CN1355940A - 适合作化学电池隔膜的复合材料 - Google Patents
适合作化学电池隔膜的复合材料 Download PDFInfo
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- CN1355940A CN1355940A CN00808739A CN00808739A CN1355940A CN 1355940 A CN1355940 A CN 1355940A CN 00808739 A CN00808739 A CN 00808739A CN 00808739 A CN00808739 A CN 00808739A CN 1355940 A CN1355940 A CN 1355940A
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Classifications
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Abstract
本发明涉及一种复合体,它具有至少1个包含一种组合物的第1层,该组合物包含(a)1~99wt%主粒度为5nm~100μm的固体(I),或由至少2种固体组成的混合物,(b)99~1wt%聚合物粘结剂(II),可由下列物质聚合获得:b1)以粘结剂(II)为基准5~100wt%下列成分的缩合产物(III),即,(α)至少1种化合物IV,它能与羧酸或与磺酸或与其衍生物或与它们中2或更多种的混合物起反应,以及(β)每摩尔化合物IV至少1摩尔具有至少1个能自由基聚合的官能团的羧酸或磺酸(V),或其衍生物,或它们中2或更多种的混合物,以及b2)以粘结剂(II)为基准0~95wt%另一种化合物(VII),其平均分子量(数均)至少是5000,在其主链或侧链中具有聚醚链段,其中该至少1个层被施加到包含至少1个传统隔膜的至少1个第2层上。
Description
本发明涉及一种尤其适合作化学电池,优选可再充电电池,特别是锂电池和锂离子电池隔膜的复合材料,涉及这种隔膜及化学电池本身,还涉及制造此种复合材料的方法。
化学电池,特别是可再充电化学电池通常是已知的,已在例如《Ullmann工业化学大全》(Ullmann’s Encyclopedia of IndustrialChemistry)第5版,卷A3,VCH出版社,Weinheim,1985,pp.343~397页中做了充分描述。
这类电池当中,锂电池和锂离子电池,由于具有高比能储存密度而占据特殊地位,尤其是作为蓄电池。
此类型电池,特别是按照Ullmann的上述节选段落的描述,在阴极中包含锰、钴、钒或镍之类的锂化复合氧化物。例如,它们,按最简单化学计量的情况可描述为LiMn2O4、LiCoO2、LiV2O5或LiNiO2。
这些复合氧化物可与能够在晶格中结合进锂离子的化合物,如石墨发生可逆反应,结果从晶格中移出锂离子,在此过程中金属离子如锰、钴或镍则被氧化。该反应可应用到化学电池中用以储存电能,其中,用电解质将能接受锂离子的化合物,也就是阳极材料,与含锂的复合氧化物,也就是阴极材料,彼此隔开,于是形成复合氧化物的锂离子可通过该电解质迁移到阳极材料中(充电过程)。
适合用来可逆地储存锂离子的化合物通常利用粘结剂固定在集电极上。
电池充电期间,电子流过外电压源,同时锂阳离子流过电解质到达阳极材料。电池使用期间,锂阳离子流过电解质,而电子则从阳极材料流经负载来到阴极材料。
为避免化学电池内出现短路,在这2个电极之间设置电绝缘但容许锂阳离子透过的层。这可以是所谓固态电解质或传统隔膜。
众所周知,固态电解质和隔膜由载体材料组成,在载体材料中结合着含有锂阳离子并起到提高锂离子电导率作用的可离解化合物,另外通常还包括其他添加剂如溶剂。
微孔膜作为隔膜的建议已提出一些时候了。例如,GB 2 027 637描述了一种微孔膜,它包含一种基质,该基质由40~90%(体积)聚烯烃和10~60%(体积)无机填料以及文中一一规定的其他成分组成。文中所描述的基质具有,以薄膜体积为基准30~95%(体积)孔隙,是一种铅蓄电池用的隔膜。
EP-B 0 715 364描述了一种具有断路(Shutdown)特性的双层电池隔膜。文中所描述的电池隔膜具有第1微孔膜,具有断路功能,该微孔膜由选自聚乙烯、以聚乙烯为主的共混物以及聚乙烯共聚物的材料制成。该隔膜还具有第2微孔膜,该膜具有增强功能,由选自聚丙烯、以聚丙烯为主的共混物以及聚丙烯共聚物的材料制成。按该文献的描述,此种隔膜具有优于先有技术的机械强度和转变能。
EP-A 0 718 901描述一种具有断路特性的三层电池隔膜。该隔膜包含第1和第3微孔聚丙烯膜,后者又包括微孔聚乙烯膜,其中第1和第3膜具有比第2膜大的耐击穿能力和较高熔点。
EP-A-0 708 791描述一种膜形式的复合聚合物电解质,它具有施涂到多孔聚四氟乙烯膜制成的基质材料上的离子导电聚合物凝胶。
DE-A 198 59 826.3描述一种适合作化学电池中隔膜的复合材料,包含传统层状隔膜,以及至少1个其他层,其中它们包含固体和聚合物粘结剂,该粘结剂是一种具有当受到加热和/或紫外辐照时能发生交联反应的活性链中基、端基和/或侧基的聚合物或共聚物。
本发明的目的,考虑到该项先有技术,首先是提供一种隔膜,它同样具有断路机制,而且还具有高温(>150℃)尺寸稳定性,以及进一步改善的机械强度,另外还具有卓越离子导电性能,或是描述DE-A 19850 826.3的复合材料的替代体系。
因此,本发明涉及一种复合材料,它包含至少1个第1层,该层包含含有下列成分的组合物,
(a)1~99wt%主粒度(Primrpartikelgrβe)为5nm~100μm的固体(I),或由至少2种固体组成的混合物,
(b)99~1wt%聚合物粘结剂(II),可由下列物质聚合获得:
b1)以粘结剂(II)为基准5~100wt%下列成分的缩合产物III,
α)至少1种化合物IV,它能与羧酸或磺酸或衍生物或与它们中2或更多种的混合物起反应,以及
