CN215904055U - 成型用包装材料及成型壳体 - Google Patents
成型用包装材料及成型壳体 Download PDFInfo
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- CN215904055U CN215904055U CN202120032478.8U CN202120032478U CN215904055U CN 215904055 U CN215904055 U CN 215904055U CN 202120032478 U CN202120032478 U CN 202120032478U CN 215904055 U CN215904055 U CN 215904055U
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4205—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups
- C08G18/4208—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups
- C08G18/4211—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups derived from aromatic dicarboxylic acids and dialcohols
- C08G18/4216—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups derived from aromatic dicarboxylic acids and dialcohols from mixtures or combinations of aromatic dicarboxylic acids and aliphatic dicarboxylic acids and dialcohols
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
- B32B15/085—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyolefins
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
- B32B15/088—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyamides
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Abstract
本实用新型涉及成型用包装材料及成型壳体,防止具有着色层的成型用包装材料的层间剥离。成型用包装材料(1),其包含作为外侧层的耐热性树脂层(2)、作为内侧层的热塑性树脂层(3)、配设于这两层之间的金属箔层(4)、配设于上述金属箔层(4)与耐热性树脂层(2)之间的第一粘接剂层(5)、以及配设于上述金属箔层(4)与热塑性树脂层(3)之间的第二粘接剂层(6),上述第一粘接剂层(5)由含有着色颜料和粘接剂的着色粘接剂组合物形成,上述着色粘接剂组合物相对于固态成分而言包含2质量%以上且小于5质量%的着色颜料,上述第一粘接剂层(5)是涂布5g/m2~10g/m2的上述着色粘接剂组合物而成的,上述第一粘接剂层(5)含有0.25g/m2~0.49g/m2的着色颜料。
Description
技术领域
本发明涉及适合作为例如笔记本电脑用、手机用、车载用、定置型二次电池(锂离子二次电池)的壳体使用、以及适合作为食品的包装材料、医药品的包装材料使用的成型用包装材料。
背景技术
为了与作为装配对象的电气设备等设备的外观和色彩统一,通常要求对锂离子二次电池等电池进行着色。例如,为了赋予厚重感、高级感,通常将设备着色为黑色,这种情况下,通常将电池也着色为黑色。
这种包装材料通常为在金属箔的两面层叠有树脂层而成的层叠体,为了将电池着色为黑色等,有下述方法:将用于包装材料的树脂层着色;在基材树脂层之下设置印刷层;将基材树脂层与遮蔽用金属层之间的粘接剂层着色;当基材树脂层由多层构成时将层间的粘接剂层着色;等等。
例如,有在电池用包装材料的基材层(树脂层)、粘接剂层、金属箔层中的任意层中设置包含识别标志的层的例子,有将设置于基材层的下层的印刷层、基材层的粘接剂层整体着色而能够使包装材料整体着色的例子(参见专利文献1、2)。
另外,还有为了促进电池用包装材料的放热而在金属箔层与外层膜之间具有黑体材料层的例子(参见专利文献3)。
现有技术文献
专利文献
专利文献1:国际公开WO2011/016506A1号公报
专利文献2:日本特开2011-054563号公报
