CN111770961A - 树脂组合物以及单层和多层膜 - Google Patents
树脂组合物以及单层和多层膜 Download PDFInfo
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- CN111770961A CN111770961A CN201980014955.3A CN201980014955A CN111770961A CN 111770961 A CN111770961 A CN 111770961A CN 201980014955 A CN201980014955 A CN 201980014955A CN 111770961 A CN111770961 A CN 111770961A
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- ethylene
- propylene
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Classifications
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Abstract
本发明的树脂组合物含有:满足下述(a)的丙烯系聚合物(A)35~59.9质量份,满足下述(b)的软质丙烯系共聚物(B)25~40质量份,含有来自不饱和羧酸和/或其衍生物的结构单元的聚烯烃(C)0.1~10质量份;和满足下述(d)的乙烯系聚合物(D)15~30质量份(其中,将(A)、(B)、(C)和(D)的合计设为100质量份),上述树脂组合物按照ASTM D-1238、以230℃、2.16kg负荷测得的MFR为7g/10分钟以上25g/10分钟以下。(a)在差示扫描量热测定中观测到的熔点(Tm)为120℃以上。(b)按照ASTM D-1238、以230℃、2.16kg负荷测得的MFR处于0.01~100g/10分钟的范围,并且满足下述条件(b-1)和(b-2)。(b-1)在差示扫描量热测定中观测到的熔点(Tm)为110℃以下,或者观测不到熔点。(b-2)具有源自丙烯的结构单元以及源自选自乙烯和碳原子数4~20的α‑烯烃中的至少1种烯烃的结构单元,源自选自乙烯和碳原子数4~20的至少1种α‑烯烃的结构单元的含量为30mol%以下,利用13C-NMR测得的全同立构三单元组分率(mm分率)为80%以上。(d)为乙烯均聚物或乙烯与选自碳原子数3~20的α‑烯烃中的至少1种α‑烯烃的共聚物,其按照ASTM D-1238、以190℃、2.16kg负荷测得的MFR为0.1~10g/10分钟的范围。包含由本发明的树脂组合物形成的层的单层或多层膜的粘接性优异、特别是在低热量下的粘接性优异,而且还变形加工时的耐白化性优异,能够适合用作食品包装材料、建筑用材料、以及形成锂离子电池的外包装体等的包装材料。另外,上述单层或多层膜在高速的变形加工和深拉深加工中也表现良好的耐白化性。
Description
技术领域
本发明涉及树脂组合物以及单层和多层膜,更详细而言,涉及能够适用于食品包装材料和建筑用材料、锂离子电池的外装材料等的单层和多层膜、以及这些膜所含有的树脂组合物。
背景技术
一直以来,聚丙烯作为刚性、耐热性、透明性等优异的热塑性成型材料被广泛利用。该聚丙烯是非极性材料,因此,与例如乙烯-乙烯醇共聚物等极性材料的粘接性不足,希望改良粘接性、特别是提高在低热量下的粘接性。以改良粘接性为目的,利用不饱和羧酸或其衍生物对聚丙烯进行改性的技术已广为人知。另外,由于聚丙烯的柔软性差,因此作为粘接剂使用时,通常在聚丙烯中配合有软质橡胶成分。