β)每摩尔化合物IV至少1摩尔具有至少1个能自由基聚合官能团的羧酸或磺酸V,或其衍生物,或它们中2或更多种的混合物,
以及
b2)以粘结剂(II)为基准0~95wt%另一种化合物VII,其平均分子量(数均)至少是5000,在其主链或侧链中具有聚醚链段,
其中该至少1个第1层被施加到包含至少1个传统隔膜的至少1个第2层上。
本发明还涉及上述类型的复合材料,其中聚合物粘结剂(IIA)可由下列物质的聚合获得,
b1)以粘结剂(IIA)为基准5~75wt%不同于羧酸或磺酸V或其衍生物但能发生自由基聚合的化合物VI,或其2或更多种的混合物,
以及
b2)以粘结剂(IIA)为基准25~95wt%另一种化合物VII,其平均分子量(数均)至少是5000,在其主链或侧链中具有聚醚链段。
下面,详细描述该至少1个第1层中含有的组合物及其制备。
固体I优选地选自无机固体,优选为无机碱性固体,选自元素周期表主族I、II、III或IV或过渡族IV元素的氧化物、混合氧化物、碳酸盐、硅酸盐、硫酸盐、磷酸盐、氨化物、亚氨化物、氮化物和碳化物;选自聚乙烯、聚丙烯、聚苯乙烯、聚四氟乙烯、聚偏二氟乙烯、聚酰胺和聚酰亚胺的聚合物;包含此类型聚合物的固态分散体;玻璃粉、纳米玻璃颗粒如Monosper(Merck)、微米玻璃颗粒如Spheriglas(Potters-Ballotini)、纳米须晶及其2或更多种的混合物,其中获得的组合物可用作固体电极和/或隔膜。
术语“固体III”包含任何在标准条件下呈固体的化合物,只要在电池,特别是锂离子电池充电期间的主导条件下,电池操作期间,既不接受也不释放电子。
作为该层中的固体III使用的化合物首先是无机固体,优选无机碱性固体,选自元素周期表主族I、II、III或IV或过渡族IV元素的氧化物、混合氧化物、硅酸盐、硫酸盐、碳酸盐、磷酸盐、氮化物、氨化物、亚氨化物和碳化物;选自聚乙烯、聚丙烯、聚苯乙烯、聚四氟乙烯、聚偏二氟乙烯、聚酰胺和聚酰亚胺的聚合物;包含此类型聚合物的固态分散体;以及它们当中2或更多种的混合物。
作为例子还可举出的特别是:氧化物,例如二氧化硅、氧化铝、氧化镁或二氧化钛,复合氧化物,例如元素硅、钙、铝、镁、钛的复合氧化物;硅酸盐,例如梯形硅酸盐、链硅酸盐、层硅酸盐(Schichtsilicate)和骨架硅酸盐(Gerüstsilicate),例如滑石、叶蜡石、Muskovit、金云母(Phlogopit)、闪石、岛硅酸盐、辉石、Sorosilicate、沸石、长石、硅灰石,特别是疏水化的硅灰石、云母、层硅酸盐;硫酸盐如碱金属硫酸盐和碱土金属硫酸盐;碳酸盐如碱金属碳酸盐和碱土金属碳酸盐,如钙、镁或钡的碳酸盐或者锂、钾或钠的碳酸盐;磷酸盐,如磷灰石;氨化物;亚氨化物;氮化物;碳化物;聚合物,如聚乙烯、聚丙烯、聚苯乙烯、聚四氟乙烯、聚偏二氟乙烯、聚酰胺、聚酰亚胺或其他热塑性塑料、热固性塑料或微凝胶、交联聚合物颗粒如Agfaperl、固态分散体,特别是包含上述聚合物的那些,还有上述固体中的2或更多种的混合物。
本发明可使用的固体I还包含无机锂离子导电固体,优选是碱性无机锂离子导电固体。
这里提到的是:硼酸锂,例如Li4B6O11*xH2O、Li3(BO2)3、Li2B4O7*xH2O、LiBO2,其中x可以是0~20的数;铝酸锂,例如Li2O*Al2O3*H2O、Li2Al2O4、LiAlO2;铝硅酸锂,例如含锂沸石、长石、长石替代物、层硅酸盐、链硅酸盐,特别是LiAlSi2O6(锂辉石)、LiAlSi4O10(Petullite)、LiAlSiO4(锂霞石),云母,例如K[Li,Al]3[AlSi]4O10(F-OH)2、K[Li,Al,Fe]3[AlSi]4O10(F-OH)2;锂沸石,特别是纤维状、片状或立方体状的,特别是通式为Li2/zO*Al2O3*xSiO2*yH2O的那些,其中z对应于化合价,x介于1.8~约12,y介于0~约8;碳化锂,例如Li2C2、Li4C、Li3N;氧化锂以及复合氧化锂,例如LiAlO2、Li2MnO3、Li2O、Li2O2、Li2MnO4、Li2TiO3;Li2NH;LiNH2;磷酸锂,例如Li3PO4、LiPO3、LiAlFPO4、LiAl(OH)PO4、LiFePO4、LiMnPO4;Li2CO3;硅酸锂,包括梯形、链形、层形和骨架(Gerüst)形式的,例如Li2SiO3、Li2SiO4以及Li6Si2;硫酸锂,例如Li2SO4、LiHSO4和LiKSO4;以及作为化合物Ib提到的锂化合物,其中导电炉黑,倘若它被用作固体I的话,则应排除在外;以及上面提到的锂离子导电固体当中2或更多种的混合物。
优选的固体I是疏水化固体I,更优选上面提到类型的疏水化的化合物。
这里尤其合适的是碱性固体。就本发明目的而言,术语碱性固体是那些与某种本身pH不大于7的液态、含水稀释剂的混合物具有高于该稀释剂的pH的那些。
有利的是,该固体I应基本不溶解在用作电解质的液体中,并且在电池介质中应为电化学惰性的。
尤其合适的固体I是主粒度为5nm~20μm,优选0.01~10μm,特别是0.1~5μm的那些,给出的粒度是采用电子显微镜确定的。该颜料的熔点优选高于化学电池的一般操作温度;而熔点高于120℃,特别是高于150℃,已证明尤其有利。
这里的颜料就其外部形状而言可以是对称的,即,具有近似于1的高∶宽∶长度尺寸比例(长宽高比)并采取珠状或粒状、近似圆的形状,但也可以是任何要求的多面体形状,例如立方体、四面体、六面体、八面体或双棱锥,或者可以是扭曲的或不对称的,即,其高∶宽∶长度尺寸比例(长宽高比)不等于1,采取,例如针状、不对称四面体、不对称双棱锥、不对称六面体或八面体、薄片、小板或纤维状的形式。如果该固体为不对称颗粒形式,则上面提到的主粒度的上限指每种情况下的最小轴线而言。
本发明使用的组合物包含1~99wt%,优选15~90wt%,更优选25~85wt%,尤其是50~80wt%固体I,以及1~99wt%,优选10~85wt%,更优选15~75wt%,尤其是20~50wt%聚合物粘结剂II或IIA。
