体混合物插入第一口袋中的装置被插入所述封套中。在一个实施方案中，可使用移液吸管以将第一可聚合单体混合物插入在所述Mylar与所述电极基材之间的第一口袋中。在一个实施方案中，第一可聚合单体混合物包含交联剂和聚合引发剂。第一可聚合单体混合物渗透或包埋到多孔基材薄膜的空隙中且使渗透的可聚合单体混合物聚合。可将任何已知的可聚合单体用作具有阴离子交换基团或可转化成阴离子交换基团的基团的第一可聚合单体而不受限制。具有阴离子交换基团的可聚合单体的实例例如有：甲基丙烯酸甲酯三甲基氯化铵、甲基丙烯酰氧基丙基三甲基乙基氯化铵、乙烯基苄基三甲基氯化铵、二烯丙基二甲基氯化铵等且可提到其他烯属不饱和季铵和叔胺单体。
理想地，第二口袋用包含具有阳离子交换基团或可转化成阳离子交换基团的基团的可聚合单体的第二可聚合单体混合物填充。用于将第二可聚合单体混合物插入第二口袋中的装置被插入所述封套中。在一个实施方案中，可使用类似于供第一口袋使用的移液吸管的移液吸管来将第二可聚合单体混合物插入在所述Mylar与电极基材之间的第二口袋中。在一个实施方案中，第二可聚合单体混合物包含交联剂和聚合引发剂。所述可聚合单体混合物渗透或包埋到多孔基材薄膜的空隙中且使渗透的可聚合单体混合物聚合。可使用任何已知的可聚合单体作为具有所述阳离子交换基团或可转化成所述阳离子交换基团的基团的第二可聚合单体而不受限制。具有阳离子交换基团的可聚合单体的实例例如有：甲基丙烯酸磺乙酯、丙烯酰胺甲基丙烷、磺酸、苯乙烯磺酸钠、甲基丙烯酸磺丙酯钾盐等且可提到其盐及衍生物。还可提到其他烯属不饱和磺酸和羧酸。
作为加到第一可聚合单体混合物或第二可聚合单体混合物中的交联剂没有特别限制。可以提到例如二乙烯基苯、二乙烯基砜、丁二烯、氯丁二烯、二乙烯基联苯、三乙烯基苯、二乙烯基萘、二烯丙胺、二乙烯基吡啶、乙二醇-二甲基丙烯酸酯、其他多元醇的二或多丙烯酸酯或二或多甲基丙烯酸酯。也可使用潜在的交联体系，诸如羟甲基丙烯酰胺加丙烯酰胺或羟甲基丙烯酰胺和苯酚。
作为聚合引发剂，可使用已知化合物而不受特别限制。可以使用例如有机过氧化物，诸如过氧化辛酰、过氧化月桂酰、2-乙基己酸过氧化叔丁酯、过氧化苯甲酰、异丁酸过氧化叔丁酯、月桂酸过氧化叔丁酯、苯甲酸过氧化叔己酯、过氧化二叔丁基；和有机偶氮化合物，诸如偶氮二异丁腈等。
在第一可聚合单体混合物和第二可聚合单体混合物中，具有阴离子或阳离子交换基团或可转化成阴离子或阳离子交换基团的基团的可聚合单体、交联剂和聚合引发剂的比例可在宽范围内，只要各组分以聚合所必需的量存在即可。交联剂的比例优选为具有离子交换基团或可转化成离子交换基团的基团的可聚合单体与交联剂的总量的约0.4-60摩尔%，更优选为约1-50摩尔%，最优选为约1-约40摩尔%。所述聚合引发剂以通常的量使用。
在一个实施方案中，在将第一可聚合单体混合物和第二可聚合单体混合物插入第一室和第二室中之后，使第一可聚合单体混合物和第二可聚合单体混合物静置选定的持续时间。合适的持续时间通常为约1-20分钟，更优选为约5-15分钟，且在一个实施方案中，为约10分钟。在静置之后，随后可在使所述可聚合混合物聚合之前除去所述可聚合单体混合物的过量部分。
在制造双极电极10的过程中，如先前所述，使可聚合单体混合物与在电极基材上由活性碳层形成的多孔基材接触。所述聚合优选在用所述双口袋封套覆盖所述多孔膜之后进行。在使所述可聚合单体混合物聚合的过程中，使用已知的聚合方法，而不受限制。在一个实施方案中，将含有电极基材的封套放置在烘箱中且使乙烯基单体聚合到所述基材的各面上。通常优选使用聚合引发剂的热聚合，因为操作容易且聚合可相对均匀地进行。所述热聚合的温度不受特别限制，且可适当地选择已知的温度条件。合适的温度通常为50-150℃，更优选为60-120℃，且在一个实施方案中，为约85℃。所述热聚合的持续时间也不受特别限制，且可适当地选择已知的持续时间条件。合适的持续时间通常为约10-120分钟，更优选为约45-90分钟，且在一个实施方案中，为约60分钟。在不偏离本发明的范围的情况下，所述可聚合单体混合物的聚合也可通过任何已知的化学催化方法或使用紫外光进行。
为了使本领域技术人员能够很好地实践本发明，以说明而不是限制的方式提供以下实施例。
实施例