这样在聚丙烯中配合软质橡胶成分时,可以得到粘接性被改善的聚丙烯系的粘接剂(例如专利文献1和专利文献2),但另一方面,软质橡胶成分在拉深加工、弯折加工这样的二次加工时成为白化的原因,因此也要求耐白化性的改良。作为特别需要拉深加工、弯折加工的具体用途,可以列举食品包装材料和建筑用材料、锂离子电池的包装材料等。
其中,近年来,锂离子电池在便携式电子设备和汽车等中的用途不断扩大,另外,在锂离子电池中,随着应对形状的自由度和小型化,将多层膜作为包装材料而成的袋型或模压型的外包装体的用途不断扩大。包含该多层膜的包装材料至少由基材层、金属箔层和热粘接性树脂层以及将这些层中相邻的2层粘接的粘接剂层构成。多层膜由于形状的自由度大,所以在制造这些袋型或模压型的外包装体时容易加工,但在使多层膜变形时,有时变形的地方会白化。由于如果外包装体存在白化的地方,则会成为短路的原因,因此要求耐白化性优异的材料。
在专利文献3中记载了一种电池用包装材料,其是通过至少将基材层、至少一面具有化学法表面处理层的金属箔层、酸改性聚烯烃层以及由高熔点聚丙烯层和乙烯-丙烯无规共聚物层构成的热封层依次叠层而成的,上述高熔点聚丙烯层比上述乙烯-丙烯无规共聚物层更靠上述金属箔层侧而配置,熔点为150℃以上。在该电池用包装材料中,通过将熔点为150℃以上的高熔点聚丙烯层比乙烯-丙烯无规共聚物层更靠金属箔层侧而配置,即使因过充电等而在外包装体内部发生温度上升时,高熔点聚丙烯层也不会熔化,得以防止金属端子与金属箔层接触,能够抑制发生内部短路。然而,对于该电池用包装材料,并不能期待充分的耐白化性。
在专利文献4中记载了一种包含丙烯-乙烯嵌段共聚物(A)的电池包装膜用聚丙烯系树脂组合物,该丙烯-乙烯嵌段共聚物(A)利用多段聚合得到,且包含满足乙烯含量等特定的条件的丙烯系聚合物成分(A1)和丙烯-乙烯无规共聚物成分(A2)。关于由该组合物形成的膜,记载了其耐热性、密封性和成型性优异,具有高的密封强度和耐冲击性,具有变形加工时的耐白化性和抗破裂性等平衡良好且均得到提高这样的效果。然而,关于耐白化性,实际情况是尚未达到所要求的水平。
进一步而言,近年来,为了提高生产性,高速成型渐成主流。成型速度高时,所施加的用于粘接的热量降低,有时不能得到充分的粘接力,因此要求即使在那样的高速成型下也能够赋予良好的粘接力的粘接性树脂。
现有技术文献
专利文献
专利文献1:日本特开平9-111069号公报
专利文献2:日本特开平4-300933号公报
专利文献3:日本特开2007-273398号公报
专利文献4:日本特开2015-230777号公报
发明内容
发明所要解决的课题
鉴于上述问题点,本发明的目的在于提供一种能够用于食品包装材料、建筑用材料和锂离子电池的外包装体等的、粘接性、特别是低热量下的粘接性优异、进一步而言变形加工时的耐白化性优异的包装材料,特别而言,提供一种能够利用共挤出或叠层涂布、层压这样的成型方法制作的包装材料。
用于解决课题的技术方案
实现上述目的的本发明是一种树脂组合物,其含有:
满足下述(a)的丙烯系聚合物(A)35~59.9质量份;
满足下述(b)的软质丙烯系共聚物(B)25~40质量份;
含有来自不饱和羧酸和/或其衍生物的结构单元的聚烯烃(C)0.1~10质量份;和
满足下述(d)的乙烯系聚合物(D)15~30质量份(其中,将(A)、(B)、(C)和(D)的合计设为100质量份),
上述树脂组合物按照ASTM D-1238、以230℃、2.16kg负荷测得的MFR为7g/10分钟以上25g/10分钟以下。
