CN104136672B - 由用有机粘合剂聚合物化合物涂覆的纤维形成的无纺布、含有该无纺布的电化学电池、及该无纺布的制备方法 - Google Patents
由用有机粘合剂聚合物化合物涂覆的纤维形成的无纺布、含有该无纺布的电化学电池、及该无纺布的制备方法 Download PDFInfo
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- CN104136672B CN104136672B CN201380005669.3A CN201380005669A CN104136672B CN 104136672 B CN104136672 B CN 104136672B CN 201380005669 A CN201380005669 A CN 201380005669A CN 104136672 B CN104136672 B CN 104136672B
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Abstract
本发明涉及：一种无纺布，其中通过在制备无纺布时将形成无纺布的纤维提供于有机粘合剂聚合物化合物的溶液中而将粘合剂聚合物涂覆于纤维；使用所述无纺布用作隔膜材料的电化学装置；并且涉及无纺布的制备方法。在无纺布形成有0.001至10μm直径的孔，由此在确保锂离子的移动，同时实现隔膜所需的机械特性。另外，当无纺布用作电化学装置的隔膜时，不需要形成另外的粘合层的工艺，从而具有简化隔膜制备方法的效果。
Description
技术领域
本发明涉及由一种由用有机粘合剂聚合物化合物涂覆的纤维形成的无纺布、以含有该无纺布作为隔膜基底的电化学电池，并且涉及一种该无纺布的制备方法，并且更具体而言，涉及一种使用通过将已纺丝的网状纤维浸在有机粘合剂聚合物化合物溶液中而使有机粘合剂聚合物化合物涂覆在纤维，并且用涂覆有上述有机粘合剂聚合物化合物形成的无纺布作为隔膜基底的电化学电池。
本发明要求于2012年11月30日在韩国提交的韩国专利申请第10-2012-0138494号和于2013年11月29日在韩国提交的韩国专利申请第10-2013-0147402号的优先权，其公开内容以引用的方式纳入本说明书。
背景技术
近来，不断提高对储能技术的关注。由于储能技术的应用领域已经扩展至移动电话、摄像机、笔记本电脑甚至电动车，不断努力研究和开发电池。关于此，电化学电池引起了最大的关注。可充放电二次电池的开发已经是特别关注的焦点。在近些年中，已经进行了大量的研究和开发以设计新的电极和用于改进电池的容量密度和比能的电池。
在最近可得的二次电池中，在20世纪90年代初期开发的锂离子二次电池由于与使用电解质水溶液的常规电池如Ni-MH电池、Ni-Cd电池、H2SO4-Pb电池等相比具有更高的操作电荷和更高的能量密度的优点而受到了大量的关注。
通常，二次电池包括阴极、阳极、插入在阴极和阳极之间的隔膜、及电解质溶液，其中，隔膜是决定二次电池寿命的重要因素，并且起到使阴极与阳极电绝缘的作用。为了将其用作隔膜，优选具有高的离子渗透性和优异的机械强度，以及对电化学电池的电解质溶液的长期稳定性。
已经进行研究通过将为薄膜或者无纺布等的形式的隔膜材料中的聚烯烃基材料或耐热材料加工而用作隔膜，并且无纺布由于孔具有相对较大的直径而限制其应用，尽管其具有低成本的优点。
发明内容