专利文献3:日本特开2011-096552号公报
发明内容
发明要解决的课题
在将上述包装材料着色为黑色的情况下,通常用包含炭黑等颜料的印刷油墨来设置印刷层。
但是,在为了将电池着色为黑色而在构成成型用包装材料的外侧树脂层的内表面设置包含炭黑作为颜料的印刷层的情况下,存在以下所述的问题。
即,在通过深拉深成型、鼓凸成型将上述黑色包装材料成型为容器 (壳体)形状时,存在含炭黑的印刷层会发生局部破裂、剥离,基底层 (不为黑色)外露,从而均匀的黑色着色受损的问题。
当在封入电极、电解液后进行黑色包装材料密封时、经黑色包装材料包装的电池在高温多湿等略严酷的环境下被使用时,也会发生这样的印刷层的局部剥离。
另外,不仅使用炭黑的黑色包装材料,用其他颜料着色的包装材料也会发生同样的问题。
而且,近年来,锂离子二次电池等电池的高容量化正在推进,对包装材料还逐渐地要求高成型性、耐热性、耐湿热性等特性。
用于解决课题的手段
本发明是鉴于上述技术背景而做出的,目的在于提供在成型时及密封时、以及即使在高温多湿等略严酷的环境下使用时也均没有着色层局部破裂、剥离的成型用包装材料。
即,本发明具有[1]~[10]记载的构成。
[1]成型用包装材料,其包含作为外侧层的耐热性树脂层、作为内侧层的热塑性树脂层、配设于这两层之间的金属箔层、配设于上述金属箔层与耐热性树脂层之间的第一粘接剂层、以及配设于上述金属箔层与热塑性树脂层之间的第二粘接剂层,所述成型用包装材料的特征在于,
上述第一粘接剂层由含有着色颜料和粘接剂的着色粘接剂组合物形成,上述着色粘接剂组合物相对于固态成分而言包含2质量%以上且小于5质量%的着色颜料,上述第一粘接剂层是涂布5g/m2~10g/m2的上述着色粘接剂组合物而成的,上述第一粘接剂层含有0.25g/m2~0.49g/m2的着色颜料。
[2]根据前项1所述的成型用包装材料,其特征在于,上述着色粘接剂组合物中的粘接剂包含二液固化型聚酯氨基甲酸酯树脂,所述二液固化型聚酯氨基甲酸酯树脂包含作为主剂的聚酯树脂和作为固化剂的多官能异氰酸酯化合物,上述聚酯树脂的数均分子量(Mn)为8,000~ 25,000、重均分子量(Mw)为15,000~50,000,它们的比率(Mw/Mn) 为1.3~2.5,上述多官能异氰酸酯化合物包含50摩尔%以上的芳香族系异氰酸酯。
[3]根据前项2所述的成型用包装材料,其中,在上述二液固化型聚酯氨基甲酸酯树脂中,作为主剂的上述聚酯树脂以二羧酸及二醇为原料,
上述二羧酸包含亚甲基链的亚甲基数为偶数的脂肪族二羧酸和芳香族二羧酸,芳香族二羧酸相对于它们的合计量的含有率为40~80摩尔%。
[4]根据前项2所述的成型用包装材料,其中,上述二液固化型聚酯氨基甲酸酯树脂的固化膜基于拉伸试验(JIS K7162)的杨氏模量为 70~400MPa。
[5]根据前项1所述的成型用包装材料,其中,上述第一粘接剂层的膜厚为4.5μm~10μm。
[6]根据前项1所述的成型用包装材料,其中,在上述金属箔层的至少一个面上具有化学转化被膜。
[7]根据前项1所述的成型用包装材料,其中,上述耐热性树脂层由热水收缩率为2%~20%的拉伸膜形成。
[8]根据前项1所述的成型用包装材料,其特征在于,在上述耐热性树脂层的外表面上具有哑光涂层。
[9]成型壳体,其特征在于,其是将前项1~8中任一项所述的成型用包装材料进行深拉深成型或鼓凸成型而成的。
[10]根据前项9所述的成型壳体,其作为电池壳体使用。
发明效果
就上述[1]所述的成型用包装材料而言,通过第一粘接剂层对成型用包装材料的外表面侧赋予颜色。着色颜料通过着色粘接剂组合物中的浓度、着色粘接剂组合物的涂布量及第一粘接剂层中的着色颜料的含量而被规定,因此可维持均匀、充分的着色且不会发生由着色颜料引起的第一粘接剂层变脆,不会使耐热性树脂层与金属箔层的接合力降低。因此,在对包装材料进行深拉深成型、鼓凸成型等成型时,在为了封闭而对包装材料进行密封时,耐热性树脂层不会发生剥离。另外,即使在高温多湿等略严酷的环境下使用时,耐热性树脂层也不会剥离。
就上述[2]所述的成型用包装材料而言,通过使用包含特定的二液固化型聚酯氨基甲酸酯树脂的粘接剂,可得到适合于粘接剂涂膜的强度和伸长率、优异的耐热性,而且能够保持粘接剂涂布适性(分子量分布宽) 和性能(分子量分布窄)的平衡。
就上述[3]、[4]所述的成型用包装材料而言,防止耐热性树脂层与金属箔层剥离的效果特别优异。
就上述[5]所述的成型用包装材料而言,第一粘接剂层的膜厚被设为 4.5μm~10μm,因此具有充分的掩蔽金属箔层的金属光泽的效果,并且可抑制卷曲的发生,成型加工时的处理性良好。
上述[6]所述的成型用包装材料中,金属箔层的表面具有化学转化被膜,因此可提供在防止粘接剂剥离的同时还可防止金属箔腐蚀的、耐腐蚀性高的成型用包装材料。
就上述[7]所述的成型用包装材料而言,热水收缩率被设为2%~ 20%,从而可以得到高成型性。
