CN106661413A - 金属箔与树脂膜的层压用粘接剂、使用该组合物的叠层体、电池外包装用包装材和电池外壳 - Google Patents

金属箔与树脂膜的层压用粘接剂、使用该组合物的叠层体、电池外包装用包装材和电池外壳 Download PDF

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Publication number
CN106661413A
CN106661413A CN201580035853.1A CN201580035853A CN106661413A CN 106661413 A CN106661413 A CN 106661413A CN 201580035853 A CN201580035853 A CN 201580035853A CN 106661413 A CN106661413 A CN 106661413A
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China
Prior art keywords
resin film
metal forming
bonding agent
lamination
layer
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Granted
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CN201580035853.1A
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CN106661413B (zh
Inventor
江夏宽人
深濑成
深濑一成
村田直树
李晖
中川康宏
土井满
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Lishennoco Co ltd
Resonac Holdings Corp
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Showa Denko KK
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    • B29C51/002—Shaping by thermoforming, i.e. shaping sheets or sheet like preforms after heating, e.g. shaping sheets in matched moulds or by deep-drawing; Apparatus therefor characterised by the choice of material
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Abstract

一种金属箔与树脂膜的层压用粘接剂等，具有聚氨基甲酸酯多元醇(A)、和饱和脂肪族和/或饱和脂环式多异氰酸酯(B)，所述聚氨基甲酸酯多元醇(A)是将含有链状聚烯烃多元醇(a1)和/或聚酯多元醇(a2)、含有羟基的烃化合物(b)、以及多异氰酸酯(c)的成分加聚而获得的，所述聚酯多元醇(a2)具有源自氢化二聚酸的结构单元和源自氢化二聚二元醇的结构单元，所述含有羟基的烃化合物(b)同时具有饱和或不饱和的环式烃结构和2个以上羟基。

Description

金属箔与树脂膜的层压用粘接剂、使用该组合物的叠层体、电 池外包装用包装材和电池外壳
技术领域
本发明涉及适合锂离子电池等二次电池的外包装材料用的粘接剂的金属箔与树脂膜的层压用粘接剂、使用该金属箔与树脂膜的层压用粘接剂而制造的叠层体、使用了该叠层体的电池外包装用包装材以及将该电池外包装用包装材成型而得的电池外壳。
背景技术
近年来，笔记本电脑、手机等电子设备的小型化、轻量化、薄型化正在推进。因此，对于电子设备用的二次蓄电池，也要求高性能化、轻量化、移动性能的提高，代替以往的铅蓄电池，具有高能量密度的锂离子电池的开发在积极地进行。此外，也能够用于电动汽车、混合动力汽车的电源的锂离子电池正在被实用化。
在锂离子电池中，使用包含锂的化合物作为正极材料，使用石墨、焦炭等碳材料作为负极材料。进而，在正极和负极之间具备由电解液或含浸了该电解液的聚合物凝胶形成的电解质层，所述电解液是在碳酸亚丙酯、碳酸亚乙酯等具有渗透力的非质子性溶剂中溶解了作为电解质的LiPF6、LiBF4等锂盐而得的电解液。
一直以来，作为电池外壳用包装材料，已知有依次叠层了作为外侧层的耐热性树脂拉伸膜层、铝箔层和作为内侧层的热塑性树脂未拉伸膜层而得的叠层体。在使用这样的结构的电池外壳用包装材料而得的电池外壳的情况下，如果电解液这样具有渗透力的溶剂透过用于电池的外包装的叠层体中的作为密封剂的膜层，则铝箔层与树脂膜层间的层压强度下降，可能会成为电解液泄露的原因。因此，开发了一种在铝箔层与内侧层之间经由粘接剂层进行粘接的电池外壳用包装材料，所述粘接剂层含有包含酸酐基或羧基、羟基等具有与异氰酸酯的反应性的官能团的树脂、和多官能异氰酸酯化合物。
