CN1331843A - 用作电化学电池中分离器的复合体 - Google Patents
用作电化学电池中分离器的复合体 Download PDFInfo
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- CN1331843A CN1331843A CN99815021A CN99815021A CN1331843A CN 1331843 A CN1331843 A CN 1331843A CN 99815021 A CN99815021 A CN 99815021A CN 99815021 A CN99815021 A CN 99815021A CN 1331843 A CN1331843 A CN 1331843A
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Abstract
本发明涉及一种复合体,它包括含下列成分的至少一层:(a)从1至99重量%的固体(Ⅰ),其具有5毫微米至100微米主要粒径,或由至少两种固体所形成的混合物;(b)从99至1重量%的聚合物粘合剂(Ⅱ),其包含:从1至100重量%的聚合物(Ⅱa)或共聚物(Ⅱa),沿着链的末端和/或侧边具有反应性基(RG),其暴露于热和/或UV辐射下时可进行交联反应,以及从0至99重量%的至少一种聚合物或共聚物(Ⅱb),其不具有反应性基,其中至少一层被涂敷在至少一层第二种层上,其中该第二种层包含至少一个惯用分离器。
Description
本发明涉及特别适合作为电化学电池,较佳是可再充电式电池,特别是锂电池和锂离子电池的分离器的复合体,涉及这些分离器和各别电化学电池本身,以及涉及一种制造这些复合体的方法。
电化学电池,特别是这些可再充电式的电化学电池是为人所熟知的,例如从Ullmann’s工业化学百科全书,第5版,卷A3,VCHVerlagsgesellschaft mbH,Weinheim 1985,第343-397页。
由于锂电池和锂离子电池的高特定能量储存密度,其在这些电池中占有特殊的地位,特别是作为二次电池。
如上所述,特别是上面从“Ullmann”所摘录出来的,此类电池包含锰、钴、钒或镍的锂化合物氧化物。这些可以化学计量上最简单的例子如LiMn2O4、LiCoO2、LiV2O5或LiNiO2来描述。
这些化合物氧化物与可将锂离子掺入其晶格中的物质如石墨进行可逆反应,自该晶格中移去锂离子时,其中的金属离子如锰、钴或镍离子被氧化。在一个电化学电池中,以电解质的方式藉自含锂化合物氧化物即阴极物质中分离接受锂离子的化合物即阳极物质令此反应可用以储存电能,其中经由该电解质,形成锂离子的化合物氧化物可移动至阳极物质(充电)。
适合可逆储存锂离子的化合物通常以粘合剂将其固定在收集电极。
在电池充电期间,电子流过外加电压来源以及锂阳离子经由电解质流向阳极物质。当使用该电池时,锂阳离子流过电解质,反之,电子经由一负载从阳极物质流向阴极物质。
为了避免电化学电池内短路,一电绝缘但锂阳离子可穿过层位于两电极间。此即所谓的固体电解质或惯用分离器。
如为人所熟知的固体电解质和分离器是由一种载体物质所组成的,掺入其中的是一种包含锂阳离子并用于增加锂离子导电度的可解离化合物,通常及其他添加剂如溶剂。
微孔薄膜一时被提出作为分离器。例如,GB 2 027 637描述一种微孔薄膜,其包含一种具有从40至90体积%的聚烯烃和从10至60体积%的无机填料的基材以及在此各别定义的其他组成物。在此所描述的基材具有30至95体积%的孔洞,以薄膜体积为基准,并且其是一种铅蓄电池的分离器。
EP-B 0 715 364描述一种具有断电特性的两层电池分离器。其所描述的电池分离器具有一层第一种微孔隔膜,其具有断电功能且是由一种选自聚乙烯、实质上含聚乙烯的掺合物及聚乙烯共聚物的物质所制成的。该分离器也具有一层第二种微孔隔膜,其具有强化功能且是由一种选自聚丙烯、实质上包含聚丙烯的掺合物及聚丙烯共聚物的物质所制成的。根据此描述,此分离器比先前技术更具较佳的机械强度和转变能量。
EP-A 0 718 901描述一种具断电特征的三层电池分离器。此分离器包含一种第一层和第三层微孔聚丙烯隔膜,其依次包括一种微孔聚乙烯隔膜,其中第一种和第三种隔膜具有较大的刺孔阻力和比第二种隔膜高的熔点。
EP-A-0 708 791描述一种隔膜形式的复合聚合物电解质,其具有一层涂覆于基材物质上的离子传导聚合物凝胶,其中基材物质是由多孔性聚四氟乙烯隔膜所制成的。
考虑此先前技术,本发明的目的是提供一种分离器,其同样地具有断电机制而且在高温下(>150℃)具有尺寸稳定性,以及进一步改善机械强度并且具有极佳的离子传导性质。
我们已发现此目的可以一种复合体来完成,其是包含至少一层第一种层,该层包含下列组成:
(a)从1至99重量%的固体(I)或由至少两种固体所形成的混合物,其中该固体的主要粒径是从5毫微米至100微米;
(b)从99至1重量%的聚合物粘合剂(II),其包含:
(IIa)从1至100重量%的聚合物或共聚物(IIa),沿着链的末端和/或侧边,其具有暴露于热和/或UV辐射时可进行交联反应的反应性基(RG),以及
(IIb)从0至99重量%的至少一种不具有反应性基RG的聚合物或共聚物(IIb),其中至少一层第一层被涂敷在至少一层第二种层上,其中第二种层包含至少一个惯用分离器。
该组合物存在于至少一层第一种层中,现在将其制法详细描述于下。
固体I最好选自一种无机固体,较佳是一种碱性无机固体,其是选自氧化物、混合氧化物、碳酸盐、硅酸盐、硫酸盐、磷酸盐、酰胺、酰亚胺,周期表中第一、第二、第三或第四主族元素、第四族过渡金属元素的氮化物和碳化物;一种选自聚乙烯、聚丙烯、聚苯乙烯、聚四氟乙烯和聚偏氟乙烯的聚合物;聚酰胺、聚酰亚胺;一种包含此类聚合物的固体分散液;玻璃粉末、毫微玻璃颗粒如Monosper(莫克)、微玻璃颗粒如Spheriglas(Potters-Ballotini)、毫微须晶及两种或多种这些颗粒的混合物,其所获得的组合物可用于作为一种固体电解质和/或分离器。
以实例方式必须特别提及:氧化物,如二氧化硅、氧化铝、氧化镁或二氧化钛、例如元素硅、钙、铝、镁、钛的化合物氧化物;硅酸盐如梯形硅酸盐、ino-、phyllo-和tectosilicate如滑石、叶蜡石、muskovite、金云母、闪石、nesosilicates、辉石、sorosilicates、沸石、长石、硅灰石,特别是疏水化硅灰石,云母、phyllosilicates;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、镁或钡碳酸盐或锂、钾或钠碳酸盐;磷酸盐如磷灰石;酰胺;酰亚胺;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、聚偏氟乙烯、聚酰胺、聚酰亚胺或其他热塑性材料、热固性材料或微凝胶、交联聚合粒子,如Agfaperl、固体分散液,特别是包含上述聚合物的那些物质,以及两种或多种上述固体的混合物。
根据本发明所用的固体I也可包含无机Li-离子传导固体,较佳是一种碱性无机Li-离子传导固体。