(a)在差示扫描量热测定中观测到的熔点(Tm)为120℃以上。
(b)按照ASTM D-1238、以230℃、2.16kg负荷测得的MFR处于0.01~100g/10分钟的范围,并且满足下述条件(b-1)和(b-2)。
(b-1)在差示扫描量热测定中观测到的熔点(Tm)为110℃以下,或者观测不到熔点。
(b-2)具有源自丙烯的结构单元以及源自选自乙烯和碳原子数4~20的α-烯烃中的至少1种烯烃的结构单元,源自选自乙烯和碳原子数4~20的至少1种α-烯烃的结构单元的含量为30mol%以下,利用13C-NMR测得的全同立构三单元组分率(mm分率)为80%以上。
(d)为乙烯均聚物或乙烯与选自碳原子数3~20的α-烯烃中的至少1种α-烯烃的共聚物,其按照ASTM D-1238、以190℃、2.16kg负荷测得的MFR为0.1~10g/10分钟的范围。
优选在上述树脂组合物中,聚烯烃(C)含有以来自马来酸酐的结构单元换算计为0.01~5质量%的来自不饱和羧酸的结构单元,并且,在聚烯烃(C)中,除上述来自不饱和羧酸的结构单元以外的结构单元中的来自丙烯的结构单元的含有比率为90~100摩尔%。
本发明的单层或多层膜包含至少1层含有上述树脂组合物的层。
作为本发明的多层膜的一个方式,可以列举包含至少1层含有上述树脂组合物的层和至少2层含有上述组合物的层以外的其他层,含有上述组合物的层的两面与上述其他层相接触的多层膜。
作为本发明的多层膜的一个方式,可以列举包含至少1层含有上述树脂组合物的层和至少1层选自含金属层、聚烯烃层和极性树脂层的层,含有上述组合物的层与上述含金属层、聚烯烃层和极性树脂层中的至少1层相接触的多层膜。
本发明的单层或多层膜可以作为食品包装材料用膜、建筑用材料用膜和电池包装用膜。
在本发明的单层或多层膜的制造方法中,将上述树脂组合物熔融挤出成型。
发明效果
包含由本发明的树脂组合物形成的层的单层或多层膜的粘接性优异、特别是低热量下的粘接性优异,进一步而言变形加工时的耐白化性优异,能够适合用作食品包装材料、建筑用材料和形成锂离子电池的外包装体等的包装材料。另外,上述单层或多层膜即使在高速的变形加工和深拉深加工中也表现良好的耐白化性。上述单层或多层膜能够利用共挤出、叠层涂布、层压这样的成型方法制作。
具体实施方式
本发明的树脂组合物含有:丙烯系聚合物(A);软质丙烯系共聚物(B);含有来自不饱和羧酸和/或其衍生物的结构单元的聚烯烃(C);和乙烯系聚合物(D)。
丙烯系聚合物(A)
作为丙烯系聚合物(A),可以列举丙烯均聚物或丙烯与至少1种除丙烯以外的碳原子数为2~20的α-烯烃的共聚物。其中,作为除丙烯以外的碳原子数为2~20的α-烯烃,可以列举乙烯、1-丁烯、1-戊烯、1-己烯、4-甲基-1-戊烯、1-辛烯、1-癸烯、1-十二碳烯、1-十四碳烯、1-十六碳烯、1-十八碳烯、1-二十碳烯等,优选乙烯或碳原子数为4~10的α-烯烃。
丙烯与这些α-烯烃的共聚物可以是无规共聚物,也可以是嵌段共聚物。在α-烯烃与丙烯的共聚物中,能够以35摩尔%以下、优选30摩尔%以下的比例含有源自这些α-烯烃的结构单元。
丙烯系聚合物(A)满足下述条件(a)。
(a)在差示扫描量热测定中观测到的熔点(Tm)为120℃以上。
上述熔点(Tm)优选为120~170℃、更优选为130~165℃。
丙烯系聚合物(A)的按照ASTM D1238、以230℃、负荷2.16kg测定的熔体流动速率(MFR)希望处于0.01~1000g/10分钟、优选处于0.05~100g/10分钟的范围。
上述丙烯系聚合物(A)可以是全同立构结构、间同立构结构中的任意一种,如后所述,可以考虑与软质丙烯系共聚物(B)的相容性而选择任一种的结构。