就上述[8]所述的成型用包装材料而言,在耐热性树脂层的外表面形成有哑光涂层,因此成型性进一步优异。
就上述[9]所述的成型壳体而言,可提供无论是在密封时还是在高温多湿等略严酷的环境下使用时、耐热性树脂层也均不剥离的成型壳体。
就上述[10]所述的成型壳体而言,可提供无论是在密封时还是在高温多湿等略严酷的环境下使用时、耐热性树脂层也不会发生局部破裂、剥离的电池壳体。
附图说明
图1为示出本发明涉及的成型用包装材料的一实施方式的剖视图。
图2为二液固化型聚酯氨基甲酸酯树脂粘接剂的固化膜的S-S曲线图。
图3为示出本发明涉及的成型用包装材料的另一实施方式的剖视图。
图4为示出本发明涉及的成型用包装材料的又一实施方式的剖视图。
图5为试验材料的立体图。
附图标记说明
1、10、20…成型用包装材料
2…耐热性树脂层(外侧层)
3…热塑性树脂层(内侧层)
4…金属箔层(铝箔)
5…第一粘接剂层(着色粘接剂组合物)
6…第二粘接剂层
11a、11b…化学转化被膜
21…哑光涂层
具体实施方式
图1为本发明的一实施方式,示出具有基本的层叠结构的电池壳体成型用包装材料1。该成型用包装材料1作为锂离子2次电池壳体的材料使用。即,上述成型用包装材料1为供于深拉深成型等成型、作为2 次电池壳体使用的材料。
上述电池壳体包装材料1包含下述构成:耐热性树脂层(外侧层)2 介由第一粘接剂层5而层叠一体化于金属箔层4的上表面,并且热塑性树脂层(内侧层)3介由第二粘接剂层6层叠一体化于上述金属箔层4 的下表面。
以下对各层进行详细说明。
(耐热性树脂层)
作为上述耐热性树脂层(外侧层)2,没有特别限定,可列举例如聚酰胺膜、聚酯膜等,优选使用它们的拉伸膜。其中,作为上述耐热性树脂层2,从成型性及强度的观点出发,特别优选使用双轴拉伸聚酰胺膜、双轴拉伸聚对苯二甲酸丁二醇酯(PBT)膜、双轴拉伸聚对苯二甲酸乙二醇酯(PET)膜或双轴拉伸聚萘二甲酸乙二醇酯(PEN)膜。作为上述聚酰胺膜,没有特别限定,可列举例如6-尼龙膜、6,6-尼龙膜、MXD 尼龙膜等。需要说明的是,上述耐热性树脂层2可以由单层形成,或者,例如也可以由包含PET膜/聚酰胺膜的多层形成。进一步地,若考虑到充分呈现出粘接剂的着色效果,则优选这些膜为无色透明。
上述耐热性树脂层2的厚度优选为9μm~50μm。使用聚酯膜时,厚度优选为9μm~50μm,使用聚酰胺膜时,厚度优选为10μm~50μm。通过设为上述优选下限值以上,可以确保作为包装材料的充分的强度,通过设为上述优选上限值以下,可以减小鼓凸成型时、拉深成型时的应力、提高成型性。
此外,上述耐热性树脂层2优选热水收缩率为2%~20%的拉伸膜。
上述热水收缩率表示在将耐热性树脂层2的试验片(10cm×10cm) 在95℃的热水中浸渍30分钟时、浸渍前后的试验片的拉伸方向上的尺寸变化率,可由下式求出。
热水收缩率(%)={(X-Y)/X}×100
X:浸渍处理前的拉伸方向的尺寸
Y:浸渍处理后的拉伸方向的尺寸。
需要说明的是,采用双轴拉伸膜时,其热水收缩率为两个拉伸方向上的尺寸变化率的平均值。
上述热水收缩率小于2%时,进行深拉深成型、鼓凸成型等成型时,难以得到高成型性。另一方面,若热水收缩率超过20%,则进行深拉深成型、鼓凸成型等成型后,在高温多湿等略严酷的环境下使用时耐热性树脂层2容易从第一粘接剂层5剥离。其中,作为上述耐热性树脂层2,优选使用热水收缩率为2.5~10%的拉伸膜。进一步地,更优选使用热水收缩率为3.0%~6.0%的拉伸膜,进一步地,特别优选使用热水收缩率为 3.5%~5.0%的拉伸膜。
(热塑性树脂层)
就上述热塑性树脂层(内侧层)3而言,针对锂离子二次电池等中使用的腐蚀性强的电解液等具备优异的耐化学药品性,并且起到对包装材料赋予热封性的作用。
作为上述热塑性树脂层3,没有特别限定,优选为热塑性树脂未拉伸膜层。上述热塑性树脂层3没有特别限定,从耐化学药品性及热封性的观点出发,优选由下述未拉伸膜构成,所述未拉伸膜由选自由聚乙烯、聚丙烯、烯烃系共聚物、它们的酸改性物及离聚物组成的组中的至少1 种的热塑性树脂形成。
上述热塑性树脂层3的厚度优选设为20μm~100μm。通过设为20μm 以上,可以充分防止针孔的产生,通过设为100μm以下,可以降低树脂使用量,能实现成本的降低。其中,上述热塑性树脂层3的厚度特别优选设为30μm~50μm。需要说明的是,上述热塑性树脂层3可以为单层,也可以为多层。作为多层膜,可例示在嵌段聚丙烯膜的两面层叠有无规聚丙烯膜的三层膜。
(金属箔层)
上述金属箔层4起到下述作用:阻止氧、水分侵入成型用包装材料 1,赋予气体阻隔性。作为上述金属箔层4,没有特别限定,可列举例如铝箔、铜箔、不锈钢箔等,通常使用铝箔。上述金属箔层4的厚度优选为20μm~100μm。通过为20μm以上,在制造金属箔时能够防止压延时产生针孔,通过为100μm以下,能减小鼓凸成型时、拉深成型时的应力,能提高成型性。
(第一粘接剂层)