这些应提及的是:硼酸锂如Li4B6O11*xH2O、Li3(BO2)3、Li2B4O7*xH2O、LiBO2、其中数字x可从0至20;铝酸锂如Li2O*Al2O3*H2O、Li2Al2O4、LiAlO2;铝硅酸锂如含锂的沸石、长石、长石取代物、phyllo-和inosilicate,特别是LiAlSi2O6(锂辉石)、LiAlSi4O10(petullite)、LiAlSiO4(eucryptite)、云母类如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、板或立方形的,特别是通式为Li2/zO*Al2O3*xSiO2*yH2O的,其中z是价数,x是从1.8至约12和y是从0至约8;碳化锂如Li2C2、Li4C;Li3N;锂氧化物和化合物锂氧化物如LiAlO2、Li2MnO3、Li2O、Li2O2、Li2MnO4、Li2TiO3;Li2NH;LiNH2;锂磷酸盐如Li3PO4、LiPO3、LiAlFPO4、LiAl(OH)PO4、LiFePO4、LiMnPO4;Li2CO3;锂硅酸盐、梯形硅酸盐形式的锂硅酸盐、ino-、phyllo-和tectasilicates如Li2SiO3、Li2SiO4和Li6Si2;锂硫酸盐如Li2SO4、LiHSO4、LiKSO4;以及如化合物Ib所提的Li化合物,其中当这些被用于作为固体I时,排除传导性黑体的存在;以及两种或多种上述Li-离子传导固体的混合物。
较佳的固体I是疏水化固体I,更佳是上述类型的疏水化化合物。
在此碱性固体是特别适合的。为了本发明目的,碱性固体是这些含有液体、含水稀释剂的混合物的pH高于此稀释剂的化合物,其中稀释剂本身的pH不超过7。
此固体最好是实质上非常不溶于用作电解质的液体中而且在电池环境中是电化学惰性的。
适合的固体I是这些主要粒径是从5毫微米至20微米,较佳是从0.01至10微米和特别是从0.1至5微米的固体,所获得的粒径是以电子显微术测得的。颜料的熔点最好是高于电化学电池的一般操作温度,特佳是熔点高于120℃,特别是高于150℃的熔点。
在此颜料在其外形可能对称,即高对宽对长(纵横比)的尺寸比为约1而且呈球或丸状外形,外形可能近圆形或者任何所需多面体形状如立方形、四面体、六面体、八面体或双角锥体或可能是扭曲或不对称即高对宽对长(纵横比)的尺寸比不等于1以及呈,例如针状、不对称四面体、不对称双角锥体、不对称六或八面体、薄片或板或者纤维状外形。若该固体是不对称粒子,上面所提供主要粒径的上限是是指各例中最小的轴。
根据本发明所用的组合物包含从1至95重量%,特佳是从15至90重量%,更佳是从25至85重量%,特别是从50至80重量%的固体I和从5至99重量%,特佳是从10至85重量%,更佳是从15至75重量%,特别是从20至50重量%的聚合物粘合剂II。
此聚合物粘合剂II包含从1至100重量%的至少一种聚合物或共聚物IIa,沿着链的末端和/或侧边,其具有暴露于热和/或UV辐射下时可进行交联反应的反应性基(RG),以及从0至99重量%的至少一种不具反应性基RG的聚合物或共聚物(IIb)。
基本上可用的聚合物IIa可为任何暴露于热和/或高能量辐射,较佳是UV光下可交联的聚合物,并且沿着链的末端和/或侧边,其具有反应性基(RG),较佳是反应性基RGa或RGb或者RGa和RGb,由此该聚合物当被热和/或辐射活化时可进行交联。
较佳是聚合物IIa是一种聚合物,其沿着链的末端和/或侧边具有至少一个异于RGa且与RGa共反应的基团RGb,其中所有聚合物分子平均具有至少一个RGa和至少一个基团RGb。
再者,从两种或多种聚合物的混合物可形成该聚合物IIa,其中一部分聚合物只有RGa和另一部分聚合物只有RGb。
而且,聚合物IIa可从两种或多种部分只有RGa和另一部分只有RGb的聚合物与其他具有RGa和RGb两者的混合物所形成。
聚合物IIa一般是由一连贯聚合物种类,较佳是从聚丙烯酸酯类所形成的。但是,各种聚合物种类的掺合物也有可能。
聚合物IIa可能包含聚合物或寡聚物物质,或者聚合物和寡聚物物质的混合物。
聚合物IIa的寡聚物和/或聚合物基本结构可包含已知聚合物例如,经-C-C-连结所构成的聚合物,其也可具有双和/或三键,或者也可经醚、酯、氨基甲酸乙酯、酰胺、酰亚胺、咪唑、酮、硫化物、砜、缩醛、脲、碳酸酯或硅氧烷连结。
寡聚物或聚合物基本结构也可为线性、分支链、环状或dendrimer型。
根据本发明所用的聚合物IIa可藉单体建造嵌合物的聚合、加聚或聚缩合获得,除了藉使建造聚合物的基团外,单体建造嵌合物也具有RGa和/或RGb,因此在聚合物的制备过程中,直接形成根据本发明的官能化聚合物IIa。
再者,根据本发明的聚合物IIa可藉官能聚合物与化合物的聚合物类似反应获得。其中该化合物具有RGa和/或RGb和至少一个可与寡聚物或聚合物基本结构的官能基反应的其他基团。
在聚合物的制备过程中,也有可能直接掺入官能基RGa和/或RGb之一,然后藉聚合物类似官能化将其他RG导入制成聚合物中。
基团RGa是具有暴露于高能量辐射,较佳是UV辐射时在三重激发态可抽出氢的结构的基团(文献上已知的Norrish II型光引发剂基团)。熟谙此技工作者可从光化学得知此类结构。该文献也列出具此类结构的适合的丙烯酸酯(衍生物)化合物。其他关于这些化合物的细节可在US 5 558 911中发现,在此关连中其整个公开范围被并入此申请中。当然,根据本发明也可能使用其他具此类RGa结构的单体、寡聚物或聚合物。
其中
R6是—CH3或—C6H5
伴随使用此类RGa丙烯酸酯使其容易地可,例如藉与其他丙烯酸酯的共聚合以获得依根据本发明方式以RGa官能化的丙烯酸酯共聚物。
具有,例如氨基但不含RGa基的碱聚合物也可容易地藉此类RGa丙烯酸酯的Michael加成以RGa官能化的。
偏好以二苯甲酮基作为RGa。在聚丙烯酸酯例子中,特高的UV反应性可以二苯甲酮衍生物达到,其中二苯甲酮基经由一个间隔基被键结在主聚合物链上。特佳的聚丙烯酸酯与藉与式24至26和34的丙烯酸酯共聚合而获得。
其他将RGa导入聚合物的省钱和较佳的方法是羟基二苯甲酮类,较佳是4-羟基二苯甲酮与聚合物的环氧基反应,较佳是4-羟基二苯甲酮加成到具有(甲基)丙烯酸缩水甘油酯内容物的聚丙烯酯中。其他较佳的方法是由一摩尔二异氰酸酯和一摩尔4-羟基二苯甲酮所制成的加成物与具有游离羟基的聚合物反应。
一种将RGa导入聚酯的较佳方法是分别在具有羟基、环氧基、异氰酸酯基和/或氨基的聚合物分别与二苯甲酮羧酸或二苯甲酮羧酸酐的聚缩合或反应或酯化过程中伴随使用二苯甲酮羧酸或二苯甲酮羧酸酐。
基团RGb是可与激发态Norrish II光引发剂基团相互作用的基团。熟谙此技的工作者所熟知的此类特定相互作用是氢转移至Norrish II结构上,造成自由基形成于H的提供者和在抽出的Norrish II结构上。经由自由基合并直接交联聚合物是可能的。光化学上所产生的自由基也可能引发一种例如可聚合官能基RGb如顺式丁烯二酸酯、反式丁烯二酸酯、(甲基)丙烯酸酯、烯丙基、环氧基、烯基、环烯基、乙烯基醚、乙烯基酯、乙烯基芳基或肉桂酸酯基的自由基所引发的聚合。
较佳RGb作为H提供者与RGa系统作用,即是不含双键。此系统固有的优点是与不饱和UV系统相比,其对干扰的灵敏度较低,因为其对所有混合的其他组成物具有较低的反应性。当然,这不是排除不饱和物质的(伴随)使用,而且在各个例子中,这是一个使其完善的工作。H-提供者基为光化学上熟谙此技的工作者所熟知的。基本上它们是具有低键能的氢的基团,特别是具有键能低于397千焦耳/摩尔的氢原子的基团。
键能的数据可从文献上得知并且可在,例如Morrison RobertThornton,有机化学,表:套管内部的Homolytic键解离能,于美国国会图书馆,刊物类别数据ISBNO-205-08453-2,1987,Allyn和Bacon公司,Simon&Schuster部门发行,Newton,麻州,美国可找到。
R3=一种二价脂族、环脂族、杂环或芳族基,未经取代或经取代,或一个单键;
R4=H,直链或支链的烷基,例如具有从1至8个碳原子,经卤基取代的芳基或异戊基苯基;