电极10通过将具有活性碳层14的电极基材12切割成10英寸(25.4cm)×21.5英寸(54.6cm)的尺寸来制造。所述电极基材的外部周边带18保持不含活性碳，围绕电极基材的两个长侧边和短底边留下1.5英寸(3.8cm)的修边。将顶边切成2英寸。封套20用具有一个长侧面开口的11英寸(27.9cm)×21.5英寸(54.6cm)的聚乙烯袋膜制成。将电极基材置于聚乙烯袋膜22之间。
围绕基材的周边将封套20的聚乙烯薄膜22热封到电极基材12的没有碳的区域18，由此围绕活性碳在电极基材的各侧上形成口袋。将封套20密封到基材上，封套20的两个长侧距离基材的边缘0.5英寸(1.3cm)且在底侧上，形成具有一个开口侧的封套。切掉封套的各长侧的0.5英寸(1.3cm)。Mylar薄片30靠近电极基材插入封套的各侧。将所述封套放置在两块玻璃板之间且将封套/玻璃板夹心结构夹牢在一起。将移液吸管插入在所述Mylar与所述电极基材之间的封套的各侧中。理想地，将所述封套/玻璃板夹心结构保持处于垂直位置，其中开口端和吸管在顶部。封套/玻璃板夹心结构使用具有两个夹具的环架适当地夹牢在Mylar托盘上。
140克的具有阴离子交换基团的第一可聚合单体混合物经一个吸管注入封套的第一口袋中且140克的具有阳离子交换基团的第二可聚合单体混合物经另一吸管注入封套的第二口袋中。所述夹心结构的多个侧面以2英寸(5.1cm)间隔夹牢，或者，直至混合物的水平面高于电极基材。使该混合物静置10分钟。
将封套20从玻璃夹心结构移出且置于Mylar托盘中。将电极基材的长边放置在封套上的底部表面附近且按压该封套。在恒定压力下将电极基材从封套的底部移动到封套的顶部，将过量的单体混合物从封套清扫到Mylar托盘中。将该封套翻转且在封套的另一侧重复该程序。
随后将封套20放置在这两块玻璃板之间且在封套/玻璃夹心结构组件的底边上连接四个大夹具。在封套/玻璃夹心结构组件的各侧边上连接六个夹具，或者这些夹具自底部到顶部放置。在封套/玻璃夹心结构的顶边连接四个夹具。随后将封套/玻璃夹心结构组件水平放置到预热85℃的烘箱中历时1小时。
将封套/玻璃夹心结构组件从烘箱中移出且使其冷却0.5小时。随后除去夹具且将封套与玻璃板分离。将封套和Mylar自电极除去且将电极放置于1N氯化钠中，直至随时使用。
技术人员也可理解的事实是，可对封套施加压力，将聚合的AIX和CIX材料在其各自的封套内压成平坦平面布置。
虽然已经在典型的实施方案中说明并描述了本发明，但并非想要将其限制于所显示的细节，因为可在决不脱离本发明的精神的情况下进行各种改进和替代。因而，本领域的技术人员仅仅使用常规实验就可想到本文公开的本发明的其他改进和等价物，且认为所有这些改进和等价物都在如由以上权利要求书限定的本发明的范围内。
要求保护的是：。
Claims (7)
1. 在多孔基材的两面上形成具有多种离子交换聚合物的双极电极的方法，所述方法包括：
在电极基材的两面上为电极基材提供活性碳层，其中所述两面具有没有活性碳层的外部周边带，
将电极基材放置在由一对聚乙烯薄膜形成的热塑性封套中；
将封套热封到电极基材的没有活性碳的外部周边带上以在电极基材的一侧上形成第一口袋且在电极基材的对侧上形成第二口袋；
将封套夹牢在两块刚性板之间；
将具有阴离子交换基团的第一可聚合单体混合物插入封套的第一口袋中；
将具有阳离子交换基团的第二可聚合单体混合物插入封套的第二口袋中；和
使第一可聚合单体混合物和第二可聚合单体混合物聚合。
2. 权利要求1的方法，其中第一可聚合单体混合物和第二可聚合单体混合物通过热聚合来聚合。
3. 权利要求2的方法，其中第一可聚合单体混合物和第二可聚合单体混合物通过将封套和电极基材水平地放置到处于85℃下的烘箱中来聚合。
4. 权利要求1的方法，其中第一阴离子可聚合单体混合物选自烯属不饱和叔胺和季胺化合物、及其盐和衍生物。
5. 权利要求1的方法，其中第二阳离子可聚合单体混合物选自烯属不饱和磺酸和、和羧酸、及其盐和衍生物。
6. 权利要求1的方法，其还包括在靠着电极基材的封套各侧插入Mylar薄片。
7. 权利要求1的方法，其还包括将第一移液吸管插入封套的第一口袋中且将第二移液吸管插入封套的第二口袋中，和将第一可聚合单体混合物和第二可聚合单体混合物分别经由第一吸管和第二吸管插入第一口袋和第二口袋中。
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- 2011-12-07 JP JP2013547501A patent/JP5849101B2/ja active Active