作为能与羧酸或磺酸V或衍生物或其2或更多种的混合物起反应的化合物IV的化合物,原则上可以是任何满足这一标准的化合物。
化合物IV优选地选自主链中唯一地包含碳原子的单羟基或多羟基醇;主链中除了包含至少2个碳原子之外还包含至少1个选自氧、磷和氮的原子的单羟基和多羟基醇;含硅化合物;含至少1个伯氨基基团的胺;含至少1个仲氨基基团的胺;氨基醇;单或多羟基硫醇;含至少1个硫醇基团和至少1个羟基基团的化合物;以及它们当中2或更多种的混合物。
这些当中,又优选含2或更多个能与羧酸或磺酸起反应的官能团的化合物IV。
倘若采用含氨基官能团的化合物IV,优选使用包含仲氨基基团的那些,这样,缩合/交联以后在粘结剂II中将会或者根本不存在游离NH基团,或者仅存在少量游离NH基团。
可提到的优选化合物详细地是:
主链中唯一地包含碳原子、具有1~20醇羟基基团,优选2~20,尤其是2~10个醇羟基基团的单羟基和多羟基醇,特别是二羟基、三羟基和四羟基醇,优选具有2~20个碳原子,例如是乙二醇、1,2-或1,3-丙二醇、1,2-或1,3-丁二醇、1,4-丁烯二醇或1,4-丁炔二醇、1,6-己二醇、新戊二醇、1,2-十二烷二醇、甘油、三羟甲基丙烷、季戊四醇和糖醇,氢醌、线型酚醛、双酚A,然而,正如从上面的定义清楚地看出的,也可采用单羟基醇,例如甲醇、乙醇、丙醇、正-、仲-或叔丁醇等;还可采用多羟基烯烃,优选具有2个端羟基基团的那些,例如α,ω-二羟基丁二烯;
聚酯多元醇,例如公开在《Ullmann工业化学大全》,第4版,卷19,62~65页中的那些,该化合物例如可通过二羟基醇与多元,优选二元多羧酸之间的反应制取;
主链中除了包含至少2个碳原子之外还包含至少1个氧原子的单羟基和多羟基醇,优选聚醚醇,例如亚烷基环氧化物,例如环氧异丁烷、环氧丙烷、环氧乙烷、1,2-环氧丁烷、1,2-环氧戊烷、1,2-环氧己烷、四氢呋喃、氧化苯乙烯的聚合产物;也可使用端基经过改性的聚醚醇,例如利用NH2端基改性的聚醚醇;这些醇优选的分子量(数均)为100~5000,更优选200~1000,尤其是300~800;此类化合物本身是已知的并且可按商品名Pluriol或P1uronic(BASF股份公司)从市场上购得;
如上面所定义的醇,其中某些或全部碳原子已被硅取代,这里尤其可使用聚硅氧烷或氧化烯-硅氧烷共聚物,或者聚醚醇与聚硅氧烷的混合物,例如描述在EP-B 581 296和EP-A 525 728中的;上面所说的也适用于这类醇的分子量;
如上面所定义的醇,尤其是聚醚醇,其中某些或全部氧原子已被硫原子取代的;上面所说的也适用于这类醇的分子量;
主链中除了包含至少2个碳原子之外还包含至少1个磷原子或至少1个氮原子的单羟基和多羟基醇,例如二乙醇胺和三乙醇胺;
由通式OH-(CH2)z-COOH的化合物衍生的内酯,其中z是1~20的数,例如ε-己内酯、β-丙内酯、γ-丁内酯或甲基-ε-己内酯;
含硅化合物,例如二-和三氯甲硅烷、苯基三氯甲硅烷、二苯基二氯甲硅烷或二甲基乙烯基氯甲硅烷;硅烷醇,例如三甲基硅烷醇;
含至少1个伯氨基和/或仲氨基基团的胺,例如丁胺、2-乙基己胺、乙二胺、六亚甲基二胺、二亚乙基三胺、四亚乙基五胺、五亚乙基六胺、苯胺或苯二胺;
聚醚二胺,例如,4,7-二氧基-癸烷-1,10-二胺和4,11-二氧基十四烷基-1,14-二胺;
单-或多羟基硫醇,例如脂族硫醇,例如甲硫醇、乙硫醇、环己烷硫醇、十二烷硫醇;芳族硫醇,例如苯硫酚、4-氯苯硫酚和2-巯基苯胺;
含至少1个巯基基团和至少1个羟基基团的化合物,例如,4-羟基-苯硫酚或上面定义的多羟基醇的单硫代衍生物;
氨基醇,例如乙醇胺、N-甲基-乙醇胺、N-乙基乙醇胺、N-丁基乙醇胺、2-氨基-1-丙醇和2-氨基-1-苯基乙醇,含2个以上与脂族键合的羟基基团的单-和多氨基多元醇,例如三(羟甲基)甲胺、葡糖胺和N,N’-双(2-羟乙基)乙二胺。
也可使用2或更多种上面所描述的化合物IV的混合物。
上述化合物IV,按照本发明,能与含至少1个可自由基聚合官能团的羧酸或磺酸V或其衍生物或其2或更多种的混合物进行缩合。化合物IV中的游离的、能缩合基团当中至少1个,优选全部,都与化合物V发生缩合。
就本发明而言,羧酸或磺酸V原则上可以是任何含至少1个可自由基聚合官能团的羧酸和磺酸以及其衍生物。这里所使用的术语“衍生物”既涵盖由在酸官能团上改性的由羧酸或磺酸衍生的化合物,例如酯、酰卤或酸酐,也涵盖由在羧酸或磺酸碳骨架上改性的由羧酸或磺酸衍生的化合物,例如卤代羧酸或卤代磺酸。
这里,作为化合物V,可特别举出下面的化合物:
α,β-不饱和羧酸或β,γ-不饱和羧酸。
这里特别合适的α,β-不饱和羧酸是下列通式的那些,其中R1、R2和R3是氢或C1-~C4-烷基基团,这些当中,丙烯酸和甲基丙烯酸又是优选的;也可成功地使用肉桂酸、马来酸、富马酸、衣康酸和对乙烯基苯甲酸,以及它们的衍生物,例如酸酐,如马来酐和衣康酸酐;
卤化物,特别是氯化物,例如丙烯酰或甲基丙烯酰氯;
酯,例如烷基基团中包含最高20个碳原子的(甲基)丙烯酸(环)烷基酯,如(甲基)丙烯酸的甲基、乙基、丙基、丁基、己基、2-乙基己基、十八烷基、月桂基、环己基、苄基、三氟甲基、六氟丙基或四氟丙基酯,聚丙二醇的单(甲基)丙烯酸酯、聚乙二醇的单(甲基)丙烯酸酯、多羟基醇的多(甲基)丙烯酸酯,例如甘油的二(甲基)丙烯酸酯、三羟甲基丙烷的二(甲基)丙烯酸酯、季戊四醇的二-或三(甲基)丙烯酸酯、二甘醇的双(单-(2-丙烯酰氧基)乙基)碳酸酯、本身又包含可自由基聚合基团的醇的多(甲基)丙烯酸酯,例如(甲基)丙烯酸与乙烯基和/或烯丙基醇的酯;
其他脂族或芳族羧酸的乙烯基酯,例如
乙酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、己酸乙烯酯、辛酸乙烯酯、癸酸乙烯酯、硬脂酸乙烯酯、棕榈酸乙烯酯、巴豆酸乙烯酯、己二酸二乙烯酯、癸二酸二乙烯酯、2-乙基己酸乙烯酯、三氟乙酸乙烯酯;
其他脂族或芳族羧酸的烯丙基酯,例如