例如，专利文献1中记载了使用使下述改性聚烯烃树脂和多官能异氰酸酯化合物溶解或分散于有机溶剂中而得的溶剂型粘接剂来形成粘接剂层的方法，所述改性聚烯烃树脂是使丙烯的均聚物或丙烯和乙烯的共聚物与烯属不饱和羧酸或其酸酐进行接枝聚合而得到的。
另一方面，专利文献2中记载了将聚烯烃多元醇和多官能异氰酸酯固化剂作为必需成分，进而添加了热塑性弹性体和/或增粘剂的粘接剂组合物；专利文献3中记载了含有主剂和固化剂的粘接剂组合物，所述主剂选自具有源自二聚体脂肪酸或其氢化物的疏水性单元的聚酯多元醇、和该聚酯多元醇的异氰酸酯伸长物中的至少1种，所述固化剂包含选自粗甲苯二异氰酸酯、粗二苯基甲烷二异氰酸酯和聚二苯基甲烷二异氰酸酯中的1种以上的多异氰酸酯化合物。
现有技术文献
专利文献
专利文献1：日本特开2010-92703号公报
专利文献2：日本特开2005-63685号公报
专利文献3：日本特开2011-187385号公报
发明内容
发明所要解决的课题
然而，专利文献1的改性聚烯烃树脂在长期保存中、溶剂溶解后有经时变化，往往存在涂布时的操作性会变得不稳定的情况，此外，所形成的粘接剂层的粘接力可能会产生不均匀。此外，还有设想车载用途等的高温下的粘接力差这样的担心。
此外，关于专利文献2和专利文献3的情况，涂布时的操作性、粘接力相对稳定，但是存在如下问题：如果粘接剂层与透过叠层体中的作为密封剂的膜层的电解液接触，则粘接力下降，从而电池的品质下降。
本发明是在上述的背景技术下完成的，其目的在于提供一种用于将层压用金属箔与树脂膜层压的粘接剂，其具有优异的粘接力、且适合用于将铝箔与热熔接性树脂膜接合。此外，本发明的另一目的在于提供一种金属箔与树脂膜的叠层体，其耐热性、耐电解液性优异、且适合电池外包装用包装材。此外，本发明的另一目的在于提供一种耐热性、耐电解液性优异的电池外壳，其是使用包含该叠层体的电池外包装用包装材料形成的。
用于解决课题的方法
即，本发明涉及以下的〔1〕～〔15〕。
〔1〕一种聚氨基甲酸酯多元醇，是用于聚氨基甲酸酯系粘接剂的多元醇，其是将含有链状聚烯烃多元醇(a1)和/或聚酯多元醇(a2)、含有羟基的烃化合物(b)、以及多异氰酸酯(c)的成分加聚而获得的，所述聚酯多元醇(a2)具有源自氢化二聚酸的结构单元和源自氢化二聚二元醇的结构单元，所述含有羟基的烃化合物(b)同时具有饱和或不饱和的环式烃结构和2个以上羟基。
〔2〕一种金属箔与树脂膜的层压用粘接剂，具有聚氨基甲酸酯多元醇(A)、和饱和脂肪族和/或饱和脂环式多异氰酸酯(B)，所述聚氨基甲酸酯多元醇(A)是将含有链状聚烯烃多元醇(a1)和/或聚酯多元醇(a2)、含有羟基的烃化合物(b)、以及多异氰酸酯(c)的成分加聚而获得的，所述聚酯多元醇(a2)具有源自氢化二聚酸的结构单元和源自氢化二聚二元醇的结构单元，所述含有羟基的烃化合物(b)同时具有饱和或不饱和的环式烃结构和2个以上羟基。
〔3〕根据〔2〕所述的金属箔与树脂膜的层压用粘接剂，前述含有羟基的烃化合物(b)是含有具有交联结构的饱和脂环结构的多元醇。
〔4〕根据〔2〕或〔3〕所述的金属箔与树脂膜的层压用粘接剂，前述含有羟基的烃化合物(b)是双酚化合物。
〔5〕根据〔2〕～〔4〕中任一项所述的金属箔与树脂膜的层压用粘接剂，前述多异氰酸酯(c)是饱和脂环式二异氰酸酯。
〔6〕根据〔2〕～〔5〕中任一项所述的金属箔与树脂膜的层压用粘接剂，前述链状聚烯烃多元醇(a1)是实质上不含有不饱和烃结构的聚烯烃多元醇。
〔7〕根据〔2〕～〔6〕中任一项所述的金属箔与树脂膜的层压用粘接剂，相对于(a1)成分和(a2)成分的总量100质量份，(b)成分为5～100质量份，相对于(a1)成分、(a2)成分和(b)成分中包含的羟基数，(c)成分中包含的异氰酸酯基数的比率为0.5～1.3。
〔8〕根据〔2〕～〔7〕中任一项所述的金属箔与树脂膜的层压用粘接剂，相对于前述聚氨基甲酸酯多元醇(A)中包含的羟基数，多异氰酸酯(B)中包含的异氰酸酯基数的比率为1～15。
〔9〕根据〔2〕～〔8〕中任一项所述的金属箔与树脂膜的层压用粘接剂，其还含有溶剂(C)。
〔10〕一种叠层体，是金属箔与树脂膜经由粘接剂层进行叠层而得的，所述粘接剂层是由〔2〕～〔9〕中任一项所述的金属箔与树脂膜的层压用粘接剂得到的。
〔11〕根据〔10〕所述的叠层体，前述金属箔是铝箔，前述树脂膜含有热熔接性树脂膜。
〔12〕根据〔10〕或〔11〕所述的叠层体，前述金属箔的厚度是10～100μm，前述树脂膜的厚度是9～100μm。
〔13〕一种电池外包装用包装材料，其是使用〔10〕～〔12〕中任一项所述的叠层体而获得的。
〔14〕一种电池外壳，其是使用〔13〕所述的电池外包装用包装材料而获得的。
〔15〕一种电池外壳的制造方法，对〔13〕所述的电池外包装用包装材料进行深拉成型或拉伸成型。
发明效果
本发明的金属箔与树脂膜的层压用粘接剂的粘接力优异，使用该金属箔与树脂膜的层压用粘接剂而形成的金属箔与树脂膜的叠层体的耐热性、耐电解液性优异，因此适合作为用于锂离子电池等二次电池的制作的电池外包装用包装材料的素材。此外，使用本发明的电池外包装用包装材料进行成型的电池外壳的耐热性、耐电解液性优异，通过使用该电池外壳，可以提供寿命长的安全的二次电池。
具体实施方式