R5=烷基、经卤基取代的烷基、经卤基取代的芳基或异戊基苯基。这些化学式是非限定性实例。
较佳是这些容易抽出H原子的基团是H原子在双键的α位置上(烯丙基H原子)。
特佳的RGb基是
(寡聚)二氢二环戊二烯醇的顺式丁烯二酸酯/反式丁烯二酸酯半酯类在工业上可容易地自顺式丁烯二酸和DCPD获得。
这些半酯可分别在一个顺利的反应中从顺式丁烯二酸酐(MA)、水和二环戊二烯(DCPD)获得或藉DCPD直接加成至MA而获得。其也可能进行DCPD直接加成至其他酸类和/或酸聚酯类。但是,这些反应大部分进行的满意度较低而且需要催化如以三氟化硼合乙醚催化。
也有兴趣的是利用羟基烷基胺经由这些酸的酰亚胺导入内型亚甲基四氢苯二甲酸结构和四氢苯二甲酸结构,如,例如DE-A-15700273或DE-A-17200323中所揭示的。
聚合物IIa的寡聚物和/或聚合物基本结构可包含已知聚合物,例如经-C-C连接,其可能也有双键和/或三键,或者经由醚、酯、氨基甲酸乙酯、酰胺、酰亚胺、咪唑、酮、硫化物、砜、缩醛、脲、碳酸酯或硅氧烷连接所构成的聚合物进行更接近上面所定义的官能化作用。
较佳是聚酯、聚醚、聚氨酯和特佳是聚丙烯酸酯。
对于本发明目的,聚酯是饱和和不饱和聚酯树脂。
在此聚酯树脂可利用具有≥2个羧基的普通且已知的羧酸和/或其酸酐和/或其酯类及具≥2个OH基的羟基化合物所构成。也可能伴随使用单官能基化合物,例如以调整聚缩合物的分子量。
可能的羧酸成份的实例是α,β-乙烯系羧酸如顺式丁烯二酸、顺式丁烯二酸酐、反式丁烯二酸、衣康酸和柠康酸,饱和脂族羧酸或其分别的酸酐,如丁二酸、己二酸、辛二酸、癸二酸和壬二酸,天然存在的脂肪酸和聚合天然存在的脂肪酸如亚麻子油脂肪酸、二聚和聚合亚麻子油脂肪酸、蓖麻油和蓖麻油脂肪酸、饱和环脂族羧酸或其分别的酸酐,如四氢苯二甲酸、六氢苯二甲酸、内型亚甲基四氢苯二甲酸和降冰片烯二羧酸、芳族羧酸或这些各别的酸酐,如异构物形式的苯二甲酸以及三-和四羧酸或这些各别的酸酐,如苯偏三酸和苯均四酸以及部分以烯丙基醇酯化的聚羧酸如苯偏三酸单烯丙基酯或苯均四酸二烯丙基酯,特别重要性是放在二苯甲酮羧酸,因为这些共聚物允许可被UV光激发的结构掺入。
可能的羟基成分的实例是至少二羟的,若所需烷氧化、脂族和/或环脂族醇如乙二醇、丙二醇、聚乙二醇、聚丙二醇、丁烷二醇异构物、丁烷二醇、三羟甲基丙烷、季戊四醇、新戊二醇、环己烷二甲醇、双酚A和氢化双酚A、OH多官能基聚合物如经羟基改质的聚丁二烯类或具有羟基的聚氨基甲酸乙酯预聚物、甘油、饱和或不饱和脂肪酸的单-和二甘油酯,特别是亚麻子油或葵花油的单甘油酯。其他可能的化合物是不饱和醇如经以烯丙基醇(部分)醚化的多官能基羟基化合物,如三羟甲基乙烷单烯丙基醚、三羟甲基乙烷二烯丙基醚、三羟甲基丙烷单烯丙基醚、三羟甲基丙烷二烯丙基醚、季戊四醇单烯丙基醚、季戊四醇二烯丙基醚、2-丁烯-1,4-二醇和烷氧基化2-丁烯-1,4-二醇。
若单官能基物质备用于调整分子量,这些最好是单官能基醇如乙醇、丙醇、丁醇、己醇、癸醇、异癸醇、环己醇、苯甲醇或烯丙基醇。对于本发明目的,聚酯一词也包含聚缩合物,其除了酯基之外还具有酰胺基和/或酰亚胺基而且可藉伴随使用氨基化合物获得。以此方式改质的聚酯可从,例如DE-A-15700273和DE-A-17200323已知。如那里所提,内型亚甲基-四氢苯二甲酸结构和四氢苯二甲酸结构经由这些酸与羟基烷基胺的酰亚胺导入暗示这些是本发明目的的基团RGb。
也可能进行DCPD加成至所用不饱和聚酯的双键上,让内型亚甲基四氢苯二甲酸结构掺入,对于本发明目的该结构是RGb。这些内型亚甲基四氢苯二甲酸结构可能位于沿着链和/或在双键末端的聚酯的双键上,例如那些经由式3物质导入的。对于本发明目的,不饱和二羧酸和/或不饱和二醇的双键是沿着链的RGb。RG可藉其缩合和/或藉聚合物类似反应被导入具官能基的聚酯上。共缩合的实例是附随使用三羟甲基丙烷二-和单烯丙基醚、季戊四醇二-和单烯丙基醚、2-丁烯-1,4-二醇、烷氧化2-丁烯-1,4-二醇、烯丙基醇和式3、4、5、7和8的化合物。
一种导入RGa的较佳方法是二苯甲酮羧酸或其酸酐共缩合。另外较佳的方法是羟基-二苯甲酮类与过量二异氰酸酯的反应产物加成至羟基-官能基聚酯。
RGb也可以此方式导入羟基-官能基聚酯。对于此,具有不同反应性的异氰酸酯基的二异氰酸酯,如异佛尔酮二异氰酸酯或甲代亚苯基1,4-二异氰酸酯最好先与一半化学计算量之,例如羟基丙烯酸酯、羟基乙烯基醚、羟基烯丙基酯、羟基烯丙基醚或式AGb4和AGb6的羟基-DCPD化合物反应,然后这些反应产物与羟基官能基聚酯反应。不同种类的羟基-官能基物质也可能同时被用于上述反应中。
经根据本发明的RG官能化的聚(甲基)丙烯酸酯树脂是另一类重要根据本发明聚合物并且可藉丙烯酸酯,若有需要与其他可共聚合的化合物共聚合而获得。
但是,根据本发明的聚合(甲基)丙烯酸酯树脂也可在溶剂中制得。其他较佳的聚合(甲基)丙烯酸酯制备方法是在一个搅拌反应器中,若需要在超计大气压下,或在连续反应器中高于所形成聚合物的熔点的温度下,进行无溶剂自由基本体聚合。
适合建造聚合(甲基)丙烯酸酯树脂的成分实例是已知的丙烯酸酯类和甲基丙烯酸酯类与具有从1至40个碳原子的脂族、环脂族、芳脂族或芳族醇类,如(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸异丙基酯、(甲基)丙烯酸正丁基酯、(甲基)丙烯酸异丁基酯、(甲基)丙烯酸叔丁基酯、(甲基)丙烯酸戊基酯、(甲基)丙烯酸异戊基酯、(甲基)丙烯酸己基酯、(甲基)丙烯酸2-乙基己基酯、(甲基)丙烯酸癸酯、(甲基)丙烯酸十一烷基酯、(甲基)丙烯酸十二烷基酯、(甲基)丙烯酸十三烷基酯、(甲基)丙烯酸环己基酯、(甲基)丙烯酸甲基环己基酯、(甲基)丙烯酸苯甲基酯、(甲基)丙烯酸四氢糠基酯和(甲基)丙烯酸糠基酯,以及3-苯基丙烯酸的酯类和其各种异构物,例如肉桂酸甲酯、肉桂酸乙酯、肉桂酸丁酯、肉桂酸苯甲基酯、肉桂酸环己基酯、肉桂酸异戊基酯、肉桂酸四氢糠基酯和肉桂酸糠基酯、丙烯酰胺、甲基丙烯酰胺、羟甲基丙烯酰胺、羟甲基甲基丙烯酰胺、丙烯酸、甲基丙烯酸、3-苯基丙烯酸、(甲基)丙烯酸(羟基烷基)酯,如乙二醇单(甲基)丙烯酸酯、丁二醇单(甲基)丙烯酸和己烷二醇单(甲基)丙烯酸酯、二元醇醚(甲基)丙烯酸酯,如甲氧基乙二醇单(甲基)丙烯酸酯、乙氧基乙二醇单(甲基)丙烯酸酯、丁氧基乙二醇单(甲基)丙烯酸酯和苯氧基乙二醇单(甲基)丙烯酸酯、丙烯酸缩水甘油酯、甲基丙烯酸缩水甘油酯以及氨基(甲基)丙烯酸酯,如2-氨基乙基(甲基)丙烯酸酯。
其他可能的成分是可进行自由基共聚合的单体,例如苯乙烯、1-甲基苯乙烯、4-叔丁基苯乙烯、2-氯苯乙烯、具有2至20个碳原子的脂肪酸的乙烯基酯类,例如醋酸乙烯酯和丙酸乙烯基酯,具有2至20个碳原子的醇类的乙烯基醚类,如乙烯基异丁基醚、氯化乙烯、氯化亚乙烯、乙烯基烷基酮,二烯类如丁二烯和异戊二烯,以及顺式丁烯二酸和巴豆酸的酯类。其他适合的单体是环乙烯基化合物,如乙烯基吡啶、2-甲基-1-乙烯基咪唑、1-乙烯基咪唑、5-乙烯基吡咯烷酮和N-乙烯基吡咯烷酮。也可能使用烯丙基系不饱单体,如烯丙基醇、烯丙基烷基酯、苯二甲酸单烯丙基酯和苯二甲酸烯丙基酯。也可使用丙烯醛和甲基丙烯醛以及可聚合的异氰酸酯。
RG可藉制备聚丙烯酸酯期间共聚合或藉接下来的聚合物类似反应将其掺入。聚合良好且具有基团RGb的化合物实例是二氢二环戊二烯基(甲基)丙烯酸酯、二氢二环戊二烯基乙基丙烯酸酯和二氢二环戊二烯基肉桂酸酯。聚合良好且具有可能进行聚合物类似官能化的其他基团的化合物实例是可共聚合的环氧基化合物如(甲基)丙烯酸缩水甘油酯或(甲基)丙烯酸(羟基烷基)酯。依此方式掺入的羟基和/或环氧基是聚合物的聚合物类似官能化反应的固定基。环氧基是,例如适合藉与(甲基)丙烯酸(RGb)反应导入丙烯酸双键和/或藉与氨基乙烯基醚化合物,如二乙醇胺二乙烯基醚反应导入乙烯基醚基团(RGb),或者藉与羟基-和/或氨基二苯甲酮类反应导入二苯甲酮基(RGa)。