乙酸烯丙基酯、丙酸烯丙基酯、丁酸烯丙基酯、己酸烯丙基酯、辛酸烯丙基酯、癸酸烯丙基酯、硬脂酸烯丙基酯、棕榈酸烯丙基酯、巴豆酸烯丙基酯、水杨酸烯丙基酯、乳酸烯丙基酯、草酸二烯丙基酯、丙二酸二烯丙基酯、琥珀酸二烯丙基酯、戊二酸二烯丙基酯、己二酸二烯丙基酯、庚二酸二烯丙基酯、肉桂酸二烯丙基酯、马来酸二烯丙基酯、邻苯二甲酸二烯丙基酯、间苯二甲酸二烯丙基酯、1,3,5-苯三羧酸三烯丙基酯、三氟乙酸烯丙基酯、全氟丁酸烯丙基酯和全氟辛酸烯丙基酯;
β,γ-不饱和羧酸及其衍生物,例如乙烯基乙酸、2-甲基乙烯基乙酸、3-丁烯酸异丁酯、3-丁烯酸烯丙基酯、2-羟基-3-丁烯酸烯丙基酯或双烯酮;
磺酸,例如乙烯基磺酸、烯丙基-和甲基烯丙磺酸以及它们的酯和卤化物,苯磺酸乙烯酯,4-乙烯基苯磺酰胺。
也可使用2或更多种上面所描述的羧酸和/或磺酸的混合物。
至于能发生可用于制备粘结剂(IIA)的自由基聚合的化合物VI,可举出的具体例子是:烯烃,例如乙烯、丙烯、丁烯、异丁烯、己烯或高级同系物和乙烯基环己烷;
(甲基)丙烯腈;
含卤烯烃化合物,例如偏二氟乙烯、偏二氯乙烯、氟乙烯、氯乙烯、六氟丙烯、三氟丙烯、1,2-二氯乙烯、1,2-二氟乙烯和四氟乙烯;
乙烯醇、醋酸乙烯酯、N-乙烯基吡咯烷酮、N-乙烯基咪唑以及乙烯基甲酰胺;
氯化氮化磷,例如二氯化氮化磷、六氯(三磷腈),还有它们被烷氧基、苯氧基、氨基或氟代烷氧基部分或完全取代的衍生物,即,可聚合生成聚磷腈的化合物;
芳族烯烃化合物,如苯乙烯或α-甲基苯乙烯;
乙烯基醚,例如甲基、乙基、丙基、异丙基、丁基、异丁基、己基、辛基、癸基、十二烷基、2-乙基己基、环己基、苄基、三氟甲基、六氟丙基或四氟丙基的乙烯基醚。
当然,也可使用上述化合物VI的混合物,在这种情况下将生成共聚物,依制备类型而定,这些产物将包含无规分布的单体,或者代表嵌段共聚物。
该化合物VI,如同缩合产物III一样,可按本领域技术人员已知的惯用方法,优选用自由基聚合方法进行聚合,下面涉及到化合物VII的讨论适用于这里所获得的分子量。
可用的化合物VII首先是平均分子量(数均)至少是5000,优选5000~20,000,000,尤其是100,000~6,000,000的、能使锂阳离子溶剂化并起到粘结剂作用的化合物。合适的化合物VII例如是含有,以化合物VII总重量为基准至少30wt%下列结构单元的聚醚和共聚物:其中R1、R2、R3和R4可以是芳基基团、烷基基团,优选甲基基团或氢,可相同或不同,并且可包含杂原子如氧、氮、硫或硅。
此类化合物例如描述在:M.B.Armand等人,《固体中的快速离子传输》(Fast Ion Transport in Solids),Elsevier,纽约,1979,131~136页,或者在FR-A 7832976中。
化合物VII也可由2或更多种此类化合物的混合物构成。
上面规定的聚合物粘结剂II和IIA也可采取泡沫体形式,在这种情况下固体I原样地分散在其中。
有利的是,化合物VII具有5,000~100,000,000,优选50,000~8,000,000的平均分子量(数均)。粘结剂II可通过,以粘结剂II为基准5~100wt%,优选30~70wt%至少1种缩合产物III与以粘结剂II为基准0~95wt%,优选30~70wt%化合物VII之间的反应制取。有利的是,粘结剂IIA的化合物VII具有5,000~100,000,000,优选50,000~8,000,000的平均分子量(数均)。粘结剂IIA可通过,以粘结剂IIA为基准5~75wt%,优选30~70wt%化合物VI与以粘结剂IIA为基准25~95wt%,特别是30~70wt%化合物VII之间的反应制取。
为制备本发明使用的1个层,可由固体I、缩合产物III以及,必要的话,化合物VII制成混合物,或者可由固体III、化合物VI以及化合物VII,还有惯用添加剂如增塑剂,优选含环氧乙烷或环氧丙烷的增塑剂,制成混合物。
可使用的其他聚合物VIII可包含热塑性塑料聚合物和离子导电聚合物。尤其应当提到的:
1)聚碳酸酯,例如聚碳酸亚乙基酯、聚碳酸亚丙基酯、聚碳酸丁二烯酯、聚碳酸亚乙烯基酯。
2)由下列物质制备的均聚物、嵌段聚合物和共聚物,
a)烯烃,例如乙烯、丙烯、丁烯、异丁烯、丙烯、己烯或更高级的同系物,丁二烯、环戊烯、环己烯、降冰片烯、乙烯基环己烷、1,3-戊二烯、1,3-、1,4-和1,5-己二烯、异戊二烯和乙烯基降冰片烯;
b)芳烃,例如苯乙烯和甲基苯乙烯;
c)丙烯酸酯或甲基丙烯酸酯,例如甲基、乙基、丙基、异丙基、丁基、异丁基、己基、辛基、癸基、十二烷基、2-乙基己基、环己基、苄基、三氟甲基、六氟丙基和四氟丙基的丙烯酸酯以及它们的甲基丙烯酸酯;
d)丙烯腈、甲基丙烯腈、N-甲基吡咯烷酮、N-乙烯基咪唑和醋酸乙烯;
e)乙烯基醚,例如甲基、乙基、丙基、异丙基、丁基、异丁基、己基、辛基、癸基、十二烷基、2-乙基己基、环己基、苄基、三氟甲基、六氟丙基和四氟丙基的乙烯基醚;
f)含卤素烯烃化合物的聚合物和共聚物,例如偏二氟乙烯、偏二氯乙烯、氟乙烯、氯乙烯、六氟丙烯、三氟丙烯、1,2-二氯乙烯、1,2-二氟乙烯以及四氟乙烯的;优选的是,氯乙烯的、丙烯腈的或偏二氟乙烯的聚合物或共聚物;由氯乙烯与偏二氯乙烯,氯乙烯与丙烯腈,偏二氟乙烯与六氟丙烯,以及偏二氟乙烯与六氟丙烯等的共聚物;由偏二氟乙烯与六氟丙烯以及选自氟乙烯、四氟乙烯和三氟乙烯之一的单体制成的三元共聚物;特别是偏二氟乙烯与六氟丙烯制成的共聚物;进一步优选的是,包含75~92wt%偏二氟乙烯和8~25wt%六氟丙烯的共聚物;
g)2-乙烯基吡啶、4-乙烯基吡啶、碳酸亚乙烯基酯。
需要和/或希望的话,调节剂,例如硫醇,可在上述聚合物制备期间使用。
3)可由例如下列物质之间的反应制取的聚氨酯,
a)6~30个碳原子的有机二异氰酸酯,例如脂族、非环状二异氰酸酯,如1,5-六亚甲基二异氰酸酯和1,6-六亚甲基二异氰酸酯,脂族环状二异氰酸酯,如1,4-亚环己基二异氰酸酯、二环己基甲烷二异氰酸酯以及异佛尔酮二异氰酸酯,或者芳族二异氰酸酯,如2,4-亚甲苯二异氰酸酯、2,6-亚甲苯二异氰酸酯、间-四甲基二甲苯二异氰酸酯、对-四甲基二甲苯二异氰酸酯、1,5-四氢化萘二异氰酸酯以及4,4’-二亚苯甲烷二异氰酸酯或者这类型化合物的混合物,