技术问题
在本发明一个示例性的实施方案中，提供了一种由具有结合性或粘合力的纤维形成的无纺布，并且提供了所述无纺布的制备方法。
另外，提供了一种形成有相对较小直径的孔的无纺布基底的隔膜。
而且，在本发明一个示例性的实施方案中，提供一种所述无纺布的制备方法。
技术方案
根据本发明一个示例性的实施方案，提供一种由用有机粘合剂聚合物化合物涂覆的纤维形成的无纺布。
所述无纺布形成有0.001至10μm直径的孔。
有机粘合剂聚合物化合物可以为选自丙烯酰基粘合剂化合物、橡胶基粘合剂化合物、硅基粘合剂化合物和乙烯基醚基粘合剂化合物中的任何一种、或其两种以上的混合物。
所述纤维可以为将选自聚氨酯、聚烯烃基树脂如聚乙烯或聚丙烯；聚酰胺；热塑性聚氨酯；聚对苯二甲酸乙二醇酯；尼龙；及其共聚物中的任何一种或其两种以上的混合物通过纺丝来形成的纤维。
无纺布可以用作电化学电池的隔膜基底。
根据本发明的另一示例性的实施方案，提供了一种电化学电池，其包括阴极、阳极、插入在阴极和阳极之间的隔膜、及电解质，其中隔膜为上文所述隔膜。
电化学电池可以为锂二次电池。
根据本发明的另一示例性的实施方案，提供了一种使用了无纺布的隔膜的制备方法，所述方法包括将已纺织的纤维浸在有机粘合剂聚合物化合物溶液的步骤。
所述方法随后进一步包括在温度为100至200℃和压力为10至500MPa的条件下对涂覆有机粘合剂聚合物化合物溶液的纤维进行压延(calendering)的步骤。
所述纤维可以为将选自聚氨酯、聚烯烃基树脂如聚乙烯或聚丙烯；聚酰胺；热塑性聚氨酯；聚对苯二甲酸乙二醇酯；尼龙；及其共聚物中的任何一种、或其两种以上的混合物通过纺丝而获得的纤维。
有机粘合剂聚合物化合物溶液可以为丙烯酰基粘合剂化合物、橡胶基粘合剂化合物、硅基粘合剂化合物或乙烯基醚基粘合剂化合物溶解于溶剂的溶液，所述溶剂为选自：丙酮、甲基乙基酮、甲基异丁基酮、甲基溶纤剂、乙基溶纤剂、四氢呋喃、1,4-二氧杂环己烷、乙二醇二甲醚、乙二醇二乙醚、丙二醇二甲醚、丙二醇二乙醚、氯仿、二氯甲烷、1,2-二氯甲烷、1,1,1-三氯乙烷、1,1,2-三氯乙烷、1,1,2-三氯乙烷、1,2,3-三氯丙烷、己烷、庚烷、辛烷、环戊烷、环己烷、苯、甲苯、二甲苯、甲醇、乙醇、异丙醇、丙醇、丁醇、叔丁醇、丙二醇单甲醚、丙二醇单乙醚、丙二醇单丙醚、丙二醇单丁醚、二丙二醇二甲醚、二丙二醇二乙醚、二丙二醇单甲醚、甲基卡必醇、乙基卡必醇、丙基卡必醇、丁基卡必醇、环戊酮、环己酮、丙二醇甲基醚乙酸酯、丙二醇乙基醚乙酸酯、丙二醇甲基醚丙酸酯、3-甲氧基丁基乙酸酯、3-甲基-3-甲氧基丁基乙酸酯、乙基-3-乙氧基丙酸酯、乙基溶纤剂乙酸酯、甲基溶纤剂乙酸酯、乙酸丁酯、乙酸丙酯和乙酸乙酯中的一种或其两种以上的混合物。
有机粘合剂聚合物化合物溶液可以具有1至100厘泊(cp)的粘度。
有益效果
在本发明中制备的构成无纺布的纤维中，涂覆有有机粘合剂聚合物，并且在将无纺布用作基底的隔膜具有更小直径例如0.001至10μm直径的孔。因此，可以克服无纺布基底隔膜所固有的机械强度问题，同时确保锂离子的圆滑的移动。
而且，通过将无纺布用作电化学电池的隔膜中，因此无需形成另外的隔膜粘合剂层，从而具有简化隔膜制备过程的效果。
附图说明
图1至图3示意性地说明根据现有技术的无纺布的制备方法。
图4至图6示意性地说明本发明无纺布的制备方法。
图7为将根据本发明制备的无纺布放大3000倍的照片。