根据本发明以RG官能化的聚氨酯是另一类根据本发明重要的聚合物而且其可以熟谙此技工作者已知的方式从多官能基,主要是双官能基异氰酸酯及聚羟基和/或聚氨基化合物获得。在此也可能包括在构成聚氨酯的过程中直接掺入RGa和/或RGb,或者接着将其导入官能基聚氨酯中。对于此的化学反应伙伴基本上是与上述聚合物的相同。RGa最好是经由官能基二苯甲酮化合物的伴随使用将其导入,以及RGb是经由式RGb4和RGb6的羟基-DCPD化合物将其导入。
可使用的碱性聚氨基甲酸乙酯结构的其他相关细节可在可用作为聚合物IIb的聚氨酯的相关讨论中找到。
根据本发明聚合物IIa是依照公知原理所制得,而且其制备方面,如以伴随使用控制或单官能基起始物设定所需分子量,或者借平衡硬性和软性成份以设定所需玻璃化转变温度等为熟谙此技工作者所熟知的。
如上所述,特别适合导入RGa于根据本发明所用的聚合物IIa中,特别是于环氧基-和/或羟基-官能化聚酯、聚氨酯或聚丙烯酸酯之化合物是:
2-、3-和4-羟基二苯甲酮、2-羟基-5-甲基羟基二苯甲酮、2-羟基-4-甲氧基二苯甲酮、2-羟基-4-辛氧基二苯甲酮、2-羟基-4-十二烷氧基二苯甲酮、2-羟基-5-氯羟基二苯甲酮、2-羟基-4-甲氧基-4’-甲基二苯甲酮、2-羟基-5-甲氧基-4’--氯二苯甲酮、4-羟基-3-甲基二苯甲酮、4-羟基-4’-甲氧基二苯甲酮、4-羟基-4’-氯二苯甲酮、4-羟基-4’-氟二苯甲酮、4-羟基-4’-氰基二苯甲酮、4-羟基-2’,4’-二甲氧基二苯甲酮、2,2’、4,4’-和2,4-二羟基二苯甲酮、4-叔丁基-2,4-二羟基二苯甲酮、2,2’-二羟基-4-甲氧基二苯甲酮、2,2’-二羟基-4-辛氧基二苯甲酮、2,2’-二羟基-4,4’-二甲氧基二苯甲酮、2,4,4’-、2,3,4-和2,4,6-三羟基二苯甲酮、2,2’-、4,4’-、2,3,4,4’-和2,3’,4,4’-四羟基二苯甲酮、2-、3-和4-氨基二苯甲酮、2-氨基-4-甲基二苯甲酮、2-氨基-6-甲基二苯甲酮、2-氨基-4’-甲基二苯甲酮、2-氨基-4’-氯-5-氟二苯甲酮、2-氨基-5-氯二苯甲酮、2-氨基-5-溴二苯甲酮、2-氨基-5-甲基二苯甲酮、2-氨基-N-乙基二苯甲酮、2-氨基-2’,5’-二甲基二苯甲酮、4-氨基-2-氨二苯甲酮、4-氨基-4’-甲氧基二苯甲酮、3,4-、4,4’-和3,3’-二氨基二苯甲酮、4,4’-双(甲基胺基)二苯甲酮、3,3’,4,4’-四氨基二苯甲酮、2-、3-和4-苯甲酰基苯甲酸、2-苯甲酰基-3’-甲基苯甲酸、2-苯甲酰基-4’-乙基苯甲酸、2-苯甲酰基-3,6-二甲基苯甲酸、2-苯甲酰基-2’,6’-二甲基苯甲酸、2-苯甲酰基-3’,4’-二甲基苯甲酸、2-苯甲酰基-2’,4’,6’-三甲基苯甲酸、2-苯甲酰基-对-羟基苯甲酸、2-苯甲酰基-4’-甲基-3’-氯苯甲酸、2-苯甲酰基-6-氯苯甲酸、4-苯甲酰基-4’-异丙基苯甲酸、4-苯甲酰基-4’-氯苯甲酸、4-苯甲酰基-4’-(2-羧基丙基)-苯甲酸、2,4-、3,4-和4,4’-二苯甲酮-二羧酸、2’,3,4-、3,3’,4-和3,4,4’-二苯甲酮三羧酸、3,3’,4,4’-二苯甲酮四羧酸和-四羧酸二酐、2-羟基-4-甲氧基-5-磺基二苯甲酮、4-(4-羧基苯氧基)二苯甲酮、4-(3,4-双(羧基)苯氧基)二苯甲酮及其对应酸酐、4-(4-羧基苯氧基)二苯甲酮-4-羧酸、4’-(4-羧基苯氧基)二苯甲酮-3,4-二羧酸及其对应酸酐、4’-(3,4-双(羧基)苯氧基)二苯甲酮-2,4-和-3,4-二羧酸及其对应酸酐、4-(4-氰基苯甲酰基)苯硫酚、4(2-羟基-乙氧基)苯基(2-羟基-2-丙基)酮、4-(2-氨基乙氧基)苯基(2-羟基-2-丙基)酮、4-(2-羟基羰基甲氧基)苯基(2-羟基-2-丙基)酮、4-(2-异氰氧基乙氧基)苯基(2-羟基-2-丙基)酮、4-(2-异氰氧基甲氧基)苯基(2-羟基-2-丙基)酮、2-([2-]6-异氰氧基己基氨基羰氧基)乙氧基硫杂噻吨酮和苯基二羟醋酸。
所用的聚合物IIa也可为聚合物和下面“聚合物IIb”中所讨论的共聚物,只要这些可提供反应性基RG,特别是RGa和/或RGb。在此特别提及可提供反应性基RG之含卤素烯烃化合物(4f类)的聚合物和共聚物。
最好以高能量辐射,特别是以UV光使根据本发明所用的聚合物IIa交联。在大部分的例子中,在此不需加入其他光引发剂,即该物质被其本身光交联,而且一个特殊的优点是其的低空气抑制程度。但是,不排除添加其他商业可取得的光引发剂。许多聚合物IIa也可以热力交联之。也具有DCPD基之不饱和系统在过氧化物和/或苯频哪醇类之C-C活泼物质的存在下具有特别高的热交联性。部份此类系统也可以热力固化,不需要过氧化物。借热和UV光之合并使用如借合并IR和UV光源可达到较佳的快速交联。
所用的聚合物IIb可以包含热塑性和离子传导聚合物。这些被特别提及的是:
1)聚碳酸酯,如聚亚乙基碳酸酯、聚亚丙基碳酸酯、聚丁二烯碳酸酯和聚亚乙烯基碳酸酯。
2)由下列化合物所制成的均聚物、嵌段聚合物和共聚物:
a)烯烃类,如乙烯、丙烯、丁烯、异丁烯、丙烯、己烯或较高碳数同系物、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)芳族烃类,如苯乙烯和甲基苯乙烯;
c)丙烯酸酯类或甲基丙烯酸酯类,如分别为甲基、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、苯甲基、三氟甲基、六氟丙基和四氟丙基之丙烯酸酯以及甲基丙烯酸酯;
d)丙烯腈、甲基丙烯腈、N-甲基吡咯烷酮、N-乙烯基咪唑和乙酸乙烯酯;
e)乙烯基醚类,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、苯甲基、三氟甲基、六氟丙基和四氟丙基乙烯基醚类;
f)含卤素烯烃化合物如氟化亚乙烯、氯化亚乙烯、氟化乙烯、氯化乙烯、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之聚合物和共聚物;较佳是氯化乙烯、丙烯腈或氟化亚乙烯的聚合物或共聚物;由氯化乙烯与氯化亚乙烯、氯化乙烯与丙烯腈、氟化亚乙烯与六氟丙烯以及氟化亚乙烯与六氟丙烯所制成的共聚物;由氟化亚乙烯和六氟丙烯以及选自氟化乙烯、四氟乙烯和三氟乙烯之一员所制成的三聚物;特别是一种由氟化亚乙烯和六氟丙烯所制成的共聚物以及其他包含从75至92重量%氟化亚乙烯和从8至25重量%六氟丙烯之较佳共聚物;
g)2-乙烯吡啶、4-乙烯基吡啶和亚乙烯基碳酸酯。
在上述聚合物的制造过程中可使用调节剂如硫醇类,若这是必须和/或所需的。
3)例如借下列化合物反应可获得的聚氨酯:
a)具有从6至30个碳原子之有机二异氰酸酯,如脂族非环状二异氰酸酯,如六亚甲基1,5-二异氰酸酯和六亚甲基1,6-二异氰酸酯,脂族环状二异氰酸酯,如环己烯1,4-二异氰酸酯、二环己基甲烷二异氰酸酯以及异佛尔酮二异氰酸酯,或芳族二异氰酸酯,如甲代亚苯基2,4-二异氰酸酯、甲代亚苯基2,6-二异氰酸酯、四甲基二甲苯间-二异氰酸酯、四甲基二甲苯对-二异氰酸酯、四氢萘1,5-二异氰酸酯和二亚苯基-甲烷4,4’-二异氰酸酯或此类化合物的混合物。
与
b)多羟基醇类,如聚酯醇、聚醚醇和二醇类。