与
b)多羟基醇,例如聚酯醇、聚醚醇以及二醇。
聚酯醇,有利的是,基本线型、具有端羟基基团,优选具有2或3个,特别是2个端羟基基团的聚合物。聚酯醇的酸值小于10,优选小于3。聚酯醇可以简单方式通过4~15个碳原子,优选4~6个碳原子的脂族或芳族二羧酸,与二醇,优选2~25个碳原子的二醇之间的酯化,或者通过3~20个碳原子内酯的聚合来制备。可使用的二羧酸例子是戊二酸、庚二酸、辛二酸、癸二酸、十二烷二酸以及,优选地己二酸和琥珀酸。合适的芳族二羧酸是对苯二甲酸、间苯二甲酸、邻苯二甲酸或者此种二羧酸与其他二羧酸的混合物,例如与联苯甲酸、癸二酸、琥珀酸和己二酸的混合物。二羧酸可单独使用或者作为混合物使用。为制备聚酯醇,必要时有利的可能是不使用二羧酸本身,而使用其对应的衍生物,例如羧酸酐或酰氯。适宜二醇的例子是二甘醇、1,5-戊二醇、1,10-癸二醇以及2,2,4-三甲基-1,5-戊二醇。优选使用1,2-乙二醇、1,3-丙二醇、2-甲基-1,3-丙二醇、1,4-丁二醇、1,6-己二醇、2,2-二甲基-1,3-丙二醇、1,4-二羟甲基环己烷、1,4-二羟乙基环己烷以及2,2-双(4-羟亚苯基)丙烷(双酚A)的乙氧基化或丙氧基化产物。依对聚氨酯所要求的性质而定,多元醇可单独使用,或者作为各种不同数量比的混合物使用。适合制备聚酯醇的内酯的例子是α,α-二甲基-β-丙内酯、γ-丁内酯以及,优选地,ε-己内酯。
所指聚醚醇为基本线型、具有羟基端基基团并含有醚键的物质。合适的聚醚醇可方便地通过环状醚,如四氢呋喃的聚合,或者通过1种或多种在亚烷基基团中含有2~4个碳原子的氧化烯,与亚烷基基团中键合着2个活性氢原子的启动分子起反应来制备。氧化烯的例子是环氧乙烷、1,2-环氧丙烷、表氯醇、1,2-环氧丁烷以及2,3-环氧丁烷。氧化烯可单独使用,依次交替使用或作为混合物使用。使用的启动分子的例子是水、二醇如乙二醇、丙二醇、1,4-丁二醇和1,6-己二醇,胺类如乙二胺、六亚甲基二胺和4,4’-二氨基二苯甲烷以及氨基醇,如乙醇胺。合适的聚酯醇和聚醚醇及其制备描述在,例如EP-B 416 386中,合适的聚碳酸酯二醇,优选基于1,6-己二醇的那些,以及它们的制备描述在,例如US-A 4 131 731中。
有利的是可使用,以醇总重量为基准最高30wt%具有2~20个碳原子,优选2~10个碳原子的脂族二醇,例如1,2-乙二醇、、1,3-丙二醇、1,4-丁二醇、1,6-己二醇、1,5-戊二醇、1,10-癸二醇、2-甲基-1,3-丙二醇、2,2-二甲基-1,3-丙二醇、2-甲基-2-丁基-1,3-丙二醇、2,2-二甲基-1,4-丁二醇、1,4-二羟甲基己烷、新戊二醇的羟基新戊酸酯、二甘醇、三甘醇和甲基二乙醇胺,或者具有8~30个碳原子的芳脂族或芳环脂族二醇,其中可能的是,芳族结构是杂环环体系或者优选地,是异构环状体系,例如萘衍生物或,特别是苯衍生物,如双酚A,两面(zweifach)对称地(被)乙氧基化的双酚A,两面对称地丙氧基化的双酚A,较高度乙氧基化的或丙氧基化的双酚A衍生物或双酚F衍生物,还有此类型化合物的混合物。
可能有利的是,使用以醇的总重量为基准最高5wt%具有3~15个碳原子,优选3~10个碳原子的脂族三元醇,例如三羟甲基丙烷或甘油,此类型化合物与环氧乙烷和/或环氧丙烷的反应产物,以及还有此类型化合物的混合物。
多羟基醇可具有官能团,例如中性基团如硅氧烷基团,碱性基,例如特别是,叔氨基基团,或者酸基团或其盐,或者很容易转化为酸基团的基团,它们可通过多羟基醇(的反应)引入的基团。可能有利的是使用具有此类型基团的二醇组分,例如N-甲基二乙醇胺、N,N-双(羟乙基)氨甲基膦酸二乙基酯或3-磺基丙基的N,N-双(羟乙基)-2-氨基乙酸酯,或者具有此类型基团、可用于制备聚酯醇的二羧酸,例如5-磺基间苯二甲酸。
酸基团尤其是磷酸、膦酸、硫酸、磺酸、羧酸或铵基团。
很容易转变为酸基团的基团例子是酯基团或盐,优选碱金属,例如锂、钠或钾的盐。
4)上面所描述的聚酯醇本身,此时注意应达到10,000~2,000,000,优选50,000~1,000,000的分子量。
5)聚胺,聚硅氧烷以及聚磷腈,特别是上面在描述聚合物IIb2时所讨论的那些。
6)聚醚醇,例如在上面讨论聚合物IIb1时作为化合物(c)的,或者在讨论聚氨酯时所描述的那些。
当然,也可使用上述聚合物VIII的混合物。本发明使用的共聚物VIII,视制备方式而定,可包含无规分布的单体,或者可以是嵌段共聚物。
聚合物VIII是按本领域技术人员已知的方式进行聚合的,优选按自由基聚合方式。聚合物VIII可以其高分子量或低聚物形式使用,或者作为其混合物使用。
聚合物VIII在聚合物粘结剂II至IIA中的比例一般介于0~99wt%,优选20~80wt%,更优选40~70wt%。
本发明优选提供一种复合材料,其第1层包含下列组合物:
如上面规定的第1层,其中聚合物VIII选自氯乙烯、丙烯腈、偏二氟乙烯的聚合物或共聚物;氯乙烯与偏二氯乙烯、氯乙烯与丙烯腈、偏二氟乙烯和六氟丙烯、偏二氟乙烯与六氟丙烯的共聚物;偏二氟乙烯与六氟丙烯以及选自氟乙烯、四氟乙烯和三氟乙烯之一的三元共聚物,并优选是偏二氟乙烯与六氟丙烯的共聚物。
本发明使用的组合物还可包含增塑剂IX。然而,也可在没有增塑剂的情况下操作。
使用的话,增塑剂IX的比例,以组合物为基准介于0.1~100wt%,优选0.5~50wt%,尤其是1~20wt%。
增塑剂IX的例子是DE-A 198 19 752中描述的那些,优选碳酸二甲酯、碳酸二乙酯、碳酸二丙酯、碳酸亚乙酯、碳酸1,2-亚丙酯、碳酸1,3-亚丙酯、有机磷化合物,特别是磷酸酯和膦酸酯,例如磷酸三甲酯、磷酸三乙酯、磷酸三丙酯、磷酸三丁酯、磷酸三(2-乙基己基)酯、聚氧化烯醚以及聚氧化烯酯,如二甘醇二甲醚(Diglyme)化合物,三甘醇二甲醚(Triglyme)化合物,以及四甘醇二甲醚(Tetraglyme)化合物;聚合物增塑剂,如热塑性聚氨酯或聚酰胺,还有它们的混合物。