具体实施方式
在下文中，将详细描述本发明。在描述之前，应理解在说明书和附属权利要求中使用的术语不应理解为限制至常用的和字典的含义，而应以发明人可以为更好地解释而合适地定义术语的原理为基础，基于与本发明相应的技术方面的含义和概念而理解。因此，在此提出的描述仅为解释目的的优选的实例，不应理解为限制本发明的范围，所以应理解其他等价方案和改性方案在不偏离本发明实质和范围下也可以做出。
如在此所使用的，术语“无纺布”是指，由纤维通过将纤维以平行或无规则的方向排列而使纤维互相缠绕的机械处理，而没有对纤维进行织造过程而制备的产品。
在本发明中使用的无纺布，由可以用作电化学电池的隔膜的材料制成的网状(web)无纺布。这种无纺布维持一定程度的强度，并且伸缩性高，具有多孔性，而且具有防水透湿性。
如在此所使用的，术语“网状纤维”和“纤维”是指纺丝而形成无纺布的纤维，并且其可以互换使用。
在本发明中，形成无纺布的纤维的非限制性的实例包括选自聚氨酯、聚烯烃基树脂如聚乙烯或聚丙烯；聚酰胺；热塑性聚氨酯；聚对苯二甲酸乙二醇酯；尼龙；及其共聚物中的任何一种、或其两种以上的混合物。而且，在本发明中，无纺布的形成材料可以由至少两种类型材料制成，并且除相同类型的细丝纤维之外，可以使用不同类型的细丝纤维，优选地，例如，含有至少一种聚烯烃组分的双组分纤维。
本发明一个示例性的实施方案的无纺布的制备方法没有特殊限制，只要可包括将已纺丝的纤维浸在有机粘合剂聚合物化合物溶液中的工艺，并且非限制性的实例可以包括使用造纸方法的湿纺法。在本发明中不特别限制纺丝条件，并且可以对应于本领域的通常条件。
纺丝的纤维直径通常为20μm或更小，并且例如可以是0.5至18μm或1至15μm。纤维的横截面可以具有各种形状，通常圆形或椭圆形、表面上具有沟槽、小的条状、三角形或多边形等。
纤维的单位面积重量为5至20g/m2，然而本发明不限于此。
本发明一个示例性的实施方案的无纺布纤维，用有机粘合剂聚合物化合物涂覆。其实例解释于图7，并且可以看出纤维被有机粘合剂聚合物化合物所涂覆(由箭头所表示)。由于纤维自身被有机粘合剂聚合物化合物涂覆，所以即使在由纤维形成的无纺布无需使用另行的粘合层或粘合剂等，无纺布本身也具有结合性或粘合力。
例如，当由涂覆有有机粘合剂聚合物化合物的纤维而形成的隔膜插入在阴极和阳极之间，并且在施加80至150℃的热量和压力而进行层压时，即使不包括另行的粘合层，也可以形成隔膜与电极之间的粘合，并且在该情况下，粘合力水平为10至100gf/25mm。在此，“粘合力水平”是指，当以100mm/min和180度拉伸隔膜时所测量的力。
在该情况下，橡胶基粘合性化合物的非限制性的实例包括合成聚异戊二烯橡胶、苯乙烯-异戊二烯-苯乙烯嵌段共聚物、天然橡胶、聚异丁烯、聚丁烯等。
丙烯酰基粘合性化合物的非限制性的实例可以包括丙烯酸酯基单体的均聚物或共聚物，所述丙烯酸酯基单体包括丙烯酸丁酯、丙烯酸异壬基酯和丙烯酸2-乙基己酯，或该丙烯酸酯基单体和另外包括丙烯酸、丙烯酸2-羟基乙酯、乙酸乙酯的单体的共聚物。
构成无纺布的网状纤维可以通过本领域已知的常用方法来形成为无纺布基底，并且除单层结构之外，根据需要使无纺布基底可以以多层结构使用以提供各种特性。多层结构不限于各种类型的无纺布基底层叠的结构，并且包括以其他各种塑料膜、无纺布、多孔层等的不同类型基底层叠的结构。