该聚酯醇最好主要为具有末端OH基之线性聚合物,较佳是这些具有两个或三个,特别是两个末端OH基的聚合物。该聚酯醇的酸值是低于10较佳是低于3。聚酯醇可以以简单的方式制备,通过用二元醇,优选具有从2至25个碳原子之二元醇酯化具有从4至15个碳原子,较佳是从4至6个碳原子之脂族或芳族二羧酸,或者借聚合具有从3至20个碳原子之内酯而制得。可使用的二羧酸实例是谷氨酸、庚二酸、辛二酸、癸二酸、十二烷基酸及较佳是己二酸和琥珀酸。适合的芳族二羧酸是对苯二甲酸、间苯二甲酸、苯二甲酸或这些二羧酸与其他二羧酸如联苯甲酸、癸二酸、琥珀酸和己二酸的混合物。该二羧酸可单独使用或使用混合物形式之二羧酸。为了制备聚酯醇,其最好偶尔使用对应酸衍生物如羧酸酐或氯化羧酸以取代二羧酸。适合的二元醇类实例是二甘醇、1,5-戊烷二醇、1,10-癸烷二醇和2,2,4-三甲基-1,4-戊烷二醇。较佳是使用1,2-乙烷二醇、1,3-丙烷二醇、2-甲基-1,3-丙烷二醇、1,4-丁烷二醇、1,6-己烷二醇、2,2-二甲基-1,3-丙烷二醇、1,4-二羟甲基环己烷、1,4-二乙醇环己烷和2,2-双(4-羟基亚苯基)丙烷(双酚A)的乙氧基化或丙氧基化产物。视聚氨酯所需性质而定,多元醇可单独使用或使用不同用量比之混合物形式的多元醇。适合用于制备聚酯醇的内酯实例为α,α-二甲基-β-丙内酯、γ-丁内酯,较佳是ε-己内酯。
聚醚醇基本上是具有末端羟基而且包含醚键之线性物质。适合的聚醚醇可容易地借聚合环状醚如四氢呋喃,或借一种或多种在亚烷基上具有从2至4个碳原子的氧化烯与包含两个键结在亚烷基上之活性氢原子的起始分子反应而制得。氧化烯的实例是环氧乙烷、1,2-环氧丙烷、表氯醇、1,2-环氧丁烷和2,3-环氧丁烷。可单独使用或者依顺序或以混合物的形式使用氧化烯。所用的起始分子实例是水、二元醇类如乙二醇、丙二醇、1,4-丁烷二醇和1,6-己烷二醇,胺类如亚乙基二胺、六亚甲基二胺和4,4’-二氨基二苯基甲烷,以及氨基醇如乙醇胺。适合的聚酯醇和聚醚醇类以及这些化合物的制法是描述于,例如EP-B 416 386中,以及适合的聚碳酸酯二醇,较佳是这些以1,6-己烷二醇为基质的聚碳酸酯二醇及这些的制法是描述于,例如US-A 4131 731中。
以该醇类的总重量为基准,较佳是使用最高达30重量%具有从2至20个碳原子,较佳是2至10个碳原子的脂族二醇,例如1,2-乙烷二醇、1,3-丙烷二醇、1,4-丁烷二醇、1,6-己烷二醇、1,5-戊烷二醇、1,10-癸烷二醇、2-甲基-1,3-丙烷二醇、2,2-二甲基-1,3-丙烷二醇、2-甲基-2-丁基-1,3-丙烷二醇、2,2-二甲基-1,4-丁烷二醇、1,4-二羟甲基环已烷、新戊二醇羟基新戊酸酯、二甘醇、三甘醇或甲基二乙醇胺,或者具有从8至30个碳原子之芳族-脂族或芳族-环脂族二醇,其中可能的芳族结构是杂环系统或较佳是等环系统,如萘衍生物或特别是苯衍生物,如双酚A、双重对称乙氧基化双酚A、双重对称丙氧基化双酚A、更高度乙氧基化或丙氧基化双酚A衍生物或者双酚F衍生物以及此类化合物的混合物。
以该醇类的总重量为基准较佳使用最高达5重量%具有从3至15个碳原子,较佳是3至10个碳原子的脂族三醇,例如三羟甲基丙烷或甘油,此类化合物与环氧乙烷和/或环氧丙烷的反应产物,或者此类化合物的混合物。
多羟基醇可具有官能基,例如中性基如硅氧烷基,碱性基如特别的叔氨基,或酸性基或其盐类或容易转化成酸性基的基团,该官能基可经由多羟基醇将其导入。较佳是使用具有此类基团之二醇成份,例如N-甲基二乙醇胺、N,N-双(羟基乙基)氨基甲基膦酸二乙基酯或N,N-双(羟基乙基)-2-胺基醋酸(3-磺基丙基)酯或具有此类基团之二羧酸,其可用于制备聚酯醇,例如5-磺基间苯二甲酸。
特别的酸性基是磷酸、膦酸、硫酸、磺酸、羧基或铵基。
容易发展成酸性基的基团实例是酯基或盐类,较佳是碱金属如锂、钠或钾的盐类。
4)本质上描述于上之聚酯醇必须小心以获得从10,000至2,000,000,较佳是从50,000至1,000,000的分子量。
5)聚胺、聚硅氧烷和聚phosphazene,特别是这些上述聚合物IIb2中所讨论的。
6)聚醚醇如,例如上述聚合物IIb1中所讨论的,如化合物(c)或聚氨酯中所讨论的。
当然也可能使用上面聚合物IIb之混合物。根据本发明所用的共聚物IIb视制备的方式而定可包含任意分布的单体或可为一种嵌段共聚物。
聚合物IIa和IIb是以熟谙此技工作者已知的惯用方式进行聚合,较佳是自由基聚合。可使用高分子量或寡聚物形式或这些的混合形式之聚合物IIa和IIb。
聚合物IIa在聚合物粘合剂II中的比例一般是从1至100重量%,较佳是从20至80重量%,最佳是从30至60重量%。聚合物IIb相对于聚合物粘合剂II的比例一般相当于从0至99重量%,较佳是从20至80重量%,最佳是从40至70重量%。
本发明最好提供具有包含下列组合物之第一层的复合体:
如上所定义的组合物,其中该聚合物IIa在沿着链的末端和/或侧边具有至少一个暴露于热和/或UV辐射时有能力抽出氢的以三重激发态存在的反应性基RGa,以及沿着链的末端和/或侧边具有至少一个异于RGa且与RGa共反应之基团RGb,其中所有聚合物分子平均具有至少一个基团RGa和至少一个基团RGb。
如上所定义的组合物,其中该聚合物IIa是一种丙烯酸酯或甲基丙烯酸酯的聚合物或共聚物而且其具有包含二苯甲酮单位之反应性基RGa以及包含二氢二环戊二烯单位之反应性基RGb。
如上所定义的组合物,其中聚合物IIb选自氯化乙烯、丙烯腈或氟化亚乙烯之聚合物或共聚物;一种由氯化乙烯与氯化亚乙烯、氯化乙烯与丙烯腈、氟化亚乙烯与六氟丙烯或者氟化亚乙烯与六氟丙烯所制成的共聚物;一种由氟化亚乙烯和六氟丙烯以及选自氟化乙烯、四氟乙烯和三氟乙烯之一员所制成的三聚物。
如上所定义的组合物,其中聚合物IIa是一种丙烯酸酯或甲基丙烯酸酯的聚合物或共聚物并且其具有包含二苯甲酮单位之反应性基RGa以及包含二氢二环戊二烯单位之反应性基RGb,而且聚合物IIb是一种由氟化亚乙烯和六氟丙烯所制成的共聚物。
再者,根据本发明所用的组合物可包含一种增塑剂III。但是,增塑剂非必须使用的。
若使用增塑剂III,以该组合物为基准其比例是从0.1至100重量%,较佳是从0.5至50重量%,特别是从1至20重量%。
增塑剂III的实例是这些描述于DE-A 198 19 752之增塑剂,较佳是碳酸二甲基酯、碳酸二乙基酯、碳酸二丙基酯、碳酸亚乙酯、1,2-碳酸亚丙酯、1,3-碳酸亚丙酯、有机磷化合物,特别是磷酸酯和膦酸酯如磷酸三甲基酯、磷酸三乙基酯、磷酸三丙基酯、磷酸三丁酯、叁(2-乙基己基)磷酸酯,聚氧化烯醚类和聚氧化烯酯类如二甘醇二甲醚化合物、三甘醇二甲醚化合物和四甘醇二甲醚化合物,聚合物增塑剂如热塑性聚氨酯或聚酰胺以及这些化合物的混合物。
根据本发明所用的组合物可分散或溶于一种无机或有机,较佳是一种有机液体稀释剂中,其中根据本发明混合物的粘度最好是从100至50,000毫帕,然后以本质上已知的方式,例如喷雾涂层、浇铸、浸渍、旋转涂层、辊式涂层、减压印刷、凹板印刷或平板印刷或扫描印刷将其涂覆在基材上。如通常,如借去除稀释剂和熟化该混合物进行进一步的加工。
适合的有机稀释剂是脂族醚类,特别是四氢呋喃和二噁烷、烃类,特别是烃混合物,如石油溶剂油、甲苯或二甲苯,脂族酯类,特别是乙酸乙酯和醋酸丁酯以及酮类,特别是丙酮、乙基甲基酮和环己烷,以及DMF和NMP。也可以使用此类稀释剂之组合物。
可能的基材是通常电极所用的物质,较佳是金属如铝或铜。也可能使用临时基材如薄膜,特别是聚酯薄膜如聚对苯二甲酸乙二醇酯薄膜。此类薄膜最好具有脱模层,较佳是从聚硅氧烷所制成的。
分离器也可热塑性地,例如借注塑、熔化浇铸、压缩、捏合或挤压制得,而且若有需要可在下一个步骤中砑光根据本发明所用的组合物。