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Patent Citations (8)
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| US4140815A (en) * | 1975-12-31 | 1979-02-20 | Allied Chemical Corporation | Method of making single film, high performance bipolar membrane |
| US4125680A (en) * | 1977-08-18 | 1978-11-14 | Exxon Research & Engineering Co. | Bipolar carbon-plastic electrode structure-containing multicell electrochemical device and method of making same |
| US5340368A (en) * | 1993-08-04 | 1994-08-23 | Valence Technology, Inc. | Method for in situ preparation of an electrode composition |
| US5688615A (en) * | 1995-11-03 | 1997-11-18 | Globe-Union, Inc. | Bipolar battery and method of making same |
| WO2002045844A2 (en) * | 2000-12-06 | 2002-06-13 | General Electric Company | Use of gradient mixtures for screening and optimization of catalysts for the production of condensation polymers |
| CN1788831A (zh) * | 2001-04-18 | 2006-06-21 | 拜奥资源公司 | 流通电容器 |
| JP2004164898A (ja) * | 2002-11-11 | 2004-06-10 | Nissan Motor Co Ltd | バイポーラ電池の製造方法、およびバイポーラ電池 |
| US20040229993A1 (en) * | 2003-02-19 | 2004-11-18 | Jianhua Huang | Highly conductive thermoplastic composites for rapid production of fuel cell bipolar plates |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103415950B (zh) | 2016-08-24 |
| CA2822226A1 (en) | 2012-07-05 |
| BR112013016759A8 (pt) | 2020-01-28 |
| BR112013016759A2 (pt) | 2016-10-11 |
| US8658241B2 (en) | 2014-02-25 |
| TWI489005B (zh) | 2015-06-21 |
| JP5849101B2 (ja) | 2016-01-27 |
| TW201231728A (en) | 2012-08-01 |
| SG191794A1 (en) | 2013-08-30 |
| KR20140005937A (ko) | 2014-01-15 |
| WO2012091870A1 (en) | 2012-07-05 |
| CA2822226C (en) | 2015-10-27 |
| KR101566599B1 (ko) | 2015-11-05 |
| US20120171361A1 (en) | 2012-07-05 |
| JP2014503014A (ja) | 2014-02-06 |
| EP2659539A1 (en) | 2013-11-06 |
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