即,作为上述丙烯系聚合物(A)的形态,可以列举全同立构丙烯系聚合物(A1)和间同立构丙烯系聚合物(A2)。
作为全同立构丙烯系聚合物(A1),可以列举:耐热性优异的均聚丙烯,例如通常除丙烯以外的共聚成分为3mol%以下的公知的均聚丙烯;耐热性与柔软性的平衡优异的嵌段聚丙烯,例如通常具有3~30质量%的正癸烷溶出橡胶成分的公知的嵌段聚丙烯;和柔软性与透明性的平衡优异的无规聚丙烯,例如通常利用差示扫描量热计DSC测定的熔化峰处于120℃以上、优选130℃~150℃的范围的公知的无规聚丙烯,为了获得目标物性,可以从这些之中适当选择,或者能够同时使用熔点或刚性不同的2种以上的上述聚丙烯成分。
这样的全同立构丙烯系聚合物(A1),例如能够通过利用以下的齐格勒催化剂体系或使用茂金属化合物作为催化剂的成分之一的茂金属催化剂体系,使丙烯聚合、或者使丙烯与其他的α-烯烃共聚而制造,其中,上述齐格勒催化剂体系包含含有镁、钛、卤素和电子供体作为必需成分的固体催化剂成分和有机铝化合物及电子供体。
间同立构丙烯系聚合物(A2)含有源自丙烯的结构单元90mol%以上以及源自选自乙烯和碳原子数4~20的α-烯烃中的一种以上的结构单元10mol%以下,优选含有源自丙烯的结构单元91mol%以上以及源自选自乙烯和碳原子数4~20的α-烯烃中的一种以上的结构单元9mol%以下(其中,将两种结构单元的合计设为100mol%)。
作为碳原子数4~20的α-烯烃,可以列举1-丁烯、3-甲基-1-丁烯、1-戊烯、1-己烯、4-甲基-1-戊烯、1-辛烯、1-癸烯、1-十二碳烯、1-十四碳烯、1-十六碳烯、1-十八碳烯、1-二十碳烯等。
间同立构丙烯系聚合物(A2)例如能够利用国际公开号WO2011/078054号所记载的方法进行制造。
(B)软质丙烯系共聚物
软质丙烯系共聚物(B)满足下述条件(b)。
(b)按照ASTM D-1238、以230℃、2.16kg负荷测得的MFR处于0.01~100g/10分钟的范围,并且满足下述条件(b-1)和(b-2)。
(b-1)熔点(Tm)为110℃以下,或者观测不到熔点。
(b-2)具有源自丙烯的结构单元以及源自选自乙烯和碳原子数4~20的α-烯烃中的至少1种烯烃的结构单元,源自选自乙烯和碳原子数4~20的至少1种α-烯烃的结构单元的含量为30mol%以下,利用13C-NMR测得的全同立构三单元组分率(mm分率)为80%以上。
以下,对条件(b)等进行详细说明。
条件(b)
软质丙烯系共聚物(B)的熔体流动速率(MFR;ASTM D-1238、230℃、2.16kg负荷下)为0.01~100g/10分钟,优选为0.01~30g/10分钟。
另外,软质丙烯系共聚物(B)满足条件(b-1)和(b-2)。
(条件(b-1))
在差示扫描量热测定中观测到的熔点(Tm)为110℃以下,或者观测不到熔点。其中,所谓观测不到熔点,是指在差示扫描量热测定中在-150~200℃的范围,观测不到结晶熔化热为1J/g以上的结晶熔化峰。熔点测定条件的详细如后述内容的实施例的项所记载。
上述熔点(Tm)优选为40~110℃、更优选为45~108℃。熔点(Tm)满足上述条件时,在与丙烯系聚合物的相容性和透明性的方面优选。
(条件(b-2))
具有源自丙烯的结构单元以及源自选自乙烯和碳原子数4~20的α-烯烃中的至少1种烯烃的结构单元,源自选自乙烯和碳原子数4~20的至少1种α-烯烃的结构单元的含量为30mol%以下,利用13C-NMR测得的全同立构三单元组分率(mm分率)为80%以上。