上述第一粘接剂层5为承担金属箔层4与作为外侧层的耐热性树脂层2的接合、并且对成型用包装材料1的外表面侧赋予颜色(包括无彩色)而掩蔽金属箔层4的层。
上述第一粘接剂层5由含有着色颜料和粘接剂的着色粘接剂组合物形成。本发明中规定上述着色粘接剂组合物中的着色颜料浓度及着色粘接剂组合物的涂布量,并且规定由它们所确定的第一粘接剂层5中的着色颜料的含量范围。通过以这3个基准规定着色颜料,从而能够得到由着色颜料带来的视觉效果,并且可防止固化后的第一粘接剂层5变脆。即,即使是着色颜料浓度低的着色粘接剂组合物,若涂布量足够则也能得到由着色颜料带来的视觉效果,由于着色粘接剂组合物中的着色颜料浓度低,因此固化后的第一粘接剂层5不会变脆,不会降低耐热性树脂层2与金属箔层4的接合力。因此,在对包装材料进行深拉深成型、鼓凸成型等成型时、为了封闭而对包装材料进行密封时,耐热性树脂层也不会剥离。另外,在高温多湿等稍严酷的环境下使用时,耐热性树脂层2也不会剥离。
上述着色粘接剂组合物包含该着色粘接剂组合物的固态成分的2质量%以上且小于5质量%的着色颜料。上述着色粘接剂组合物中的着色颜料的含有率小于2质量%则视觉效果差,为5质量%以上则第一粘接剂层5容易变硬变脆,与金属箔层4的粘接力下降,耐热性树脂层2变得容易剥离。上述着色颜料的优选含有率为2.5质量%~4.9质量%。
上述第一粘接剂层5是涂布5g/m2~10g/m2的着色粘接剂组合物而成的。若上述着色粘接组合物的涂布量小于5g/m2,则掩蔽金属箔层4 的金属光泽的效果差,由着色颜料带来的视觉效果变弱。另一方面,若上述着色粘接组合物的涂布量超过10g/m2,则加工性下降,成本增加。上述着色粘接组合物的优选涂布量为6g/m2~10g/m2。
另外,上述第一粘接剂层5的膜厚优选为4.5μm~10μm的范围。膜厚小于4.5μm时,掩蔽金属箔层4的金属光泽的效果小。另一方面,若膜厚超过10μm,则有可能制作成型用包装材料1时干燥时间变长而制造效率下降、或者制作的成型用包装材料1产生卷曲而成型加工时的处理性下降。卷曲是指下述现象:由于成型用包装材料1的制作工序中的熟化处理,外侧层(耐热性树脂层2)与内侧层(热塑性树脂层3)中使用的材料的收缩率差异导致成型用包装材料1的端缘上卷。若成型用包装材料1产生卷曲,则在对电池壳体、容器主体、盖材进行成型加工时变得难以处理。因此,通过将第一粘接剂层5的膜厚设为4.5μm~10μm的范围,能够成为可充分获得金属箔层4的金属光泽的掩蔽效果、且可抑制卷曲的产生从而处理性良好的成型用包装材料1。上述第一粘接剂层5 的特别优选的膜厚为5μm~7μm。
上述第一粘接剂层含有0.25g/m2~0.49g/m2的着色颜料。上述第一粘接剂层5中的着色颜料的含量小于0.25g/m2时,掩蔽金属箔层4的金属光泽的效果小,由着色颜料带来的视觉效果变弱,在0.49g/m2时可得到充分的视觉效果,因此超过0.49g/m2的大量着色颜料会造成浪费。上述第一粘接剂层5中,着色颜料的优选含量为0.25g/m2~0.3g/m2。
上述着色粘接剂组合物中,着色颜料的种类没有限制,可使用偶氮系颜料、酞菁系颜料、稠合多环系颜料、无机系颜料等。另外,作为黑色颜料,可推荐炭黑。另外,着色颜料优选使用平均粒径为0.1μm~5μm 的颜料,特别优选的平均粒径为0.5μm~2.5μm。在进行颜料分散时,优选使用颜料分散机来进行颜料分散,在进行颜料分散时,还可以使用表面活性剂等颜料分散剂。
上述着色粘接剂组合物中粘接剂的种类没有限定,但条件是粘接强度及成型性优异、能抑制深成型时的层间剥离。作为满足上述条件的粘接剂,可推荐包含下述二液固化型聚酯氨基甲酸酯树脂的粘接剂,所述二液固化型聚酯氨基甲酸酯树脂包含作为主剂的聚酯树脂和作为固化剂的多官能异氰酸酯化合物。
上述聚酯树脂是以多元羧酸及多元醇为原料的共聚物,优选的材料及组成如下。
作为上述多元羧酸,优选使用脂肪族二羧酸和芳香族二羧酸这两者。另外,脂肪族二羧酸的亚甲基链的亚甲基数的奇偶是会对树脂的结晶性造成影响的因素,具有偶数个亚甲基的二羧酸会生成结晶性高的硬的树脂,因此优选使用具有偶数个亚甲基的脂肪族二羧酸。作为亚甲基数为偶数的脂肪族二羧酸,可例示琥珀酸(亚甲基数为2)、己二酸(亚甲基数为4)、辛二酸(亚甲基数6)、癸二酸(亚甲基数8)。
作为芳香族二羧酸,可例示间苯二甲酸、对苯二甲酸、萘二甲酸、邻苯二甲酸酐。
另外,通过将芳香族二羧酸相对于脂肪族二羧酸与芳香族二羧酸的合计量的含有率设为40~80摩尔%的范围,换言之通过将脂肪族二羧酸的含有率限定在20~60摩尔%的范围,从而能够成为下述成型用包装材料:可生成粘接强度高且成型性良好的树脂,成型性良好从而能够成型出侧壁高的壳体,并且能够抑制金属箔层4与耐热性树脂层2的层间剥离。另外,芳香族二羧酸的含有率小于40摩尔%,则膜物性下降、变得容易发生内聚剥离,因此变得容易发生层间剥离。另一方面,若芳香族二羧酸的含有率超过80%,则有树脂变硬、密合性能下降的倾向。特别优选的芳香族二羧酸的含有率为50~70摩尔%。