本发明的金属箔与树脂膜的层压用粘接剂含有聚氨基甲酸酯多元醇(A)、和饱和脂肪族和/或饱和脂环式多异氰酸酯(B)，所述聚氨基甲酸酯多元醇(A)是将含有链状聚烯烃多元醇(a1)和/或聚酯多元醇(a2)、含有羟基的烃化合物(b)、以及多异氰酸酯(c)的成分加聚而获得的，所述聚酯多元醇(a2)具有源自氢化二聚酸的结构单元和源自氢化二聚二元醇的结构单元，所述含有羟基的烃化合物(b)同时具有饱和或不饱和的环式烃结构和2个以上羟基。
在本发明的金属箔与树脂膜的层压用粘接剂中，前述聚氨基甲酸酯多元醇(A)相当于主剂，前述饱和脂肪族和/或饱和脂环式多异氰酸酯(B)相当于固化剂。
本发明的金属箔与树脂膜的层压用粘接剂可以适用于金属箔与树脂膜的粘接，特别是作为金属箔与树脂膜层压用的粘接剂是有用的，其叠层体可以适合作为电池外包装用包装材料使用。
在这里，本说明书中的“～”，意思是“～”这样的符号前的值以上、“～”这样的符号后的值以下。
<聚氨基甲酸酯多元醇(A)>
如上所述，用于本发明的聚氨基甲酸酯多元醇(A)是将含有(a1)和/或(a2)成分、(b)成分以及(c)成分的成分进行加聚而得到的。
〔链状聚烯烃多元醇(a1)〕
本发明的“链状聚烯烃多元醇(a1)”，意思是不包含脂环结构的聚烯烃多元醇(a1)。
用于本发明的链状聚烯烃多元醇(a1)(以下也称为“聚烯烃多元醇(a1)”)只要含有使1种或2种以上的烯烃聚合或共聚而成的聚烯烃骨架、和2个以上羟基、且不具有脂环结构的物质就没有特别限制。作为具体例，可举出聚丁二烯多元醇、聚异戊二烯多元醇等聚二烯多元醇、聚二烯多元醇与聚烯烃的接枝聚合物和这些聚二烯多元醇、接枝聚合物的氢化物等。这些聚烯烃多元醇可以单独或混合2种以上来使用。从由本发明的金属箔与树脂膜的层压用粘接剂得到的粘接剂层的耐电解液性的观点出发，优选结构中实质上不包含不饱和烃结构的链状聚烯烃多元醇，可举出例如，上述举出的各种聚二烯多元醇的氢化物、接枝聚合物的氢化物。作为它们的市售品，可举出例如，GI-1000、GI-2000、GI-3000(均为日本曹达株式会社制)、エポール(出光兴产株式会社制)等。
聚烯烃多元醇(a1)的数均分子量优选为1000～10,000。如果数均分子量为1000以上，则由本发明的金属箔与树脂膜的层压用粘接剂得到的粘接剂层即使接触到电解液，其粘接力也变得不容易下降；如果数均分子量为10,000以下，则后述的聚氨基甲酸酯多元醇(G)在溶剂中的溶解性、和涂布本发明的金属箔与树脂膜的层压用粘接剂时的操作性变得良好。
需要说明的是，本发明中的数均分子量是使用凝胶渗透色谱法(昭和电工株式会社制，Shodex GPC System-11，“Shodex”(注册商标))，在下述条件下在常温下进行测定，利用标准聚苯乙烯标准曲线而求出的值。
柱：昭和电工株式会社制，KF-806L
柱温：40℃
试样：试样聚合物的0.2质量％四氢呋喃溶液
流量：2ml/分钟
洗脱液：四氢呋喃
检测器：差示折射率计(RI)
〔具有源自氢化二聚酸的结构单元、和源自氢化二聚二元醇的结构单元的聚酯多元醇(a2)〕
从由本发明的金属箔与树脂膜的层压用粘接剂得到的粘接剂层的耐电解液性的观点出发，用于本发明的、具有源自氢化二聚酸的结构单元和源自氢化二聚二元醇的结构单元的聚酯多元醇(a2)(以下也称为“聚酯多元醇(a2)”)具有源自氢化二聚酸的结构单元、和源自氢化二聚二元醇的结构单元。
本说明书中的“二聚酸”，是指使具有烯属双键的碳原子数为14～22的脂肪酸(以下也称为“不饱和脂肪酸A”)在双键部进行反应而得的二聚体酸。优选为使具有2～4个烯属双键的不饱和脂肪酸A与具有1～4个烯属双键的不饱和脂肪酸A进行反应而得的二聚体酸，更优选为使具有2个烯属双键的不饱和脂肪酸A与具有1或2个烯属双键的不饱和脂肪酸A进行反应而得的二聚体酸。作为上述不饱和脂肪酸A，可举出十四碳烯酸(粗租酸、抹香鲸酸、肉豆蔻脑酸)、十六碳烯酸(棕榈油酸等)、十八碳烯酸(油酸、反油酸、异油酸等)、二十碳烯酸(顺式-9-二十碳烯酸等)、二十二碳烯酸(芥酸、鲸蜡烯酸、巴西烯酸等)、十四碳二烯酸、十六碳二烯酸、十八碳二烯酸(亚油酸等)、二十碳二烯酸、二十二碳二烯酸、十八碳三烯酸(亚麻酸等)、二十碳四烯酸(花生四烯酸等)等，最优选油酸或亚油酸。通常，所得的二聚酸由于双键的结合部位、异构化的原因，所以是结构不同的二聚酸混合物，可以进行分离后使用，也可以直接使用，进而，所得的二聚酸也可以含有少量的单体酸(例如6重量％以下，特别是4重量％以下)、三聚酸以上的多聚体酸等(例如6重量％以下，特别是4重量％以下)。
本说明书中的“氢化二聚酸”，是指将上述二聚酸的碳-碳双键氢化而得的饱和二羧酸。作为氢化二聚酸的市售品，可举出例如，EMPOL1008和EMPOL1062(均为BASF社制)、PRIPOL1009等(クローダ社制)等。
本发明中的“氢化二聚二元醇”，是将上述二聚酸、上述氢化二聚酸和其低级醇酯中的至少1种在催化剂存在下进行还原，将二聚酸的羧酸或羧酸酯部分制成醇，在原料中具有碳-碳双键的情况下将其双键氢化而获得二醇，将这样的二醇作为主成分的氢化二聚二元醇。作为氢化二聚二元醇的市售品，可举出例如，Sovermol908(BASF社制)、PRIPOL2033等(クローダ社制)。