自根据本发明所用之组合物制成薄膜后,可去除挥发性成分如溶剂或增塑剂、
根据本发明所用的组合物可依本质上已知的方式交联,例如借离子或离子化辐射照射或一种电子光束,较佳是以从20至2000仟伏特的加速电压及从5至50Mrad的辐射剂量,或者以UV或可见光,较佳是以普通方式加入一种引发剂如特别是不超过1重量%之量的苯偶酰二甲基缩酮或1,3,5-三甲基苯甲酰基三苯基膦氧化物,以聚合物IIa为基准以及一般在从0.5至15分钟的时间内交联;借经由自由基聚合,较佳是在高于60℃下进行热交联,其中最好引发剂,例如偶氮基双异丁烯腈的添加量一般是不超过5重量%,较佳是从0.05至1重量%,以聚合物IIa为基准;借电化学诱发聚合;或借离子聚合,例如借酸催化阳离子聚合,其中可能的催化剂主要是酸类,较佳是路易士酸如BF3,特别是LiBF4或LiPF6。含锂离子的催化剂,如LiBF4或LiPF6在此最好保留在固体电解质或分离器中作为传导盐。
上述交联可以,但非必须在惰性气体中发生。根据本发明,在此可控制辐射时间使其完全交联或仅有短时间UV光预辐射以仅部分交联。
如最如所提及,至少一层第二种根据本发明模制涂层包含一种惯用分离器。根据本发明,在此可使用任何惯用分离器。
就此而论,应特别提及下列化合物:
-以微孔聚烯烃薄膜为基料的分离器,如,例如以商标名Celgard和Hipore可商业取得的以及特别描述于EP-A 0 718 901和EP-B 0715 364中的分离器,以参考方式将其两者整个范围并入本发明申请案中;聚乙烯薄膜和聚丙烯薄膜,以及在此相似地可使用各别包含聚乙烯和聚丙烯与其他聚合物之掺合物的薄膜;
-购自Goretex之微孔聚四氟乙烯(PTFE)薄膜,如,例如EP-A0 798 791所描述的,也以参考方式将其并入本发明申请案中;
-薄金属板、纤维以及非织布物,其所有皆是利用纤维聚合物物质所制成的,如聚烯烃、聚酰胺或聚酯纤维;
-以商标名Nafion所取得的薄膜;
-以二氟化亚乙烯和六氟丙烯之共聚物为基料的薄膜,如,例如US 5 540 741和US 5 478 668中所描述的;
-均聚物、嵌段聚合物和共聚物,在各例中其包含填料而且可借挤压获得的,其是由下列化合物所制得
(a)烯烃类,如乙烯、丙烯、丁烯、异丁烯、丙烯、己烯或较高碳数的同系物、丁二烯、环戊烯、环己烯、降冰片烯或乙烯基环己烷;
(b)芳族烃类,如苯乙烯或甲基苯乙烯;
(c)丙烯酸酯或甲基丙烯酸酯,如分别为甲基、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、苯甲基、三氟甲基、六氟丙基或四氟丙基之丙烯酸酯以及甲基丙烯酸酯;
(d)丙烯腈、甲基丙烯腈、N-甲基吡咯烷酮、N-乙烯基咪唑或乙酸乙烯酯;
(e)乙烯基醚类,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、苯甲基、三氟甲基、六氟丙基或四氟丙基乙烯基醚类;
(f)含卤素烯烃化合物如氯化乙烯、氟化乙烯、氟化亚乙烯、氯化亚乙烯、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,
其中在这些聚合物中,使用根据本发明固体(I)作为填料;此类挤压薄膜的组合物和制法是详细描述于DE-A 19713072.0。
为了制造新颖复合体,将至少一层第一种层与至少一层第二种层结合在一起并且根据本发明,可使用任何已知方法将这两种层结合在一起。例如可在大气压力下加工,如浇铸或刮第一种层的起始物,或者借在超计大气压下加工,如挤压、压层,特别是热压层、砑光或压缩将第一种层涂覆在第二种层上。在此所得的复合体可借辐射或电化学或热力熟化或交联。而且,可先熟化或者部份或完全热交联至少一层第一种层的起始物质,然后如上所描述,在大气压力下或在超计大气压下与根据本发明所用的第二种层结合在一起。若预制成的薄膜,即至少一层薄膜形式之第一种层以及薄膜形式之惯用分离器被结合在一起,这最好是以压层方式,一般在从约100至约160℃,较佳是从约115至约140℃(热压层)的温度下进行,其中在各例中所用的正确温度特别是视各别所用的惯用分离器而定。例如,若在此使用聚丙烯薄膜,其温度可能微高于使用聚乙烯薄膜时的温度。若该复合体是以压层方法所制成的,第一种层的组合物可呈部份或完全交联形式以及压层后所获得的复合体若有需要可再度将其交联或另外直接发使用而无需进行后-交联。
若新颖复合体被用于作为电化学电池中的分离器,该复合体与惯用的阳极和阴极结合。而且,可掺入已知作为传导盐之包含锂阳离子的可分解化合物,若有需要及其他添加剂,特别是如有机溶剂,其有时也被称为电解质。在制造该新颖复合体的过程中掺混入部份或全部最后提及的物质,或在制得复合体后再将其导入。
可能使用的传导盐是为人所熟知的且被描述于,例如EP-A 0 096629中。根据本发明所用的传导盐较佳是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在各例中是从2至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)、Li亚胺盐、Li甲基化物盐类,或者两种或多种这些盐类的混合物,以及较佳是使用LiPF6作为传导盐。
可能的有机电解质溶剂是上面“增塑剂”处所讨论的化合物及这些所用之较佳溶剂是惯用有机电解质,较佳是酯类如碳酸亚乙酯、碳酸亚丙酯、碳酸二甲基酯或碳酸二乙基酯或这类化合物的混合物。
新颖复合体的厚度最好是从5至500微米,较佳是从10至500微米,最佳是从10至200微米,特别是从15至100微米。
该复合体可与阳极和阴极组合形成一种电化学电池,依次其为一种固体复合体件。此复合体件最好具有从30至2000微米之总厚度,特别是从50至1000微米之总厚度。
本发明也提供一种制造此类复合体之方法,其包含下列阶段:
(I)制造至少一层如上所定义的第一种层;
(II)制造至少一层如上所定义的第二种层;以及
(III)制造以惯用涂层方法使至少一层第一种层与至少一层第二种层结合。
至少一层第一种层最好被制造在一种临时基材上。根据本发明,在此可使用惯用临时基材,如由一种聚合物或一种较佳的涂层纸所制成的脱模薄膜,如一种硅化聚酯薄膜。但是,也可在永久基材上如一种收集电极制造此第一种层或甚至完全不需要基材。
借提供涂层或制造薄膜之大气压加工方法如浇铸或刮,或者另外借在超计大气压下加工法,如挤压、压层,特别是热压层、砑光或压缩进行上面所定义之涂层的结合和制造。所得复合体若有需要可借辐射或电化学或热力熟化或交联之。
也可使用上述方法让新颖复合体与惯用电极结合在一起,因此制造一种含有组成份之复合体件(脱模薄膜/分离器/电极)。
也可能以双面涂敷复合体以提供一种具有组成份阳极/分离器/阴极之复合体件。
对于此,在>80℃下将该复合体,作为一种分离器与阳极薄膜和/或阴极薄膜压层在一起。在此新颖的复合体可容易地被压层成惯用阳极或阴极,获得一种复合体件-阳极/-或阴极/-分离器-,然后其可依次与惯用阴极或阳极结合。
不需要各别利用基材和收集电极也可制得如上所述之阳极/分离器/阴极的复合体件,因为如上所定义之包含至少一层第一种层与至少一层第二种层的新颖复合体本质上具有足够的机械稳定性以用于电化学电池中。
在这些涂层被结合在一起之前或者最好是在这些涂层被结合在一起之后,若有需要,可在与适合的收集电极如与一种金属箔完成接触后,或者甚至在复合体或复合体件已分别被导入电池套子后,再将电解质和传导盐放此类复合体件中或放入电化学电池中。在此,新颖复合体中涂层的特殊微孔结构容许电解质和传导盐以置换孔洞中的空气而被吸收,其中特殊微孔结构特别是借所存在之定义于上的固体(I)决定的。视所用的电解质而定,装填是发生在从0至约100℃。