作为上述多元醇,可例示乙二醇、丙二醇、1,3-丁二醇、1,4-丁二醇、二乙二醇、二丙二醇、新戊二醇、1,5-戊二醇、1,6-己二醇、辛二醇、1,4- 环己二醇、2-丁基-2-乙基-1,3-丙二醇。
关于上述聚酯树脂的分子量,分别地,将数均分子量(Mn)规定为 8,000~25,000的范围,将重均分子量(Mw)规定为15,000~50,000的范围,进一步地将它们的比率(Mw/Mn)设为1.3~2.5。通过使数均分子量(Mn)为8,000以上、重均分子量(Mw)为15,000以上,从而可得到适当的涂膜强度和耐热性,通过使数均分子量(Mn)为25,000以下、重均分子量(Mw)为50,000以下,从而不会过度变硬、可得到适当的涂膜伸长率。另外,通过使其比率(Mw/Mn)为1.3~2.5,能够成为适当的分子量分布,且保持粘接剂涂布适性(分布宽)和性能(分布窄)的平衡。上述聚酯树脂的特别优选的数均分子量(Mn)为10,000~ 23,000,特别优选的重均分子量(Mw)为20,000~40,000,特别优选的 (Mw/Mn)为1.5~2.3。
上述聚酯树脂的分子量可以通过用多官能性的异氰酸酯进行扩链来调节。即,用NCO连接主剂中的聚酯成分则生成末端为羟基的聚合物,可以通过调节异氰酸酯基与聚酯的羟基的当量比来调节聚酯树脂的分子量。本发明中,优选使用以它们的当量比(OH/NCO)成为1.01~10的方式连接而成的聚酯树脂。另外,作为其他的分子量调节方法,可列举改变多元羧酸与多元醇的缩聚反应的反应条件(调节多元羧酸与多元醇的配合摩尔比)。
另外,可以添加环氧系树脂、丙烯酸系树脂作为粘接主剂的添加剂。
上述作为固化剂的多官能异氰酸酯化合物可以使用芳香族系、脂肪族系、脂环族系的各种异氰酸酯化合物。作为具体例,可列举源自脂肪族系的六亚甲基二异氰酸酯(HDI)、异佛尔酮二异氰酸酯(IPDI)、芳香族系的甲苯二异氰酸酯(TDI)、二苯基甲烷二异氰酸酯(MDI)等二异氰酸酯中的一种或两种以上的多官能异氰酸酯改性体。作为改性方法,除了与水、甘油、三羟甲基丙烷等多官能活性氢化合物的加合物以外,还可列举利用异氰脲酸酯化、碳二亚胺化、聚合化等多聚化反应得到的多官能异氰酸酯改性体,也可以使用这些中的一种或混合使用两种以上。但是,为了增大固化后的粘接强度、得到耐热性树脂层2的剥离防止效果,优选含有50摩尔%以上的芳香族系异氰酸酯化合物。特别优选的芳香族系异氰酸酯化合物的含有率为70摩尔%以上。
上述二液固化型聚酯氨基甲酸酯树脂中,主剂与固化剂的配合比例优选为:相对于多元醇羟基(-OH)1摩尔,以异氰酸酯官能团(-NCO) 2~25摩尔的比例进行配合。若它们的摩尔比(-NCO)/(-OH)小于2,则异氰酸酯官能团(-NCO)变少,有无法进行充分的固化反应、无法得到适当的涂膜强度及耐热性的可能性。另一方面,若(-NCO)/(-OH) 超过25、异氰酸酯官能团(-NCO)变多,则有与多元醇以外的官能团的反应过度进行,涂膜过度变硬,无法得到适当的伸长率的可能性。特别优选的多元醇羟基与异氰酸酯官能团的摩尔比(-NCO)/(-OH)为5~ 20。
上述二液固化型聚酯氨基甲酸酯树脂的、反应后的固化膜优选具有以下的物性。上述固化膜优选基于拉伸试验(JIS K7162)的杨氏模量为 70~400Mpa,以确保成型用包装材料1的良好的成型性和层间的接合强度。特别优选的杨氏模量为100~300MPa。另外,优选断裂强度为20~ 70Mpa、断裂伸长率为50~400%。特别优选的断裂强度为30~50MPa,特别优选的断裂伸长率为100~300%。进一步地,优选拉伸应力-应变曲线(S-S曲线)在断裂前不显示强度下降。图2示出S-S曲线的3个模式。相对于拉伸应力,模式A的应变量小、模式B的应变量大,但是均是应变量随着拉伸应力的增加而增加,观察不到断裂前的强度下降。另一方面,模式C中拉伸应力在应变量增加的过程中下降,在断裂前显示强度下降。本发明中,优选二液固化型粘接剂的固化膜在S-S曲线中无强度下降。进一步优选的是,S-S曲线中无强度急剧变化的拐点。
对于上述包含二液固化型聚酯氨基甲酸酯树脂的粘接剂而言,使作为聚酯树脂原料的多元羧酸及多元醇缩聚,根据需要进一步用多官能性的异氰酸酯进行扩链,并混合溶剂及氨基甲酸酯化反应催化剂、用于提高粘接力的偶联剂、环氧树脂、消泡剂、流平剂、紫外线吸收剂、抗氧化剂等各种添加剂而制成流动状的聚酯树脂溶液,向其中配合作为固化剂的多官能异氰酸酯化合物或进一步配合溶剂,制备成低粘度流动状物。
着色粘接剂组合物通过以规定比例来配合着色颜料及用上述方法制备的包含二液固化型聚酯氨基甲酸酯树脂的粘接剂(包含溶剂、各种添加剂)而制备。金属箔层4与耐热性树脂层2的贴合方法没有限定,可推荐被称为干式层压的方法。具体而言,在金属箔层4的上表面或耐热性树脂层2的下表面、或这两个面上涂布所制备的着色粘接剂组合物,使溶剂蒸发而制成干燥被膜后,使金属箔层4和耐热性树脂层2贴合。然后再按照二液固化型聚酯氨基甲酸酯树脂的固化条件使其固化。由此,金属箔层4和耐热性树脂层2介由第一粘接剂层5而接合。需要说明的是,着色粘接剂组合物的涂布方法可例示凹版涂布法、逆向辊涂法、唇辊涂法(lip rollcoating)等。