用于本发明的聚酯多元醇(a2)可以通过使以前述氢化二聚酸作为必需成分的酸成分、和以前述氢化二聚二元醇作为必需成分的醇成分在酯化催化剂的存在下进行缩合反应而制造。或者，还可以通过使以前述氢化二聚酸的低级烷基酯作为必需成分的酯成分、和以前述氢化二聚二元醇作为必需成分的醇成分在酯交换催化剂的存在下进行酯交换反应而制造。
〔同时具有饱和或不饱和的环式烃结构和2个以上羟基的含有羟基的烃化合物(b)〕
从由本发明的金属箔与树脂膜的层压用粘接剂得到的粘接剂层的耐电解液性的观点出发，用于本发明的同时具有饱和或不饱和的环式烃结构和2个以上羟基的含有羟基的烃化合物(b)(以下也称为“含有羟基的环式烃(b)”)只要是具有不饱和或饱和脂环式烃结构和2个以上羟基、且其他部分的结构是由烃构成的化合物就没有特别限制。
作为饱和环式烃结构，可举出环戊烷骨架、环己烷骨架、环庚烷骨架等环烷烃骨架，降冰片烷骨架、金刚烷骨架、三环癸烷骨架等具有桥连结构的饱和脂环结构等，作为具有那样的结构的含有羟基的环式烃(b)，可举出环戊烷二醇、环己烷二醇、环己烷二甲醇、降冰片烷二醇、金刚烷二醇、三环癸烷二甲醇等。这些化合物可以单独或混合2种以上来使用。优选包含具有桥连结构的饱和脂环结构的环式烃，作为优选的例子，可举出降冰片烷二醇、金刚烷二醇、三环癸烷二甲醇等。作为它们的市售品，可举出金刚烷三醇(出光兴产株式会社制，三菱ガス化学株式会社制)、TCDアルコールDM(オクセア社制)等。
作为不饱和环式烃结构，可举出环戊烯骨架、环己烯骨架、环庚烯骨架、[4n]轮烯骨架等环烯烃骨架，苯骨架、萘骨架、蒽骨架、薁骨架、[4n+2]轮烯骨架等共轭环结构，二环戊二烯骨架等具有桥连结构的不饱和脂环结构等，作为具有那样的结构的多元醇(b)，可举出环己烯二醇、联苯酚、双酚、萘二醇、二环戊二烯二甲醇等。这些化合物可以单独或混合2种以上来使用。优选为双酚，可举出双酚A、双酚B、双酚C、双酚E、双酚F、双酚G、双酚Z等，更优选为双酚A。
〔多异氰酸酯(c)〕
作为用于本发明的多异氰酸酯(c)，只要是含有2个以上异氰酸酯基的化合物、或其多聚体就无特别限制。可举出例如，1,4-环己烷二异氰酸酯、异佛尔酮二异氰酸酯、亚甲基双(4-环己基异氰酸酯)、1,3-双(异氰酸酯基甲基)环己烷、1,4-双(异氰酸酯基甲基)环己烷、降冰片烷二异氰酸酯等饱和脂环式二异氰酸酯，2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、二苯基甲烷-4,4’-二异氰酸酯、1,3-苯二甲基二异氰酸酯、1,4-苯二甲基二异氰酸酯等芳香族二异氰酸酯，六亚甲基二异氰酸酯、2,4,4-三甲基六亚甲基二异氰酸酯、2,2,4-三甲基六亚甲基二异氰酸酯等脂肪族二异氰酸酯，或者它们的脲基甲酸酯化多聚体、异氰脲酸酯化物、缩二脲改性物等。这些化合物可以单独或混合2种以上来使用。优选为饱和脂环式二异氰酸酯，可举出1,4-环己烷二异氰酸酯、异佛尔酮二异氰酸酯、亚甲基双(4-环己基异氰酸酯)、1,3-双(异氰酸酯基甲基)环己烷、1,4-双(异氰酸酯基甲基)环己烷、降冰片烷二异氰酸酯等，特别优选为异佛尔酮二异氰酸酯(3-异氰酸酯基甲基-3,5,5-三甲基环己基异氰酸酯)、亚甲基双(4-环己基异氰酸酯)(别名：二环己基甲烷-4,4’-二异氰酸酯)。作为它们的市售品，可举出デスモジュールI、デスモジュールW(分别是バイエル社制)、IPDI、H12MDI(分别是デグッサ社制)等。
〔聚氨基甲酸酯多元醇(A)的制造方法〕
作为用于本发明的聚氨基甲酸酯多元醇(A)的制造方法，可通过以下反应来进行：在二月桂酸二丁基锡、二月桂酸二辛基锡、2-乙基己酸铋、四乙酰丙酮锆这样的公知的氨基甲酸酯化催化剂的存在下或存在这些催化剂的条件下，使聚烯烃多元醇(a1)和/或聚酯多元醇(a2)、含有羟基的环式烃化合物(b)、和多异氰酸酯(c)进行加聚反应。在催化剂的存在下使其反应，在缩短反应时间的意义上是优选的。此外，该催化剂还作为聚氨基甲酸酯多元醇(A)与饱和脂肪族和/或饱和脂环式多异氰酸酯(B)进行反应并固化时的固化促进剂发挥作用，因此存在催化剂是优选的。但是，如果过于大量使用，则最终有可能会对作为金属箔与树脂膜的层压用粘接剂的物性产生不良影响，因此，相对于(a1)、(a2)、(b)和(c)成分的总量100质量份，使用量优选为0.001～1质量份，更优选为0.005～0.5质量份，进一步优选为0.01～0.3质量份。此外，加聚反应可以使聚烯烃多元醇(a1)和/或聚酯多元醇(a2)、含有羟基的环式烃化合物(b)、和多异氰酸酯(c)全部一次进行反应，也可以在使聚烯烃多元醇(a1)和/或聚酯多元醇(a2)、和含有羟基的环式烃化合物(b)分别各自与多异氰酸酯(c)反应、或者将(a2)、(b)成分适当组合并与多异氰酸酯(c)反应之后，将所有成分混合而进一步使其反应。后者的方法可举出例如，在使含有羟基的环式烃化合物(b)和多异氰酸酯(c)进行反应而获得聚氨基甲酸酯多异氰酸酯后，使聚烯烃多元醇(a1)和/或聚酯多元醇(a2)进行反应而获得聚氨基甲酸酯多元醇(A)等方法。
此外，该加聚反应可以在溶剂中进行。对使用的溶剂无特别限制，但是如果使用与后述的本发明的金属箔与树脂膜的层压用粘接剂中可以含有的溶剂(C)相同的溶剂，则可以省去蒸馏除去溶剂等工序，能够更低成本且减少环境负荷地制造。