新颖的电化学电池可特别地用于作为一种汽车电池、用具电池、扁平式电池、车上电池、静态用具之电池或电拖拉电池、
该新颖复合体具有下列优于至今供以用于电化学电池之分离器的优点:
-惯用分离器与包含固体(I)之组合物的结合可获得一种具有优异机械稳定性,特别是极佳尺寸稳定性和压缩强度良好的复合体;
-新颖复合体可用于为此目的所用的商业可取得卷切机上,而无任何电池制造上的困难;
-该新颖复合体是具有断电机制的分离器。
现在将利用一些实例来描述本发明。
在此图1至5于各例中显示实例1-5中所得电化学电池的循环(电压:4.15伏特)结果。制备实例I(PA1)
将800克二甲苯加热至85℃。
由下列化合物所制成之混合物构成的进料I100克之 丙烯酸月桂基酯300克之 丙烯酸二氢二环戊二烯酯120克之 甲基丙烯酸缩水甘油酯480克之 丙烯酸乙基己基酯和2克之 巯基乙醇
与由下列化合物所构成之进料II同时开始:30克之 Wako V 59(Azostarter V 59)和200克之 二甲苯。
进料I在1.5小时内以及进料II在2小进内流发电荷。在此温度是被固定在从80至90℃。让该混合物继续在90℃下反应3小时。
然后加入166克4-羟基二苯甲酮和0.83克二甲基氨基吡啶。让反应继续进行从2至3小时直到环氧化物值达到<0.01。实例1
将20克甲基丙烯酸硅烷疏水化硅灰石(Tremin283-600 MST)分散在15克丙酮中。然后将54克包含6克氟化亚乙烯-六氟丙烯共聚物(Kynarflex2801,ELF Atochem)之溶液和4.6克如制备实例1中所制得的PA1溶液加入于34克二甲苯中。最后,加入2.8克叁(2-乙基己基)磷酸酯。
然后在60℃下利用一个具有500微米浇铸缝隙的刮刀将所得组合物涂覆在基材上,在5分钟内去除溶剂,剥掉干涂层后所得薄膜的厚度为约27微米。
在115℃下以压层器滚筒将所得薄膜压层在一种8微米厚不含其他添加剂之商业可取得的微孔PE膜(Celgard)。使用一种Ibico压层器。一旦完成压层,被压在微孔PE膜上之薄层在超光化萤光管(TL 09,Philips)环境中以5厘米的距离光交联5分钟。
所得复合体被用于作为分离器并且与作为阴极之LiCoO2和作为阳极之石墨组合在一起以获得一种“三明治”电池。利用LiPF6作为传导盐及一种1∶1之碳酸亚乙酯和碳酸二亚乙酯的混合物作为液体电解质,施予4.15伏特电压令所得电化学电池循环。
利用此电极可达到的特定电池数据如下:电池测试阴极表面积:1平方厘米阳极表面积:1平方厘米阴极重/单位面积:270克/平方米电解质∶1M LiPF6/碳酸亚乙酯(EC)∶碳酸二亚乙酯(DEC)=1∶1表1
循环 | Li(进) | Li(出) | 库仑效率[%] |
1 | -96 | 105 | 91 |
2 | -97 | 97 | 100 |
3 | -94 | 96 | 98 |
4 | -93 | 93 | 98 |
5 | -89 | 89 | 100 |
从此循环所得结果是分别列于上面表1和图1和2中。在此图1表示充电和放电测验对时间的变化图,其中V是所施电压和t是经过的时间。引人注意的是实例1之三明治电池的充电和放电容量并不随时间而各别变化。由图2可确认之,其中将比充电和放电容量[毫安培时/克]对循环数目(Z)作图。可见到,例如在第5个循环,此电池在阴极上的比充电容量为89毫安培时/克。实例2
依一种相似于实例1利用PA1作为交联系统之方法制造复合体,所不同的是,最初所得薄膜在实例1的条件下照射2秒,然后依相似于实例1之方法将其与PE膜结合在一起。然后如实例1,以UV照射所得复合体并用作为分离器。表2和图3表示电化活性研究的结果。表2
循环数目 | 半循环 | 电流密度[毫安培/平方厘米] | 比电容[毫安培时/克]充电 放电 | |
1 | c(Li出) | 0.5 | 111.6 | |
d(Li入) | -1.0 | 89.1 | ||
2 | c(Li出) | 0.5 | 94.8 | |
d(Li入) | -1.0 | 88.3 | ||
3 | c(Li出) | 0.5 | 89.2 | |
d(Li入) | -1.0 | 85.5 | ||
4 | c(Li出) | 0.5 | 85.7 | |
d(Li入) | -1.0 | 83.5 | ||
5 | c(Li出) | 0.5 | 84.6 | |
d(Li入) | -1.0 | 82.1 | ||
6 | c(Li出) | 0.5 | 82.9 | |
c(Li出) | 0.25 | 6.4 | ||
d(Li入) | -3.0 | 59.5 | ||
7 | c(Li出) | 1.0 | 48.7 | |
d(Li入) | -2.0 | 66.7 | ||
8 | c(Li出) | 1.0 | 65.0 | |
d(Li入) | -2.0 | 66.6 | ||
9 | c(Li出) | 1.0 | 66.7 | |
d(Li入) | -2.0 | 65.8 | ||
10 | c(Li出) | 1.0 | 66.1 | |
d(Li入) | -2.0 | 64.7 | ||
11 | c(Li出) | 1.0 | 65.1 | |
d(Li入) | -2.0 | 63.6 | ||
12 | c(Li出) | 0.5 | 72.5 | |
c(Li出) | 0.25 | 6.0 |
此电池在第5个循环上所获得的放电容量是约82毫安培时/克。实例3
依一种相似于实例2之方法制造电化学电池,但在实例3中,最初所获得的复合体不再另外接受UV后-照射。然后如实例1或2进行循环。此循环结果分别表示于表3和图4中。表3
循环数目 | 半循环 | 电流密度[毫安培/平方厘米] | 比电容[毫安培时/克]充电 放电 | |
1 | c(Li出) | 0.5 | 126.0 | |
d(Li入) | -1.0 | 97.9 | ||
2 | c(Li出) | 0.5 | 100.3 | |
d(Li入) | -1.0 | 97.2 | ||
3 | c(Li出) | 0.5 | 100.8 | |
d(Li入) | -1.0 | 96.9 | ||
4 | c(Li出) | 0.5 | 99.5 | |
d(Li入) | -1.0 | 96.2 | ||
5 | c(Li出) | 0.5 | 99.0 | |
d(Li入) | -1.0 | 95.5 | ||
6 | c(Li出) | 0.5 | 97.6 | |
c(Li出) | 0.25 | 5.4 | ||
d(Li入) | -3.0 | 91.1 | ||
7 | c(Li出) | 1.0 | 83.7 | |
d(Li入) | -2.0 | 88.4 | ||
8 | c(Li出) | 1.0 | 89.3 | |
d(Li入) | -2.0 | 88.1 | ||
9 | c(Li出) | 1.0 | 89.9 | |
d(Li入) | -2.0 | 88.0 | ||
10 | c(Li出) | 1.0 | 89.6 | |
d(Li入) | -2.0 | 87.5 | ||
11 | c(Li出) | 1.0 | 88.6 | |
d(Li入) | -2.0 | 86.8 | ||
12 | c(Li出) | 0.5 | 94.5 | |
c(Li出) | 0.25 | 4.5 |
此电池在第5个循环上所获得的放电容量是约95.5毫安培时/克。实例4