(第二粘接剂层)
作为上述第二粘接剂层6,没有特别限定,可列举例如由聚氨基甲酸酯系粘接剂、丙烯酸系粘接剂、环氧系粘接剂、聚烯烃系粘接剂、弹性体系粘接剂、氟系粘接剂、酸改性聚丙烯粘接剂等形成的粘接剂层。其中,优选使用丙烯酸系粘接剂、聚烯烃系粘接剂,这种情况下可以提高包装材料1的耐电解液性及水蒸气阻隔性。
金属箔层4与热塑性树脂层3的贴合方法没有限定,和上述金属箔层4和耐热性树脂层2的贴合同样地,可例示将构成第二粘接剂层的粘接剂进行涂布并使其干燥后进行贴合的干式层压法。
(成型用包装材料的制作)
在金属箔层4的上表面介由上述第一粘接剂层5(着色粘接剂组合物)贴合耐热性树脂层2,在下表面介由第二粘接剂层6贴合热塑性树脂层3,由此制成层叠物。将该层叠物按照所使用二液固化型聚酯氨基甲酸酯树脂的固化条件在规定温度下进行保持,由此在金属箔层4的两面分别介由第一粘接剂层5及第二粘接剂层6接合耐热性树脂层2及热塑性树脂层3,由此制作成型用包装材料1。
需要说明的是,对于本发明的成型用包装材料而言,各层的贴合方法及贴合工序并不限定于上述的方法及工序,利用其他方法、工序制作的情况也包含在本发明中。
[成型用包装材料的其它方式]
本发明的成型用包装材料不限于图1所示的层叠结构,也可以追加层而提高作为包装材料的功能。图3所示的成型用包装材料10为在金属箔层4的两面形成有化学转化被膜11a、11b的材料。另外,图4所示的成型用包装材料20为除了形成有上述化学转化被膜11a、11b以外还在耐热性树脂层2的外表面形成有哑光涂层21的材料。
(金属箔层的化学转化被膜)
成型用包装材料的外侧层及内侧层为由树脂形成的层,对这些树脂层而言,存在极微量的光、氧气、液体从壳体的外部进入的可能性,且存在内容物(电池的电解液、食品、医药品等从内部渗出的可能性。如果这些侵入物到达金属箔层,则成为金属箔层的腐蚀原因。本发明的成型用包装材料中,通过在金属箔层4的表面形成耐腐蚀性高的化学转化被膜11a、11b,从而可以实现金属箔层4的耐腐蚀性的提高。
化学转化被膜为通过对金属箔表面实施化学转化处理而形成的被膜,例如,可通过对金属箔实施铬酸盐处理、使用了锆化合物的无铬型化学转化处理来形成。例如,在铬酸盐处理的情况下,在进行了脱脂处理的金属箔的表面涂布下述1)~3)中的任一混合物的水溶液后进行干燥。
1)磷酸、与铬酸、与氟化物的金属盐及氟化物的非金属盐中的至少一者的混合物
2)磷酸、与丙烯酸系树脂、壳聚糖衍生物树脂及酚系树脂中的任一者、与铬酸及铬(III)盐中的至少一者的混合物
3)磷酸、与丙烯酸系树脂、壳聚糖衍生物树脂、酚系树脂中的任一者、与铬酸及铬(III)盐中的至少一者、与氟化物的金属盐及氟化物的非金属盐中的至少一者的混合物
上述化学转化被膜11a、11b以铬附着量计优选为0.1~50mg/m2,特别优选为2~20mg/m2。利用上述铬附着量的化学转化被膜,能够形成耐腐蚀性高的成型用包装材料。
需要说明的是,图3的成型用包装材料10为在金属箔层4的两面形成有化学转化被膜11a、11b的例子,但是在任意一个面上具有化学转化被膜的包装材料也包含在本发明中。
(哑光涂层)
哑光涂层21形成在耐热性树脂层2的外表面,为对成型用包装材料 20的表面赋予良好的滑动性、提高成型性的层。
上述哑光涂层21为由在耐热性树脂成分中分散含有无机微粒的树脂组合物形成的哑光涂层。其中,上述哑光涂层21优选为下述构成:由在二液固化型的耐热性树脂中含有0.1质量%~1质量%的平均粒径为 1μm~10μm的无机微粒的树脂组合物形成。
作为上述耐热性树脂,可列举例如丙烯酸系树脂、环氧系树脂、聚酯系树脂、氨基甲酸酯系树脂、聚烯烃系树脂、氟系树脂等。从成型性、耐化学药品性、耐溶剂性及耐划痕性优异的观点出发,优选使用下述树脂:所述树脂由包含含有苯氧树脂及氨基甲酸酯树脂的主剂树脂和固化剂的树脂组合物形成,并且上述主剂树脂中的苯氧树脂与氨基甲酸酯树脂的质量比为,相对于苯氧树脂1,氨基甲酸酯树脂为0.5~2。另外,可以使用主剂为多元醇、固化剂为多官能异氰酸酯的二液固化型耐热性树脂的耐热性树脂。
作为上述无机微粒,没有特别限定,可列举例如二氧化硅、氧化铝、氧化钙、碳酸钙、硫酸钙、硅酸钙等,其中优选使用二氧化硅。
上述哑光涂层21的形成可通过将包含上述无机微粒和耐热性树脂的哑光涂覆组合物涂布在耐热性树脂层2的表面并使其固化来进行。
上述哑光涂层21的固化后的厚度优选为0.5~5μm。若为比上述下限值薄的层,则滑动性提高效果差,若为比上限值厚的层,则成本增加。特别优选的厚度为1~3μm的范围。