在无纺布基底形成的孔径和无纺布基底的厚度，可以基于纤维的直径而不同，其程度为在制备无纺布等过程中纤维积累的程度等，并且可以通过压延工艺而调节。在一个示例性的实施方案中，在无纺布基底形成的孔当用毛细管流量气孔计(capillary flowporometer)测量时具有的直径范围为0.001至10μm，并且当孔径落在该范围内时，可以确保锂离子的有利的移动。
而且，无纺布基底的厚度可以为0.1至100μm或者5至50μm。从弹性、可加工性、耐久性、防止不需要的体积增加的方面看，无纺布基底的厚度满足该范围是优选的。
无纺布基底的渗透率范围为1至10sec/100mL。
本发明另一示例性的实施方案涉及多孔网状无纺布的制备方法。
现有的无纺布的制备方法的实施方案示例性地示于图1至图3中。根据该现有技术，所述制备方法包括：将网状纤维2通过纺丝设备1在常规溶液3中纺丝的步骤(图1)；干燥网状纤维2的步骤(图2)；通过压延辊4对已干燥的网状纤维2进行压延的步骤(图3)。在此，“常规溶液”是指不包含有机粘合剂聚合物的溶液。随后，为使无纺布具有粘合力，在常规方法中另外进行形成粘合层的步骤。
根据本发明一个示例性的实施方案的制备方法示例性地示于图4至图6中。根据本发明，所述方法包括：将通过纺丝设备1纺丝的网状纤维2浸至粘合剂聚合物化合物溶液的步骤(图4)；使形成有粘合剂聚合物化合物涂层6的网状纤维2干燥的步骤(图5)；通过压延辊4在已干燥的网状纤维2具有目标孔径的温度和压力条件下对已干燥的网状纤维2进行压延的步骤(图6)。这样制备的非纺丝网状纤维具有结合性或粘合力。
在本说明书中，有机粘合剂聚合物化合物溶液是指，丙烯酰基粘合剂化合物、橡胶基粘合剂化合物、硅基粘合剂化合物或乙烯基醚基粘合剂化合物包含在溶剂中的溶液。所述溶剂可以使用选自：丙酮、甲基乙基酮、甲基异丁基酮、甲基溶纤剂、乙基溶纤剂、四氢呋喃、1,4-二氧杂环己烷、乙二醇二甲醚、乙二醇二乙醚、丙二醇二甲醚、丙二醇二乙醚、氯仿、二氯甲烷、1,2-二氯甲烷、1,1,1-三氯乙烷、1,1,2-三氯乙烷、1,1,2-三氯乙烷、1,2,3-三氯丙烷、己烷、庚烷、辛烷、环戊烷、环己烷、苯、甲苯、二甲苯、甲醇、乙醇、异丙醇、丙醇、丁醇、叔丁醇、丙二醇单甲醚、丙二醇单乙醚、丙二醇单丙醚、丙二醇单丁醚、二丙二醇二甲醚、二丙二醇二乙醚、二丙二醇单甲醚、甲基卡必醇、乙基卡必醇、丙基卡必醇、丁基卡必醇、环戊酮、环己酮、丙二醇甲基醚乙酸酯、丙二醇乙基醚乙酸酯、丙二醇甲基醚丙酸酯、3-甲氧基丁基乙酸酯、3-甲基-3-甲氧基丁基乙酸酯、乙基-3-乙氧基丙酸酯、乙基溶纤剂乙酸酯、甲基溶纤剂乙酸酯、乙酸丁酯、乙酸丙酯和乙酸乙酯中的一种、或其两种以上的混合物，但并不限于此。从纤维上粘合剂聚合物化合物在纤维中均匀地涂覆的方面看，粘合剂聚合物化合物溶液优选具有1至100厘泊(cp)范围的粘度。
所述粘合剂聚合物化合物视需要可以进一步包括各种添加剂，例如含有多元醇如丙三醇、聚乙二醇和聚丙二醇的增塑剂、水溶性或吸水性树脂如聚丙烯酸、交联聚丙烯酸和聚乙烯基吡咯烷酮、松香基增粘剂、萜烯基增粘剂或石油基增粘剂软化剂、填料、颜料等。
涂覆有粘合剂聚合物化合物的网状纤维，可以在40至100℃的温度下以本领域的通常方式干燥1至10分钟。从可以在短时间内进行干燥并防止纤维或粘合剂聚合物的熔融的方面看，干燥温度在所述范围内是优选的。