如实例1,先制造一种薄膜,未经照射在140℃下将其压在一种阳极(石墨在Cu薄膜)上,并且在115℃下将所得复合体件压在一种8微米厚之微孔PE膜(Celgard)上。
以一种相似于实例1利用LiCoO2作为阴极之方法组成一种“三明治”电池并研究其电化学活性。该结果列于表4和图5中。表4
循环数目 | 半循环 | 电流密度[毫安培/平方厘米] | 比电容[毫安培时/克]充电 放电 | |
1 | c(Li出) | 0.5 | 108.4 | |
d(Li入) | -1.0 | 81.2 | ||
2 | c(Li出) | 0.5 | 91.0 | |
d(Li入) | -1.0 | 83.7 | ||
3 | c(Li出) | 0.5 | 88.4 | |
d(Li入) | -1.0 | 81.7 | ||
4 | c(Li出) | 0.5 | 85.4 | |
d(Li入) | -1.0 | 79.7 | ||
5 | c(Li出) | 0.5 | 82.1 | |
d(Li入) | -1.0 | 77.0 | ||
6 | c(Li出) | 0.5 | 77.9 | |
c(Li出) | 0.25 | 4.2 | ||
d(Li入) | -3.0 | 62.3 | ||
7 | c(Li出) | 1.0 | 49.3 | |
d(Li入) | -2.0 | 51.8 | ||
8 | c(Li出) | 1.0 | 49.9 | |
d(Li入) | -2.0 | 47.2 | ||
9 | c(Li出) | 1.0 | 46.6 | |
d(Li入) | -2.0 | 43.9 | ||
10 | c(Li出) | 1.0 | 43.7 | |
d(Li入) | -2.0 | 41.3 | ||
11 | c(Li出) | 1.0 | 41.1 | |
d(Li入) | -2.0 | 38.8 | ||
12 | c(Li出) | 0.5 | 54.3 | |
c(Li出) | 0.25 | 5.0 |
此电池在第5个循环上所获得的放电容量是约77毫安培时/克。
实例5和实例6被描述于下并且两者皆关于新颖复合体的制造,然后其可以一种相似于实例1至4中所描述的复合体之方式用于电化学电池中。实例5
以刮刀将一种包含下列化合物之悬浮液20克之 Tremin800EST硅灰石34克之 二甲苯6克之 Kynarflex28012.9克之 叁(2-乙基己基)磷酸酯15克之 丙酮和4.6克之 一种包含下列化合物之溶液100克之 丙烯酸月桂基酯300克之 丙烯酸二氢二环戊二烯基酯120克之 甲基丙烯酸缩水甘油酯480克之 丙烯酸乙基己基酯2克之 巯基乙醇30克之 WakoV79200克之 二甲苯166克之 4-羟基二苯甲酮和0.83克之 二甲基氨基吡啶涂覆在一种微孔聚烯烃薄膜上(Celgard2300),在室温下干燥之,如实例1中所描述的以光化学方式熟化之并且在真空中干燥之(<0.1毫巴)。实例6
以刮刀将一种包含下列化合物之悬浮液30克之 Kynarflex280120克之 Aerosil12.5克之 苯二甲酸二丁基酯和200克之 丙酮涂覆在一种微孔聚烯烃薄膜上(Celgard2300)并在室温下干燥之。然后以乙醚萃取该复合体数次。
Claims (11)
1.一种复合体,它包含含下列成份之至少一层:
(a)从1至99重量%之固体(I),其具有5毫微米至100微米主要粒径,或由至少两种固体所形成的混合物;
(b)从99至1重量%之聚合物粘合剂(II),其包括:
(IIa)从1至100重量%之聚合物或共聚物(IIa),沿着链的末端和/或侧边具有反应性基(RG),其暴露于热和/或UV辐射下时可进行交联反应,以及
(IIb)从0至99重量%之至少一种聚合物或共聚物(IIb),其不具反应性基RG,
其中至少一层被涂敷在至少一层第二种层上,其中该第二种层包含至少一个惯用分离器。
2.根据权利要求1之复合体,其中至少一种惯用分离器选自一种微孔聚烯烃薄膜和一种聚四氟乙烯薄膜。
3.根据权利要求1或2之复合体,其中该固体I选自一种无机固体,其选自氧化物、混合氧化物、硅酸盐、硫酸盐、碳酸盐、磷酸盐、氮化物、酰胺、酰亚胺和周期表中第一、第二、第三或第四主族元素或第四族过渡金属元素的碳化物;一种选自聚乙烯、聚丙烯、聚苯乙烯、聚四氟乙烯和聚偏氟乙烯的聚合物;聚酰胺、聚酰亚胺;以及一种包含此类聚合物之固体分散液;和两种或多种这些物质的混合物。
4.根据权利要求1至3中任一项之复合体,其中聚合物IIa沿着链的末端和/或侧边具有至少一个反应性基RGa,当反应性基暴露于热和/或UV辐射下,其在三重激发态下可抽出氢,而且沿着链的末端和/或侧边,其具有至少一个异于RGa且可与RGa共反应之基团RGb,其中所有聚合物分子平均具有至少一个基团RGa和至少一个基团RGb。
5.根据权利要求1至4中任一项之复合体,其中聚合物IIa是一种丙烯酸酯或甲基丙烯酸酯的聚合物或共聚物并且具有包含二苯甲酮单位之反应性基RGa和包含二氢二环戊二烯单位之反应性基RGb。
6.根据权利要求1至5中任一项之复合体,其中聚合物IIb选自氯化乙烯、丙烯腈或氟化亚乙烯之聚合物或共聚物;由氯化乙烯与氯化亚乙烯、氯化乙烯与丙烯腈、氟化亚乙烯与六氟丙烯或氟化亚乙烯与六氟丙烯所制成的共聚物;由氟化亚乙烯与六氟丙烯以及选自包含氟化乙烯、四氟乙烯和三氟乙烯中之一员所制成的三聚物。
7.根据权利要求1至6中任一项之复合体,其中聚合物IIa是一种如权利要求5中所定义的聚合物以及聚合物IIb是由氟化亚乙烯和六氟丙烯所制成的共聚物。
8.一种分离器,它包含至少一种权利要求1至7中任一项之复合体。
9.一种电化学电池,它包含权利要求8之分离器。
10.一种制造权利要求1至7中任一项之复合体的方法,其包括下列阶段:
(I)制造至少一层权利要求1至7中任一项所定义的第一层;
(II)然后使至少一层第一层与至少一层包含至少一种惯用分离器之第二层结合。
11.根据权利要求10的方法,其中结合至少一层与至少一层包含至少一种分离器之第二种层,借刮刀将至少一层涂覆在至少一种惯用分离器上,或者至少一层被压层,较佳是热压层在至少一种分离器上。
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WO2000026977A1 (de) | 2000-05-11 |
DE59902883D1 (de) | 2002-10-31 |
JP2002529891A (ja) | 2002-09-10 |
KR100688402B1 (ko) | 2007-03-09 |
CN100477340C (zh) | 2009-04-08 |
AU1268900A (en) | 2000-05-22 |
KR20010100979A (ko) | 2001-11-14 |
US6632561B1 (en) | 2003-10-14 |
BR9915069A (pt) | 2001-07-17 |
DE19850826A1 (de) | 2000-05-11 |
CA2348917C (en) | 2010-01-19 |
ES2184511T3 (es) | 2003-04-01 |
BR9915069B1 (pt) | 2011-02-08 |
CA2348917A1 (en) | 2000-05-11 |
TW457738B (en) | 2001-10-01 |
EP1138092A1 (de) | 2001-10-04 |
EP1138092B1 (de) | 2002-09-25 |
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