上述哑光涂层21的表面的光泽度值优选以基于JIS Z8741的60°反射角测定值计而设为1%~15%。上述光泽度值例如利用BYK公司制的光泽度测试仪“micro-TRI-gloss-s”以60°反射角进行测定而得到。
形成上述哑光涂层21的工序可以在介由第一粘接剂层5将耐热性树脂层2贴合于金属箔层4后的任意时刻实施。可以在贴合耐热性树脂层2后且贴合热塑性树脂层3前形成哑光涂层21,也可以在将耐热性树脂层2及热塑性树脂层3贴合于金属箔层4后形成哑光涂层21。
需要说明的是,图4的成型用包装材料20示出了在图1的基本构成上增加了化学转化被膜11a、11b及哑光涂层21这两者的例子,但并非必须同时具备上述两者,在图1的基本构成上仅追加哑光涂层21的包装材料也包含在本发明中。
[成型壳体]
通过对本发明的成型用包装材料1、10、20进行成型(深拉深成型、鼓凸成型等),可以得到成型壳体(电池壳体等)。
实施例
然后,对本发明的具体实施例进行说明。需要说明的是,本发明不受这些实施例的特别限定。
[成型用包装材料的制作]
在以下的实施例1~5和比较例1~5中,制作图4所示的层叠结构的成型用包装材料20。就上述实施例及比较例而言,仅构成第一粘接剂层5的着色粘接剂组合物中的着色颜料浓度、着色粘接剂组合物的涂布量及第一粘接剂层中的着色颜料的含量、及耐热性树脂层2不同,其他材料相同。相同的材料如下所述。
金属箔层4为由厚度40μm的A8079构成的铝箔4,在该铝箔的两面涂布由聚丙烯酸、三价铬化合物、水、醇形成的化学转化处理液,于 150℃进行干燥而形成化学转化被膜11a、11b。该化学转化被膜11a、11b 的铬附着量为10mg/m2。
作为内侧层的热塑性树脂层3是厚度为40μm的未拉伸聚丙烯膜。
作为第二粘接剂层6,使用聚丙烯酸系粘接剂。
(第一粘接剂层)
构成第一粘接剂层5的着色粘接剂组合物中,使用炭黑作为着色颜料,使用二液固化型聚酯氨基甲酸酯树脂作为粘接剂,其通过以下方法而制备。
首先,制备作为二液固化型聚酯氨基甲酸酯树脂的主剂的聚酯树脂 (聚酯多元醇)。对于主剂而言,将新戊二醇30摩尔份、乙二醇30摩尔份、1,6-己二醇40摩尔份于80℃熔融,边搅拌边于210℃使作为脂肪族二羧酸的己二酸(亚甲基数4)30摩尔份、作为芳香族二羧酸的间苯二甲酸70摩尔份进行20小时缩聚反应,得到聚酯多元醇。该聚酯多元醇的数均分子量(Mn)为12,000、重均分子量(Mw)为20,500,它们的比率(Mw/Mn)为1.71。进一步向该聚酯多元醇40质量份中加入乙酸乙酯60质量份,制成流动状的聚酯多元醇树脂溶液。另外,羟值为 2.2mgKOH/g(溶液值)。
然后,向上述的聚酯多元醇树脂溶液100质量份、乙酸乙酯64.4质量份中配合平均粒径为1.0μm的所需量的炭黑,使用颜料分散机将炭黑颜料分散,得到将炭黑浓度相对于固态成分(聚酯多元醇与炭黑的合计) 调节为表1所示的浓度的含着色颜料的主剂。然后,相对于上述含着色颜料的主剂100质量份配合作为固化剂的、作为芳香族异氰酸酯化合物的甲苯二异氰酸酯(TDI)(芳香族系)与三羟甲基丙烷的加合物 (NCO%13.0%,固态成分75%)7.1质量份,进一步配合乙酸乙酯34.1 质量份并充分搅拌,由此得到着色粘接剂组合物。上述着色粘接剂组合物中,异氰酸酯官能团(-NCO)与聚酯多元醇羟基(-OH)的摩尔比(-NCO)/(-OH)为10。
制作上述二液固化型聚酯氨基甲酸酯树脂粘接剂的固化膜,即第一粘接剂层的组成中除了着色颜料以外的组成的固化膜,评价其物性。
按照干燥后的厚度成为50μm的方式在非粘接性的未处理PP膜上涂布二液固化型聚酯氨基甲酸酯树脂粘接剂,使溶剂干燥后,于60℃进行熟化而使其固化,直至残存异氰酸酯成为5%以下为止。将固化膜从未处理PP膜剥离,切成15mm宽,将其作为试验片。
在标记点距离为50mm、拉伸速度为200mm/min的条件下对所制作的试验片进行拉伸试验,测定杨氏模量、断裂强度及断裂伸长率,结果,杨氏模量为140MPa,断裂强度为48MPa,断裂伸长率为217%。另外,求出该拉伸试验中的S-S曲线,结果其模式为图2所示的模式A。
(耐热性树脂层)
实施例1~4及比较例5使用热水收缩率为4.0%的厚度为25μm的双轴拉伸尼龙膜,实施例5及比较例1~4使用热水收缩率为1.5%的 25μm的双轴拉伸尼龙膜(参见表1)。需要说明的是,热水收缩率利用上述方法而测定。
(各层的贴合)
在形成有化学转化被膜11a、11b的铝箔4的一个面上,涂布规定量的着色粘接剂组合物并使其干燥,形成第一粘接剂层5。将各例的着色粘接剂组合物的组成及涂布量(干燥后的重量)示于表1,并且将由它们计算而得的第一粘接剂层5中的炭黑含量及干燥后的第一粘接剂层5 的膜厚示于表1。然后,在上述第一粘接剂层5上贴合耐热性树脂层2。
接着,在上述铝箔的另一个面上涂布聚丙烯酸系粘接剂作为第二粘接剂层6,贴合热塑性树脂层3。