干燥后，网状纤维可以在100至200℃的温度范围下进行压延。当压延温度满足该范围时，可以切实地实现无纺布的拉伸强度和纤维之间的间隙，并且可以防止以纺丝的纤维和粘合剂聚合物的熔融。
而且，压延压力可以设定为为1至10巴。当从无纺布的拉伸强度、纤维之间的间隙、及滚筒耐久性的方面看，压延压力满足上述范围是优选的。
如上所述，制备的无纺布对其用途无特殊限制，尤其，可以用作电化学电池的隔膜。
对可以与本发明的隔膜一起使用的电极无特别限定，并且可以通过本领域已知的通常方法，将电极活性材料粘结在电极集电器的状态制备。
在上述电极活性材料中，阴极活性材料的非限制性的实例可以采用可用于常规电化学电池的阴极的通常阴极活性材料，尤其可以使用锂镁氧化物、锂钴氧化物、锂镍氧化物、锂铁氧化物或组合这些的锂复合氧化物。
阳极活性材料的非限制性的实例可以使用可用于现有电化学电池的阳极中的通常阳极活性材料，尤其可以使用吸附/脱附锂的材料如锂金属或锂合金、碳、石油焦(petroleum coke)、活性炭、石墨或其他碳类等。
阴极集电器的非限制性的实例可以为由铝、镍或由这些的结合制成的箔等，阳极集电器的非限制性的实例可以为由铜、金、镍或铜合金，或由这些结合制成的箔。
可以用于本发明的电解质溶液可以为如A+B-结构的电解质盐溶解或解离于电解质溶剂中的电解质溶液，在电解质盐中，A+A+包括如Li+、Na+和K+的碱金属阳离子或这些的结合而成的离子，B-包括如PF6 -、BF4 -、Cl-、Br-、I-、ClO4 -、AsF6 -、CH3CO2 -、CF3SO3 -、N(CF3SO2)2 -和C(CF2SO2)3 -的阴离子或这些的结合而成的离子，所述溶剂可以选自碳酸亚丙酯(PC)、碳酸亚乙酯(EC)、碳酸二乙酯(DEC)、碳酸二甲酯(DMC)、碳酸二丙酯(DPC)、二甲基亚砜、乙腈、二甲氧基乙烷、二乙氧基乙烷、四氢呋喃、N-甲基-2-吡咯烷酮(NMP)、碳酸乙基甲酯(EMC)、γ-丁内酯、或其混合物，但并不限于此。
对于电解液的注入而言，根据最终产品的制备工艺和所需的物理特性，可以用在电池的制备工艺中的合适的步骤进行。即，电解液的注入可以在电池组装前或者在电池组装的最后步骤等进行。
根据本发明的电极视需要可以选择性地进一步包括导电材料、粘合剂、填料等成分。
导电材料可以包括但不限于乙炔黑、或炭黑等。
粘合剂可以为选自聚四氟乙烯、聚偏二氟乙烯、聚氟乙烯、聚丙烯腈、腈橡胶、聚丁二烯、聚苯乙烯、苯乙烯丁二烯橡胶、聚硫化物橡胶、丁基橡胶、氢化苯乙烯丁二烯橡胶、硝化纤维素和羧甲基纤维素中的一种以上。
根据本发明的电池可以通过本领域已知的常用方法制备，例如以使电极活性材料和粘合剂分散于有机溶剂而制备浆料，然后将该浆料涂布在电极集电器后将所得物干燥和压缩，而后将隔膜插入在阴极与阳极之间而制备，然而本发明不限于此。
Claims (10)
1.一种用于电化学电池的隔膜，其中，所述隔膜是通过使用无纺布作为基底而形成的；
所述的无纺布是籍由将已纺织的纤维浸在有机粘合剂聚合物化合物的溶液中，通过用该有机粘合剂聚合物化合物涂覆而得的具有结合性或粘合力的纤维来形成的；
所述有机粘合剂聚合物化合物为选自丙烯酰基粘合剂化合物、橡胶基粘合剂化合物、硅基粘合剂化合物和乙烯基醚基粘合剂化合物中的一种或其两种以上的混合物。
2.根据权利要求1的隔膜，其中，所述无纺布具有0.001至10μm直径的孔。
3.根据权利要求1的隔膜，其中，所述纤维由选自聚氨酯、聚烯烃基树脂、聚酰胺、热塑性聚氨酯、聚对苯二甲酸乙二醇酯、尼龙及其共聚物中的一种或其两种以上的混合物纺丝而成。