制造聚氨基甲酸酯多元醇(A)时，相对于(a1)、(a2)和(b)成分中包含的羟基数，多异氰酸酯(c)中包含的异氰酸酯基数的比率(以下也称为“NCO/OH比”)优选为0.5～1.3，更优选为0.7～1.2，进一步优选为0.8～1.1。如果是0.5以上，则由本发明的金属箔与树脂膜的层压用粘接剂得到的粘接剂层即使接触电解液，粘接力也变得不容易下降；如果是1.3以下，则聚氨基甲酸酯多元醇(A)制造时的凝胶化不容易发生，此外涂布本发明的金属箔与树脂膜的层压用粘接剂时的操作性变得良好。需要说明的是，各多元醇成分中包含的羟基数可以利用JIS K 1557-1这样的滴定法、JIS K 1557-6这样的分光法等公知的方法求出。在后述的实施例中，使用了JIS K 1557-1(滴定法)。各异氰酸酯成分中包含的异氰酸酯基数可以利用JIS K 6806这样的滴定法等公知的方法求出。
制造聚氨基甲酸酯多元醇(A)时，相对于(a1)和(a2)成分的总量100质量份，含有羟基的环式烃化合物(b)的比率优选为5～100质量份，更优选为10～50质量份，进一步优选为10～45质量份。如果是5质量份以上，则由本发明的金属箔与树脂膜的层压用粘接剂得到的粘接剂层即使接触电解液，粘接力也变得不容易下降；如果是100质量份以下，则聚氨基甲酸酯多元醇(A)在溶剂中的溶解性、和涂布本发明的金属箔与树脂膜的层压用粘接剂时的操作性变得良好。
<饱和脂肪族和/或饱和脂环式多异氰酸酯(B)>
本发明中的饱和脂肪族和/或饱和脂环式多异氰酸酯(B)(以下也称为“多异氰酸酯(B)”)在本发明的金属箔与树脂膜的层压用粘接剂中是作为固化剂配合的，与前述的作为制造聚氨基甲酸酯多元醇(A)时的原料记载的多异氰酸酯(c)区别开来记载。
用于本发明的饱和脂肪族和/或饱和脂环式多异氰酸酯(B)只要是包含2个以上异氰酸酯基的化合物或它们的多聚体就没有特别限制。可举出例如，六亚甲基二异氰酸酯、2,4,4-三甲基六亚甲基二异氰酸酯、2,2,4-三甲基六亚甲基二异氰酸酯等脂肪族二异氰酸酯，1,4-环己烷二异氰酸酯、异佛尔酮二异氰酸酯、亚甲基双(4-环己基异氰酸酯)、1,3-双(异氰酸酯基甲基)环己烷、1,4-双(异氰酸酯基甲基)环己烷、降冰片烷二异氰酸酯等饱和脂环式二异氰酸酯，或者它们的脲基甲酸酯化多聚体、异氰脲酸酯化物、缩二脲改性物等。这些化合物可以单独或混合2种以上来使用。从由本发明的金属箔与树脂膜的层压用粘接剂得到的粘接剂层的耐电解液性的观点出发，更优选为饱和脂肪族二异氰酸酯与饱和脂环式二异氰酸酯的组合、以及仅使用饱和脂环式二异氰酸酯。
多异氰酸酯(B)相对于聚氨基甲酸酯多元醇(A)的NCO/OH比优选为1～20，更优选为1～15，进一步优选为1～13。如果NCO/OH比为1以上，则由本发明的金属箔与树脂膜的层压用粘接剂得到的粘接剂层的粘接力、特别是对树脂膜的粘接力变得良好；如果NCO/OH比为20以下，则由本发明的金属箔与树脂膜的层压用粘接剂得到的粘接剂层即使接触电解液，粘接力也不容易下降。
<溶剂(C)>
本发明的金属箔与树脂膜的层压用粘接剂可以含有溶剂(C)。溶剂(C)只要是能够溶解或分散聚氨基甲酸酯多元醇(A)和多异氰酸酯(B)的溶剂就没有特别限制。可举出例如，甲苯、二甲苯等芳香族系有机溶剂，环己烷、甲基环己烷、乙基环己烷等脂环式系有机溶剂，正己烷、正庚烷等脂肪族系有机溶剂，乙酸乙酯、乙酸丙酯、乙酸丁酯等酯系有机溶剂，丙酮、甲基乙基酮、甲基丁基酮等酮系有机溶剂等。这些溶剂可以单独或混合2种以上来使用。
其中，从聚氨基甲酸酯多元醇(A)的溶解性的观点出发，特别优选乙酸乙酯、乙酸丙酯、乙酸丁酯、甲苯、甲基环己烷、甲基乙基酮，更优选甲苯、甲基乙基酮。
相对于包含(A)、(B)和(C)成分的金属箔与树脂膜的层压用粘接剂100质量份，溶剂(C)的含量优选为40～95质量份，更优选为50～95质量份，进一步优选为80～90质量份。如果为40质量份以上，则涂布本发明的金属箔与树脂膜的层压用粘接剂时的操作性变得良好；如果为95质量份以下，则将本发明的金属箔与树脂膜的层压用粘接剂进行涂布、固化而得到的叠层体的厚度的控制性变得良好。
<其他成分>
本发明的金属箔与树脂膜的层压用粘接剂可以根据需要含有反应促进剂、增粘剂、增塑剂等添加剂。反应促进剂是用于促进聚氨基甲酸酯多元醇(A)和多异氰酸酯(B)的反应的，可举出例如，作为有机锡化合物的二月桂酸二辛基锡、二乙酸二辛基锡，作为叔胺的2,4,6-三(二甲基氨基甲基)苯酚、二甲基苯胺、二甲基对甲苯胺、N,N-二(β-羟基乙基)-对甲苯胺等。这些反应促进剂可以单独使用或并用2种以上。
作为前述增粘剂，没有特别限定。例如，在天然系中，可举出聚萜烯系树脂、松香系树脂等；在石油系中，可举出由石脑油的分解油馏分得到的脂肪族(C5)系树脂、芳香族(C9)系树脂、共聚(C5/C9)系树脂、脂环族系树脂等。此外，可举出将这些树脂的双键部分氢化而得的氢化树脂。该增粘剂可以仅使用1种，也可以并用2种以上。作为前述增塑剂，没有特别限定，可举出例如，聚异戊二烯、聚丁烯等液状橡胶、加工油等。
此外，只要在不损害本发明的效果的范围，可以含有酸改性聚烯烃树脂等热塑性树脂、热塑性弹性体。作为可以配合的热塑性树脂和热塑性弹性体，可举出例如，乙烯-乙酸乙烯酯共聚树脂、乙烯-丙烯酸乙酯共聚树脂、SEBS(苯乙烯-乙烯-丁烯-苯乙烯)、SEPS(苯乙烯-乙烯-丙烯-苯乙烯)等。