本发明使用的组合物可溶解在或分散到无机或有机,优选有机、液体稀释剂中,这里本发明的混合物优选应具有100~50,000mPas的粘度,然后按本身已知的方式施涂到基材上,例如采用喷涂、流延、浸涂、旋涂、辊涂、凸版印刷、凹版印刷或平版印刷或丝网印刷。进一步的加工可按通常的方式进行,例如除去稀释剂和将混合物固化。
合适的有机稀释剂是脂族醚,特别是四氢呋喃和二氧杂环己烷,烃类,特别是烃类混合物,如石油溶剂油(Benzin)、甲苯或二甲苯,脂族酯,特别是乙酸乙酯和乙酸丁酯,以及酮类,特别是丙酮、丁酮,以及环己烷,还有DMF和NMP。还可使用这类型稀释剂的组合。
可能使用的基材是通常用于电极的材料,优选金属,如铝和铜。还可能使用临时中间基材,如薄膜,特别是聚酯薄膜,如聚对苯二甲酸乙二醇酯薄膜。有利的是,此类型薄膜可带有剥离层,优选用聚硅氧烷制成。
隔膜也可用热塑性加工方式生产,例如通过注塑、熔体流延、压塑、捏合或挤塑,而且必要的话,本发明使用的组合物可在随后步骤中进行轧光。
由本发明使用的组合物成形为薄膜之后,可除去挥发性成分,如溶剂或增塑剂。
本发明使用的组合物可按本身已知的方式进行交联,例如通过以离子或电离射线进行辐照,采用电子束,优选配合20~2000kV的加速电压以及5~50Mrad的辐射剂量,采用紫外线或可见光,其中,有利的是按惯用方式加入引发剂如苯偶酰二甲基缩酮或1,3,5-三甲基苯甲酰三苯基氧化膦,其用量,具体地说,以聚合物粘结剂II/IIA为基准不大于1wt%,进行通常介于0.5~15min的交联;可采用按自由基聚合的热交联,优选在高于60℃的温度,此时有利的是加入引发剂,例如偶氮二异丁腈,用量一般不超过5wt%,优选0.05~1wt%,以聚合物粘结剂II/IIA为基准;可采用电化学诱导聚合;或者采用离子聚合,例如用酸催化的阳离子聚合,此时可能的催化剂主要是酸,优选路易斯酸,如BF3,或者特别是LiBF4或LiPF6。这里有利的是,可将含锂离子的催化剂如LiBF4或LiPF6仍保留在固体电极或隔膜中作为导电盐。
上面所描述的交联优选在惰性气氛下进行。这里的辐照时间,按照本发明可如此控制以使得完全交联,或者仅做短时间的紫外线预辐照,以便仅产生部分交联。
如文章开头所述,本发明模塑件的至少1个第2层包含传统隔膜。按照本发明,任何传统隔膜均可在这里使用。
下面将具体地介绍这方面的情况:
-基于微孔聚烯烃薄膜的隔膜,作为市售品,例如有商品名Celgard和Hipore以及描述在,特别是EP-A 0 718 901中以及EP-B 0 715 364中,在此将这2篇的全部内容收入本文作为参考;聚乙烯薄膜和聚丙烯薄膜,以及还有包含聚乙烯或聚丙烯与其他聚合物的共混物的薄膜,也同样可用于这里;
-由Goretex供应的微孔聚四氟乙烯(PTFE)薄膜,例如描述在EP-A 0 798 791中,也收入本文作为参考;
-纤网(Vliese)、纤维以及非织造纺织材料,即所谓的“Nonwovens”,全都可用纤维聚合物材料生产,聚合物材料例如聚烯烃、聚酰胺或聚酯纤维;
-以商品名Nafion供应的薄膜;
-基于偏二氟乙烯与六氟丙烯共聚物的薄膜,例如描述在美国专利5 540 741和美国专利5 478 668中;
-均聚物、嵌段共聚物和共聚物,它们包含填料并可由下列材料通过挤塑制备:
(a)烯烃,例如乙烯、丙烯、丁烯、异丁烯、丙烯、己烯或更高级同系物、丁二烯、环戊烯、环己烯、降冰片烯或乙烯基环己烷;
b)芳烃,例如苯乙烯和甲基苯乙烯;
c)丙烯酸酯或甲基丙烯酸酯,例如甲基、乙基、丙基、异丙基、丁基、异丁基、己基、辛基、癸基、十二烷基、2-乙基己基、环己基、苄基、三氟甲基、六氟丙基或四氟丙基的丙烯酸酯或甲基丙烯酸酯;
d)丙烯腈、甲基丙烯腈、N-甲基吡咯烷酮、N-乙烯基咪唑、醋酸乙烯;
e)乙烯基醚,例如甲基、乙基、丙基、异丙基、丁基、异丁基、己基、辛基、癸基、十二烷基、2-乙基己基、环己基、苄基、三氟甲基、六氟丙基、四氟丙基的乙烯基醚;
f)含卤素烯烃化合物,例如氯乙烯、氟乙烯、偏二氟乙烯、偏二氯乙烯、六氟丙烯、三氟丙烯、1,2-二氯乙烯、1,2-二氟乙烯或四氟乙烯,其中本发明的固体(I)用作这些聚合物中的填料;此类型挤塑薄膜所涉及的组合物和生产详细描述在DE-A 197 13 072.0中。
为了制备本发明的复合材料,令至少1个第1层与至少1个第2层互相接触,其中,按照本发明,所有已知方法均可用于将此类型的层合并在一起。因此,第1层可采用大气压压力下的方法施加到第2层上,例如采取第1层的原料的流延或刮涂,或者也可采取在超过大气压压力下的方法,例如挤塑、层合,特别是热层合,压延或压塑。这里所形成的复合材料可通过射线或电化学或通过加热实现交联或固化。另外,该至少1个第1层的原料也可首先完全地或部分地实施热交联或固化,然后按如上所述,在大气压压力或超过大气压压力下与本发明使用的第2层合在一起。如果是预制薄膜,即,将该至少1个第1层以薄膜形式,与传统隔膜,也是薄膜形式,合在一起的成膜情况,这将优选采用层合实施,温度一般在约50~约160℃,优选约70~约120℃,其中每种情况采取的确切温度都取决于每种情况下使用的传统隔膜。例如,倘若这里使用聚丙烯薄膜,则温度可能稍高于使用聚乙烯薄膜时的温度。如果复合材料采用层合来生产,则第1层的组合物也可处于部分或完全交联的形式,而层合后获得的复合材料,需要的话,可再次交联,或者不经“后交联”而直接使用。
如果本发明的复合材料用作化学电池中的隔膜,则该复合材料将与传统阳极和阴极合并在一起。另外,也可结合进含锂阳离子的可离解的化合物,所谓的导电盐,以及需要的话,其他添加剂,例如特别是有机溶剂,所谓的电解质。最后提到的物质的某些或全部可在本发明的复合材料的生产期间混入,或者在它已经生产出来以后引入。