4.一种电化学电池，其包括阴极、阳极、插入在阴极和阳极之间的隔膜、及电解质，其中，
所述隔膜为权利要求1-3中的任一权利要求所述的隔膜。
5.根据权利要求4的电化学电池，其特征在于，
所述电化学电池为锂二次电池。
6.一种使用无纺布制备用于电化学电池的隔膜的方法，所述无纺布由具有结合性或粘合力的纤维形成，所述方法包括：
将已纺织的纤维浸在有机粘合剂聚合物化合物的溶液中；
所述有机粘合剂聚合物化合物为选自丙烯酰基粘合剂化合物、橡胶基粘合剂化合物、硅基粘合剂化合物和乙烯基醚基粘合剂化合物中的一种或其两种以上的混合物。
7.根据权利要求6的方法，进一步包括：
随后在温度为100至200℃和压力为10至500MPa下对涂覆有有机粘合剂聚合物化合物溶液的纤维进行压延的步骤。
8.根据权利要求6的方法，其特征在于，
所述纤维通过将选自聚氨酯、聚烯烃基树脂、聚酰胺、热塑性聚氨酯、聚对苯二甲酸乙二醇酯、尼龙及其共聚物中的任何一种或其两种以上的混合物纺丝而获得。
9.根据权利要求6的方法，其中所述溶剂为选自丙酮、甲基乙基酮、甲基异丁基酮、甲基溶纤剂、乙基溶纤剂、四氢呋喃、1,4-二氧杂环己烷、乙二醇二甲醚、乙二醇二乙醚、丙二醇二甲醚、丙二醇二乙醚、氯仿、二氯甲烷、1,2-二氯甲烷、1,1,1-三氯乙烷、1,1,2-三氯乙烷、1,1,2-三氯乙烷、1,2,3-三氯丙烷、己烷、庚烷、辛烷、环戊烷、环己烷、苯、甲苯、二甲苯、甲醇、乙醇、异丙醇、丙醇、丁醇、叔丁醇、丙二醇单甲醚、丙二醇单乙醚、丙二醇单丙醚、丙二醇单丁醚、二丙二醇二甲醚、二丙二醇二乙醚、二丙二醇单甲醚、甲基卡必醇、乙基卡必醇、丙基卡必醇、丁基卡必醇、环戊酮、环己酮、丙二醇甲基醚乙酸酯、丙二醇乙基醚乙酸酯、丙二醇甲基醚丙酸酯、3-甲氧基丁基乙酸酯、3-甲基-3-甲氧基丁基乙酸酯、乙基-3-乙氧基丙酸酯、乙基溶纤剂乙酸酯、甲基溶纤剂乙酸酯、乙酸丁酯、乙酸丙酯和乙酸乙酯中的一种或其两种以上的混合物。
10.根据权利要求6的方法，其中所述有机粘合剂聚合物化合物溶液具有为1至100厘泊的粘度。
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| KR1020130147402A KR101546481B1 (ko) | 2012-11-30 | 2013-11-29 | 유기 바인더 고분자 화합물로 피복되어 있는 섬유로 형성된 부직포, 이러한 부직포를 포함하고 있는 전기화학소자 및 상기 부직포의 제조방법 |
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| CN108140787B (zh) * | 2015-08-17 | 2022-01-04 | 赛尔格有限责任公司 | 改进的电池隔板和相关方法 |
| JP6848051B2 (ja) * | 2017-03-28 | 2021-03-24 | 株式会社東芝 | 電極構造体および二次電池 |
| CN108539251A (zh) * | 2018-05-09 | 2018-09-14 | 安徽宝岛新能源发展有限公司 | 一种电动汽车用便携式锂电池 |
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