(叠层体)
本发明的叠层体是使金属箔与树脂膜经由由本发明的金属箔与树脂膜的层压用粘接剂(以下有时简单称为“本发明的层压用粘接剂”。)得到的粘接剂层进行接合而得的。此外，在本发明的叠层体中，只要包含使金属箔与树脂膜经由由本发明的层压用粘接剂得到的粘接剂层进行接合而得的层，则还可以包含金属箔彼此和/或树脂膜彼此经由由本发明的层压用粘接剂得到的粘接剂层进行接合而得的层。该接合方法可以使用热层压方式、干式层压方式等公知的方法。所谓热层压方式，是指通过使不包含溶剂(C)的本发明的层压用粘接剂在与粘接剂层相接的那层表面进行加热熔融、或与和粘接剂层相接的那层一起进行加热挤出，来使粘接剂介于叠层体的层间，从而形成粘接剂层的方式。此外，所谓干式层压方式，是指通过将包含溶剂(C)的本发明的层压用粘接剂涂布于与粘接剂层相接的那层的表面，使其干燥后，与另一层叠加并进行压接，来使粘接剂介于叠层体的层间，从而形成粘接剂层的方式。
对本发明的叠层体的用途没有特别限定，但作为有用的用途，可举出包装用途。作为包装在叠层体中的内容物，可举出含有酸、碱、有机溶剂等的液状物，例如，油灰(稠油灰、稀油灰等)、涂料(油性涂料等)、漆(清漆等)、汽车用复合物等的溶剂系的物质。此外，该叠层体还适合包装锂离子电池的电解液，因此可以作为电池外包装用包装材料使用，且是优选的。在作为电池外包装用包装材料使用的情况下，优选的是：金属箔是铝箔，且树脂膜包含热熔接性树脂膜，此外在铝箔的外侧设置由耐热性树脂膜构成的外层。
(电池外包装用包装材料)
本发明的电池外包装用包装材料是在本发明的叠层体的金属箔的外侧设置包含耐热性树脂膜的外层而成的。此外，根据需要，为了提高机械强度、耐电解液性等特性，可以制成附加了第1中间树脂层或/和第2中间树脂层等的构成。作为优选的形态，具体而言可以制成以下那样的构成。需要说明的是，粘接剂层意思是“由本发明的层压用粘接剂得到的粘接剂层”，将金属箔层以铝箔层的形式例示。
(1)外层/铝箔层/粘接剂层/树脂膜层
(2)外层/第1中间树脂层/铝箔层/粘接剂层/树脂膜层
(3)外层/铝箔层/第2中间树脂层/粘接剂层/树脂膜层
(4)外层/第1中间树脂层/铝箔层/第2中间树脂层/粘接剂层/树脂膜层
(5)涂布层/外层/铝箔层/粘接剂层/树脂膜层
(6)涂布层/外层/第1中间树脂层/铝箔层/粘接剂层/树脂膜层
(7)涂布层/外层/铝箔层/第2中间树脂层/粘接剂层/树脂膜层
(8)涂布层/外层/第1中间树脂层/铝箔层/第2中间树脂层/粘接剂层/树脂膜层
上述中，作为第1中间树脂层，出于提高电池外包装用包装材料的机械强度的目的，使用聚酰胺树脂、聚酯树脂或聚乙烯树脂等。作为第2中间树脂层，主要出于提高耐电解液性的目的，与第1中间树脂层同样，使用聚酰胺树脂、聚酯树脂或聚乙烯树脂、聚丙烯等热粘接性挤出树脂。树脂膜层可以使用单层的树脂膜、多层的树脂膜(通过2层的共挤出或3层的共挤出等进行制造)。此外，第2中间树脂层也可以使用单层的树脂膜、多层的共挤出树脂膜。对第1中间树脂层和第2中间树脂层的厚度没有特别限定，但在设置它们的情况下，通常为0.1～30μm左右。
(外层的耐热性树脂膜)
在外层使用的树脂膜是耐热性、成型性、绝缘性等优异的树脂膜。一般使用聚酰胺(尼龙)树脂或聚酯树脂的拉伸膜。该外层膜的厚度为9～50μm左右，如果小于9μm，则在进行包装材料的成型时，拉伸膜的伸长不足，铝箔发生颈缩，容易发生成型不良。另一方面，在超过50μm的情况下，成型性的效果并不显著提高，反而只是使体积能量密度下降，同时成本上升而已。外层膜的厚度更优选为10～40μm左右，进一步优选为20～30μm。
作为该在外层使用的膜，在将拉伸膜的拉伸方向记为0°的情况下，以0°、45°、90°这3个方向分别成为拉伸方向的方式将膜切成规定的大小，进行拉伸试验，此时使用其抗拉强度为150N/mm2以上、优选为200N/mm2以上、进一步优选为250N/mm2以上，且这3个方向的拉伸引起的伸长为80％以上、优选为100％以上、进一步优选为120％以上这样的膜，在获得更尖锐的形状这点上是优选的。通过使抗拉强度为150N/mm2以上、或拉伸引起的伸长为80％以上，可以充分发挥上述效果。需要说明的是，抗拉强度和拉伸引起的伸长的值是在膜的拉伸试验(试验片的长度150mm×宽度15mm×厚度9～50μm，拉伸速度100mm/min)中直到断裂的值。试验片是分别沿着3个方向切成的。
(金属箔)
金属箔发挥对水蒸气等的阻隔性的作用，作为材质，一般使用纯铝系或铝-铁系合金的O材(软质材)，且是优选的。作为铝箔的厚度，为了确保加工性以及确保防止氧气、水分浸入包装内的屏障性，优选为10～100μm左右。在铝箔的厚度小于10μm的情况下，在成型时可能出现铝箔的断裂、或者产生针孔，从而可能浸入氧气、水分。另一方面，在铝箔的厚度超过100μm的情况下，成型时断裂的改善效果、针孔产生防止效果并不显著提高，只是包装材料的总厚度变厚、质量增加、体积能量密度下降而已。铝箔一般使用厚30～50μm左右的铝箔，优选使用厚40～50μm的铝箔。需要说明的是，为了提高与树脂膜的粘接性、耐蚀性，优选对铝箔预先进行硅烷偶联剂、钛偶联剂等底涂层处理，铬酸盐处理等化学处理。