在使用哑光涂层21时,将作为耐热性树脂的氟乙烯-乙烯基酯80质量份、作为无机微粒的硫酸钡10质量份、粉状二氧化硅10质量份混合,由此制备哑光涂覆组合物。以干燥后的厚度成为2μm的方式将该哑光涂覆组合物涂布于耐热性树脂层2。
进一步地,将该贴合物在40℃环境下熟化5天,由此得到图4所示的成型用包装材料20。
[成型用包装材料的评价]
对于进行上述操作而得到的各成型用包装材料,基于下述评价法进行评价。将它们的结果示于表1。
(掩蔽性)
从耐热性树脂层2侧目视观察成型用包装材料20,看不到金属箔层 4评价为“有掩蔽性:〇”,能看到金属箔层4评价为“无掩蔽性:×”。
(有无剥离)
对于各实施例、各比较例中的各自,分别制造30个成型用包装材料 20。对各成型用包装材料20,以内侧的热塑性树脂层3与冲头接触的方式用冲头和模头等进行深拉深成型而形成长33mm×宽54mm×深4.0mm 的凸部31,制作在凸部31的周围具有平坦的凸缘这种形状的试验材料30(参见图5)。
将上述试验材料30的凸部31的顶面32压碎,对压碎后的试验材料 30进行高温高湿试验及温水浸没试验,并研究耐热性树脂层2有无剥离。高温高湿试验中,使所压碎的试验材料30在温度70℃、湿度90%的气氛中保持2周。另外,温水浸没试验中,使所压碎的试验材料30浸没在 45℃的温水中并保持2周。
两试验中,均目视观察试验后的30个试验材料30,基于以下基准判定耐热性树脂层2从金属箔层4剥离的试验材料30的个数。
◎:0个
〇:1~2个
△:3~5个
×:6~30个
(卷曲特性)
将上述实施例1~5及比较例1~5中制造的成型用包装材料20切成 100mm×100mm的坯料(日语:ブランク)形状,由此制作试验材料。接着,将这些试验材料以其哑光涂层21朝上的方式置于水平基台上,测定此时由于卷曲而翘起的高度,按照下述基准进行评价。
〇:0~20mm
×:超过20mm
(成型高度)
使用不限制成型深度的直模,将成型用包装材料在下述成型条件下进行1级深拉深成型,对各成型深度(9.0mm、8.5mm、8.0mm、7.5mm、 7.0mm、6.5mm、6.0mm、5.5mm、5.0mm、4.5mm、4.0mm)评价成型性,研究能够进行在角部完全不产生针孔及破裂的良好成型的最大成型深度 (mm),基于下述判定基准评价成型性。评价为◎及〇则为合格品。需要说明的是,通过目视观察有无透过针孔的透射光来研究有无针孔。
成型条件
成型模具…冲头:33mm×54mm,模头:80mm×120mm,角R:2mm,冲头R:1.3mm,模头R:1mm
判定基准
不产生针孔及破裂的最大成型深度为:
◎:7.0mm以上
○:6.0mm以上且小于7.0mm
△:超过5.0mm且小于6.0mm
×:5.0mm以下
(综合评价)
基于掩蔽性、高温高湿试验、温水浸没试验、卷曲特性、成型高度这5个试验,按照下述基准进行综合评价。
◎:有2个以上◎且没有×。
〇:有1个◎且没有×
×:有×或△[表1]
由表1可确认,实施例1~5在严苛的环境下也不发生耐热性树脂层剥离,可得到基于着色颜料的掩蔽性,且不易卷曲、成型性也优异。
产业上的可利用性
本发明涉及的成型用包装材料优选作为笔记本电脑用、手机用、车载用、定置型的锂离子聚合物二次电池等电池的壳体使用,此外还优选作为食品的包装材料、医药品的包装材料,但是不特别限于这些用途。其中,特别优选用于电池壳体。
本申请基于2020年1月10日提出申请的日本专利申请-日本特愿 2020-2778号及2020年12月2日提出申请的日本专利申请-日本特愿 2020-199974号主张优先权,其公开内容直接构成本申请的一部分。
应认识到,在此使用的术语及表述是为了说明而使用的,并非为了进行限定性解释而使用,也不排除在此示出且说明的特征事项的任何等同物,本申请权利要求范围内的各种变形也是允许的。
Claims (6)
1.成型用包装材料,其包含作为外侧层的耐热性树脂层、作为内侧层的热塑性树脂层、配设于这两层之间的金属箔层、配设于所述金属箔层与耐热性树脂层之间的第一粘接剂层、以及配设于所述金属箔层与热塑性树脂层之间的第二粘接剂层,所述成型用包装材料的特征在于,
所述第一粘接剂层是涂布5g/m2~10g/m2的含有着色颜料和粘接剂的着色粘接剂组合物而成的。
2.根据权利要求1所述的成型用包装材料,其中,所述第一粘接剂层的膜厚为4.5μm~10μm。
3.根据权利要求1所述的成型用包装材料,其中,在所述金属箔层的至少一个面上具有化学转化被膜。
4.根据权利要求1所述的成型用包装材料,其中,所述耐热性树脂层由热水收缩率为2%~20%的拉伸膜形成。
5.根据权利要求1所述的成型用包装材料,其特征在于,在所述耐热性树脂层的外表面具有哑光涂层。
6.成型壳体,其特征在于,其是将权利要求1~5中任一项所述的成型用包装材料进行深拉深成型或鼓凸成型而成的。
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