可使用的导电盐一般是已知的,例如描述在EP-A 0 096 629中。按本发明,优选使用的导电盐是LiPF6、LiBF4、LiClO4、LiAsF6、LiCF3SO3、LiC(CF3SO2)3、LiN(CF3SO2)2、LiN(SO2CnF2n+1)2、LiC[(CnF2n+1)SO2]3、Li(CnF2n+1)SO2,其中n每种情况下为2~20,LiN(SO2F)2、LiAlCl4、LiSiF6、LiSbF6、(RSO2)nXLi(nX=1O,1S,2N,2P,3C,3Si;R=CmF2m+1,其中m=0~10或C1~C20烃类)、锂的亚氨化物盐、锂的甲基化物盐(Methidsalze),或者它们的2或更多种的混合物,其中尤其优选使用LiPF6作为导电盐。
可能的有机电解质溶剂是上面在“增塑剂”题目下所讨论的化合物,其中,优选使用的是传统有机电解质,优选酯类,例如碳酸亚乙酯、碳酸亚丙酯、碳酸二甲酯和碳酸二乙酯,或者此类型化合物的混合物。
有利的是,本发明的复合材料的厚度为5~500μm,优选10~500μm,更优选10~200μm,尤其是15~100μm。
该复合材料可与阳极和阴极组装在一起成为化学电池,后者本身也是一种固态复合制品。有利地是该复合制品可具有30~2000μm的总厚度,尤其是50~1000μm的总厚度。
本发明还提供一种生产此类型复合材料的方法,包括下列阶段:
(A)生产上面规定的至少1个第1层;
(B)生产上面规定的至少1个第2层;以及
(C)然后,将至少1个第1层与至少1个第2层按传统层合方法组合在一起。
该至少1个第1层优选在临时基材上生成。按照本发明,传统使用的临时基材可在这里使用,该基材例如是剥离膜,由聚合物或由优选涂布的纸制成,例如硅化处理的聚酯膜。然而,该第1层也可在永久基材上,例如集电极生成,或者甚至可以根本不用基材。
上面所规定的层合在一起及其制备,可全都利用提供层或制备层的大气压压力方法来实施,例如流延或刮涂,或者采用超过大气压压力的处理方法,例如挤塑、层合,特别是热层合、压延或压塑。所制成的复合材料,必要的话可利用射线、电化学手段或加热实现交联或固化。
也可利用上面描述的方法将本发明的复合材料与传统电极合在一起,从而制备一种由各组成部分(剥离膜/隔膜/电极)组成的复合制品。
还可采取对该复合材料的双面涂布,从而提供一种由阳极/隔膜/阴极组成的复合制品。
为此,作为隔膜的该复合材料,与阳极膜和/或阴极膜可在>80℃的温度下层合在一起。例如本发明的复合材料在这里可方便地层合到传统阳极或阴极上,从而获得复合制品阳极或阴极/隔膜,然后再将它与传统阴极或阳极合在一起成为包含阴极-隔膜-阳极的复合材料。
由上述阳极/隔膜/阴极组成的复合制品也可在不用基材或不用集电极电极的情况下制成,因为包含如上面规定的至少1个第1和至少1个第2层的本发明的复合材料,本身就具有足够用于化学电池中的机械稳定性。
向此类型复合制品或向化学电池中放入电解质和导电盐的步骤,可在各层合并在一起之前和优选在各层合并在一起之后,希望的话在与适当集电极,例如金属箔接触之后,甚至在该复合材料或者复合制品被引入到电池外壳以后实施。这里本发明的复合材料中各层的特殊微孔结构,特别是由上面规定的固体I的存在所决定的,能够吸入电解质和导电盐并赶出孔内的空气。取决于所用电解质,灌注可在0℃~约100℃的温度实施。
本发明的化学电池尤其可用作汽车电池、电器电池或平面电池以及用作机载电池(Bordbatterie)、静止场合的电池或电力牵引电池。
与迄今用于化学电池的隔膜相比,本发明的复合材料具有下列优点:
-传统隔膜与含固体I的组合物的组合所提供的复合材料具有不同寻常的机械稳定性,特别是优异尺寸稳定性和改善的耐压强度;
-本发明的复合材料可毫无困难地用于为该目的的市售卷绕设备上生产电池;
-本发明的复合材料是一种具有断路机制的隔膜。
现在,将利用某些实例来说明本发明。
实施例
制备实例1:隔膜的制备
75g以环氧硅烷进行疏水化处理、粒度为3μm的硅灰石(Tremin800 EST,Quarzwerke Frechen),利用高速搅拌器分散在300g甲苯中。然后,12.5g平均分子量Mw=2,000,000的聚环氧乙烷(Polyox,联合碳化物公司)、12.5g环氧丙烷-环氧乙烷嵌段共聚物的甲基丙烯酸二酯(PluriolPE 6000,BASF公司)以及0.02g紫外光引发剂(LucirinBDK,BASF公司)被加入到混合物中,然后混合物在60℃采用刮刀、流延间隙300μm,被施涂到硅化处理的聚对苯二甲酸乙二醇酯薄膜上,在5min内除去甲苯,揭下干燥的涂层后获得约30μm厚的薄膜。
制备实例2:PEO粘结层的制备
6g平均分子量Mw=2,000,000的聚环氧乙烷(Polyox,联合碳化物公司)溶解在300g甲苯中。该溶液在60℃刮涂到硅化处理的聚对苯二甲酸乙二醇酯薄膜上,以获得厚约3μm的PEO粘结层。
实例
为制备复合材料,上述2种薄膜利用Ibica,型号IL12HR的层合机在80℃彼此紧密结合在一起。随后,除去PEO粘结层一侧上的硅化处理的聚对苯二甲酸乙二醇酯薄膜。然后,将市售Celgard2300型隔膜(Hoechst Celanese)施加到PEO粘结层一侧。然后,这2种薄膜借助层合机在80℃紧密结合在一起。冷却后,可将第2硅化处理的聚对苯二甲酸乙二醇酯薄膜从复合隔膜上除去。
Claims (10)
1.一种复合材料,它包含至少1个第一层,该层包含含有下列成分的组合物,
(a)1~99wt%主粒度为5nm~100μm的固体(I),或由至少2种固体组成的混合物,
(b)99~1wt%聚合物粘结剂(II),可由下列物质聚合获得:
b1)以粘结剂(II)为基准5~100wt%下列成分的缩合产物III,
α)至少1种化合物IV,它能与羧酸或与磺酸或与衍生物或与它们中2或更多种的混合物起反应,以及
β)每摩尔化合物IV至少1摩尔具有至少1个能自由基聚合官能团的羧酸或磺酸V,或其衍生物,或它们中2或更多种的混合物,
以及
b2)以粘结剂(II)为基准0~95wt%另一种化合物VII,其平均分子量(数均)至少是5000,在其主链或侧链中具有聚醚链段,
其中该至少1个第1层已被施加到包含至少1个传统隔膜的至少1个第2层上。
2.权利要求1的复合材料,其中该至少1个第1层包含聚合物粘结剂(IIA),后者可由下列物质的聚合获得,