(树脂膜)
作为树脂膜，优选聚丙烯、聚乙烯、马来酸改性聚丙烯、乙烯-丙烯酸酯共聚物或离聚物树脂等热熔接性树脂膜。这些树脂具有热封性，是发挥提高针对腐蚀性强的锂二次电池的电解液等的耐化学品性的作用的树脂。这些树脂膜的膜厚优选为9～100μm，更优选为20～80μm，最优选为40～80μm。如果树脂膜的厚度为9μm以上，则可获得充分的热封强度，对电解液等的耐蚀性变得良好。如果树脂膜的厚度为100μm以下，则电池外包装用包装材料的强度充分，且成型性变得良好。
(涂层)
本发明的电池外包装用包装材料可以在外层上设置涂层。作为涂层的形成法，有涂布气体阻隔性聚合物的方法、蒸镀铝金属、氧化硅/氧化铝等无机氧化物来涂布金属和无机物的薄膜的方法等。通过设置涂层，可获得水蒸气和其他气体阻隔性更优异的叠层体。
(电池外壳)
本发明的电池外壳是通过将本发明的电池外包装用包装材料成型而得的。本发明的电池外包装用包装材料的耐电解液性、耐热性、水蒸气和其他气体阻隔性优异，可适合作为二次电池、特别是锂离子电池用的电池外壳使用。此外，本发明的电池外包装用包装材料的成型性非常良好，因此可以通过按照公知的方法进行成型而简便地获得本发明的电池外壳。对成型的方法不特别限定，但如果通过深拉成型或拉伸成型进行成型，则能够制作复杂的形状、尺寸精度高的电池外壳。
实施例
以下通过实施例和比较例来更具体地说明本发明，但本发明不受这些实施例任何限制。
(合成例1)
向带有搅拌机、水分离器的反应容器中加入作为氢化二聚二元醇的“Sovermol908”(BASF社制)220.00g、作为氢化二聚酸的“EMPOL1008”(BASF社制)230.00g、作为催化剂的二月桂酸丁基锡“KS-1260”(堺化学工业制)0.10g，在约240℃下，一边从常压下开始使缩合水流出一边进行减压，同时进行脱水酯化反应，从而获得聚酯多元醇(以下记为聚酯多元醇(1)。)。
(合成例2)
向具备搅拌装置、温度计和冷凝器的反应容器中投入双酚A(新日铁化学制，化合物名2,2-双(4-羟基苯基)丙烷)23.29g、“KS-1260”(堺化学工业制，二月桂酸二丁基锡)0.01g、以及“デスモジュールI”(バイエル社制异佛尔酮二异氰酸酯)34.02g、甲基乙基酮113.13g，一边进行搅拌一边使用油浴升温至85～90℃。然后，一边进行2.5小时搅拌一边持续反应，从而获得聚氨基甲酸酯多异氰酸酯(以下记为聚氨基甲酸酯多异氰酸酯(2)。)的甲基乙基酮溶液。
(合成例3)
使用双酚F(本州化学工业制)20g代替双酚A，除此以外，与合成例2同样操作，从而获得聚氨基甲酸酯多异氰酸酯(以下记为聚氨基甲酸酯多异氰酸酯(3)。)的甲基乙基酮溶液。
(合成例4)
向具备搅拌装置、温度计和冷凝器的反应容器中投入聚酯多元醇(1)112.50g、“TCDアルコールDM”(オクセア社制，三环癸烷二甲醇)12.50g、氢醌单甲基醚(和光纯药工业制)0.04g、“KS-1260”(堺化学工业制，二月桂酸二丁基锡)0.03g、以及“デスモジュールW”(バイエル社制，亚甲基双(4-环己基异氰酸酯))28.97g、甲苯70g，一边进行搅拌一边使用油浴升温至85～90℃。然后，一边进行2.5小时搅拌一边持续反应。然后，测定红外吸收光谱，确认异氰酸酯基的吸收消失，结束反应，进一步投入甲苯636.5g，进行搅拌溶解，从而获得聚氨基甲酸酯多元醇(以下记为聚氨基甲酸酯多元醇(4)。)的甲苯溶液(固体成分浓度为18质量％)。
(合成例5～10、比较合成例11～13)
通过与合成例3同样的方法，以如表2所示的成分、量来进行合成，从而获得聚氨基甲酸酯多元醇(4)～(13)的甲苯溶液或甲苯与甲基乙基酮的混合溶剂溶液(固体成分浓度为18质量％)。
在表2中，GI-1000、GI-2000是日本曹达制氢化聚丁二烯多元醇，G-1000是日本曹达制聚丁二烯多元醇，14BG是三菱化学制1,4-丁二醇。
关于合成例1～10和比较合成例11～13，示于表1、表2。
(实施例1)
向由合成例4得到的聚氨基甲酸酯多元醇(4)的甲苯溶液33.33g(固体成分6.00g，甲苯27.33g)中添加“デュラネートTKA-100”(旭化成ケミカルズ株式会社制，六亚甲基二异氰酸酯异氰脲酸酯化物)0.34g、甲苯15.08g，调制成金属箔与树脂膜的层压用粘接剂1。接着，使用该层压用粘接剂1，如下操作，通过干式层压方式制造具有外层/外层用粘接剂/铝箔层/层压用粘接剂1/树脂膜的结构的电池外包装用包装材料。
外层：拉伸聚酰胺膜(厚度25μm)
外层用粘接剂：氨基甲酸酯系干式层压用粘接剂(东洋モートン株式会社制：AD502/CAT10，涂布量3g/m2(涂布时))
铝箔层：铝-铁系合金的铝箔(AA标准8079-O材，厚度40μm)
层压用粘接剂1：上述金属箔与树脂膜的层压用粘接剂1(涂布量：干燥后的厚度为2μm)
树脂膜：未拉伸聚丙烯膜(厚度30μm)
(实施例2～7、比较例1～5)
通过与实施例1同样的方法，以如表3所示的成分、量来进行金属箔与树脂膜的层压用粘接剂2～12的调制，使用各个金属箔与树脂膜的层压用粘接剂来制造电池外包装用包装材料。
在表3中，酸改性聚丙烯是利用马来酸酐和丙烯酸辛酯进行了改性的酸改性聚丙烯(酸值20mg/KOH)，ミリオネートMR-200是日本聚氨基甲酸酯制聚二苯基甲烷二异氰酸酯。
<剥离强度>
关于所得的电池外壳用包装材料，测定常态T字剥离强度、电解液溶剂浸渍后的T字剥离强度和85℃气氛下的T字剥离强度。测定的条件、方法如下述的(1)～(3)所示。各试验以n＝2进行，取其平均值。此外，将结果示于表4中(单位均为N/15mm)。
(1)常态T字剥离强度
使用长度150mm×宽度15mm的试验片和Autograph AG-X(精密万能试验机，株式会社岛津制作所制)，在23℃×50％RH气氛下，以剥离速度100mm/min使其剥离，测定铝箔层与未拉伸聚丙烯膜层间的180°剥离强度。
(2)电解液溶剂浸渍后的T字剥离强度
将长度150mm×宽度15mm的试验片浸渍于电解液溶剂(碳酸亚乙酯/碳酸二乙酯，质量比50/50)中，在85℃气氛下放置1日后取出，使用该试验片，与上述(1)同样操作来测定铝箔层与未拉伸聚丙烯膜层间的180°剥离强度。
(3)85℃气氛下的T字剥离强度
使用长度150mm×宽度15mm的试验片和Autograph AG-X(株式会社岛津制作所制)，放置在85℃气氛下，在使试验片的温度变为85℃后，以剥离速度100mm/min使其剥离，测定铝箔层与未拉伸聚丙烯膜层间的180°剥离强度。
[表1]
表1
[表2]
[表3]
[表4]
表4
(单位N/15mm)
由表4的结果可知，本发明的金属箔与树脂膜的层压用粘接剂(实施例1～7)在常态T字剥离强度、电解液溶剂浸渍后的T字剥离强度和85℃气氛下的T字剥离强度中的任一项均优异。
与此相对，在使用不包含(b)成分作为聚氨基甲酸酯多元醇的原料的金属箔与树脂膜的层压用粘接剂的情况下(比较例1～4)，常态T字剥离强度、电解液溶剂浸渍后的T字剥离强度和85℃气氛下的T字剥离强度中的任一项均不充分，在使用以改性聚烯烃为主剂的金属箔与树脂膜的层压用粘接剂的情况下(比较例5)，可知85℃气氛下的T字剥离强度不充分。
产业上的可利用性
本发明的金属箔与树脂膜层压用金属箔与树脂膜的层压用粘接剂即使在电解液浸渍后、高温下也具有优异的粘接力，尤其适合铝箔与热熔接性树脂膜的接合用。此外，本发明的叠层体的耐热性、耐电解液性优异，因此可适用于在锂离子电池等二次电池的制作中使用的电池外包装用包装材料，通过将该叠层体进行成型，可以制造耐热性、耐电解液性优异的电池外壳。而且，通过使用该电池外壳，从而寿命长的安全的二次电池的制造变得可能。

Claims (15)

1.一种聚氨基甲酸酯多元醇，是用于聚氨基甲酸酯系粘接剂的多元醇，其是将含有链状聚烯烃多元醇a1和/或聚酯多元醇a2、含有羟基的烃化合物b、以及多异氰酸酯c的成分加聚而获得的，所述聚酯多元醇a2具有源自氢化二聚酸的结构单元和源自氢化二聚二元醇的结构单元，所述含有羟基的烃化合物b同时具有饱和或不饱和的环式烃结构和2个以上羟基。
2.一种金属箔与树脂膜的层压用粘接剂，具有聚氨基甲酸酯多元醇A、和饱和脂肪族和/或饱和脂环式多异氰酸酯B，所述聚氨基甲酸酯多元醇A是将含有链状聚烯烃多元醇a1和/或聚酯多元醇a2、含有羟基的烃化合物b、以及多异氰酸酯c的成分加聚而获得的，所述聚酯多元醇a2具有源自氢化二聚酸的结构单元和源自氢化二聚二元醇的结构单元，所述含有羟基的烃化合物b同时具有饱和或不饱和的环式烃结构和2个以上羟基。
3.根据权利要求2所述的金属箔与树脂膜的层压用粘接剂，所述含有羟基的烃化合物b是含有具有交联结构的饱和脂环结构的多元醇。
4.根据权利要求2或3所述的金属箔与树脂膜的层压用粘接剂，所述含有羟基的烃化合物b是双酚化合物。
5.根据权利要求2～4中任一项所述的金属箔与树脂膜的层压用粘接剂，所述多异氰酸酯c是饱和脂环式二异氰酸酯。
6.根据权利要求2～5中任一项所述的金属箔与树脂膜的层压用粘接剂，所述链状聚烯烃多元醇a1是实质上不含有不饱和烃结构的聚烯烃多元醇。
7.根据权利要求2～6中任一项所述的金属箔与树脂膜的层压用粘接剂，相对于a1成分和a2成分的总量100质量份，b成分为5～100质量份，相对于a1成分、a2成分以及b成分中包含的羟基数，c成分中包含的异氰酸酯基数的比率为0.5～1.3。
8.根据权利要求2～7中任一项所述的金属箔与树脂膜的层压用粘接剂，相对于所述聚氨基甲酸酯多元醇A中包含的羟基数，多异氰酸酯B中包含的异氰酸酯基数的比率为1～15。
9.根据权利要求2～8中任一项所述的金属箔与树脂膜的层压用粘接剂，其还含有溶剂C。
10.一种叠层体，是金属箔与树脂膜经由粘接剂层进行叠层而得的，所述粘接剂层是由权利要求2～9中任一项所述的金属箔与树脂膜的层压用粘接剂得到的。
11.根据权利要求10所述的叠层体，所述金属箔是铝箔，所述树脂膜含有热熔接性树脂膜。
12.根据权利要求10或11所述的叠层体，所述金属箔的厚度为10～100μm，所述树脂膜的厚度为9～100μm。
13.一种电池外包装用包装材料，其是使用权利要求10～12中任一项所述的叠层体而获得的。
14.一种电池外壳，其是使用权利要求13所述的电池外包装用包装材料而获得的。
15.一种电池外壳的制造方法，对权利要求13所述的电池外包装用包装材料进行深拉成型或拉伸成型。
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