b1)以粘结剂(IIA)为基准5~75wt%不同于羧酸或磺酸V,也不同于其任何衍生物并能自由基聚合的化合物VI,或其2或更多种的混合物,
以及
b2)以粘结剂(IIA)为基准25~95wt%另一种化合物VII,其平均分子量(数均)至少是5000,在其主链或侧链中具有聚醚链段。
3.权利要求1或2的复合材料,其中该至少1个传统隔膜选自微孔聚烯烃薄膜和聚四氟乙烯薄膜。
4.权利要求1~3中任何一项的复合材料,其中固体I选自无机固体,该固体选自:元素周期表主族I、II、III或IV或过渡族IV元素的氧化物、混合氧化物、硅酸盐、硫酸盐、碳酸盐、磷酸盐、氮化物、氨化物、亚氨化物和碳化物;选自聚乙烯、聚丙烯、聚苯乙烯、聚四氟乙烯、聚偏二氟乙烯的聚合物;聚酰胺;聚酰亚胺;以及包含此类型聚合物的固态分散体;及其2或更多种的混合物。
5.权利要求1~4中任何一项的复合材料,其中该至少1个第1层包含至少1种其他聚合物VIII,该聚合物VIII选自氯乙烯、丙烯腈、偏二氟乙烯的聚合物或共聚物;氯乙烯与偏二氯乙烯、氯乙烯与丙烯腈、偏二氟乙烯和六氟丙烯、偏二氟乙烯与六氟丙烯的共聚物;由偏二氟乙烯与六氟丙烯以及选自氟乙烯、四氟乙烯和三氟乙烯之一构成的三元共聚物。
6.权利要求5的复合材料,其中聚合物VIII是由偏二氟乙烯与六氟丙烯构成的共聚物。
7.包含权利要求1~6中任何一项的至少1种复合材料的隔膜。
8.包含权利要求7的隔膜的化学电池。
9.一种生产权利要求1~6中任何一项的复合材料的方法,它包括下列阶段:
(A)生产权利要求1~6中任何一项的至少1个第1层;
(B)生产权利要求1~6中任何一项的至少1个第2层;以及
(C)然后,将至少1个第1层与至少1个第2层按传统层合方法组合在一起。
10.权利要求9的方法,其中,为将至少1个第1层与包含至少1个隔膜的至少1个第2层合在一起,该至少1个第1层通过刮涂被施加到该至少1个传统隔膜上,或者该至少1个第1层被层合,优选热层合到至少1个传统隔膜上。
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DE19916109.7 | 1999-04-09 | ||
DE19916109A DE19916109A1 (de) | 1999-04-09 | 1999-04-09 | Als Separatoren in elektrochemischen Zellen geeignete Verbundkörper |
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EP (1) | EP1183743A1 (zh) |
JP (1) | JP2002541644A (zh) |
KR (1) | KR20010112412A (zh) |
CN (1) | CN1355940A (zh) |
AU (1) | AU4398900A (zh) |
CA (1) | CA2369483A1 (zh) |
DE (1) | DE19916109A1 (zh) |
RU (1) | RU2001130341A (zh) |
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-
2000
- 2000-03-29 TW TW089105824A patent/TW488108B/zh not_active IP Right Cessation
- 2000-04-07 CN CN00808739A patent/CN1355940A/zh active Pending
- 2000-04-07 AU AU43989/00A patent/AU4398900A/en not_active Abandoned
- 2000-04-07 RU RU2001130341/09A patent/RU2001130341A/ru not_active Application Discontinuation
- 2000-04-07 WO PCT/EP2000/003134 patent/WO2000062355A1/de not_active Application Discontinuation
- 2000-04-07 US US09/958,288 patent/US6746803B1/en not_active Expired - Fee Related
- 2000-04-07 EP EP00925182A patent/EP1183743A1/de not_active Withdrawn
- 2000-04-07 JP JP2000611325A patent/JP2002541644A/ja not_active Withdrawn
- 2000-04-07 KR KR1020017012830A patent/KR20010112412A/ko not_active Application Discontinuation
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WO2000062355A1 (de) | 2000-10-19 |
CA2369483A1 (en) | 2000-10-19 |
AU4398900A (en) | 2000-11-14 |
RU2001130341A (ru) | 2003-07-20 |
TW488108B (en) | 2002-05-21 |
DE19916109A1 (de) | 2000-10-12 |
KR20010112412A (ko) | 2001-12-20 |
EP1183743A1 (de) | 2002-03-06 |
US6746803B1 (en) | 2004-06-08 |
JP2002541644A (ja) | 2002-12-03 |
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