作为碳原子数4~20的α-烯烃,可以列举3-甲基-1-丁烯、1-丁烯、1-戊烯、1-己烯、4-甲基-1-戊烯、1-辛烯、1-癸烯、1-十二碳烯、1-十四碳烯、1-十六碳烯、1-十八碳烯、1-二十碳烯等。作为选自乙烯和碳原子数4~20的α-烯烃中的至少1种烯烃,特别优选乙烯、1-丁烯、1-己烯、4-甲基-1-戊烯、1-辛烯。
源自选自乙烯和碳原子数4~20的至少1种α-烯烃的结构单元的含量优选为5~30mol%、更优选为7~26mol%。
利用13C-NMR测定算出的全同立构三单元组分率(mm)优选为85%以上。全同立构三单元组分率(mm)处于上述范围时,在保持机械物性和耐油性的方面优选。
(其他的条件)
软质丙烯系共聚物(B)在135℃十氢化萘中测得的特性粘度[η]希望为0.1~10dL/g、优选为0.5~10dL/g。
该软质丙烯系共聚物(B)利用X射线衍射测得的结晶度优选为20%以下、更优选为0~15%。
该软质丙烯系共聚物(B)具有单一的玻璃化转变温度,利用差示扫描量热测定(DSC)得到的玻璃化转变温度(Tg)通常在-50℃~10℃的范围、优选在-40℃~0℃的范围、更优选在-35℃~0℃的范围。当软质丙烯系共聚物(B)的玻璃化转变温度(Tg)在上述范围内时,耐寒性、低温特性优异,并且表现出应力吸收性能,因而优选。
差示扫描量热测定例如如下所述进行。将10.00mg左右试样装入专用铝皿中,使用Seiko Instrument Inc.制造的DSCRDC220,根据以200℃/min从30℃升温至200℃,在200℃保持5分钟后,以10℃/min从200℃降温至-100℃,在-100℃再保持5分钟,接着以10℃/min升温时的吸热曲线,求出上述玻璃化转变温度(Tg)。
另外,软质丙烯系共聚物(B)利用GPC测得的分子量分布(Mw/Mn、聚苯乙烯换算、Mw:重均分子量、Mn:数均分子量)优选为3.5以下、更优选为3.0以下、进一步优选为2.5以下。另外,下限值例如为1.5以上。
关于软质丙烯系共聚物(B),可以利用极性单体对其一部分进行接枝改性。作为极性单体,可以列举含有羟基的烯属不饱和化合物、含有氨基的烯属不饱和化合物、含有环氧基的烯属不饱和化合物、芳香族乙烯基化合物、不饱和羧酸或其衍生物、乙烯基酯化合物、氯乙烯等。改性了的软质丙烯系共聚物(B)可以通过在如上所述的软质丙烯系共聚物(B)上接枝聚合极性单体而得到。在软质丙烯系共聚物(B)上接枝聚合如上所述的极性单体时,极性单体相对于软质丙烯系共聚物(B)100质量份,通常以1~100质量份、优选5~80质量份的量使用。该接枝聚合通常在自由基引发剂的存在下进行。作为自由基引发剂,可以使用有机过氧化物或者偶氮化合物等。自由基引发剂既可以与软质丙烯系共聚物(B)和极性单体直接混合使用,也可以溶解在少量的有机溶剂中之后使用。作为该有机溶剂,只要是能够溶解自由基引发剂的有机溶剂,就能够没有特别限定地使用。另外,在软质丙烯系共聚物(B)上接枝聚合极性单体时,也可以使用还原性物质。在使用还原性物质时,能够提高极性单体的接枝量。
软质丙烯系共聚物(B)利用极性单体的接枝改性,可以利用目前公知的方法进行,例如,可以通过将软质丙烯系共聚物(B)溶解在有机溶剂中,接着将极性单体和自由基引发剂等加入到溶液中,在70~200℃、优选80~190℃的温度下反应0.5~15小时、优选1~10小时而进行。另外,也可以使用挤出机等,在无溶剂的条件下使软质丙烯系共聚物(B)与极性单体反应,制造改性了的软质丙烯系共聚物(B)。希望该反应通常在软质丙烯系共聚物(B)的熔点以上、具体为120~250℃的温度下,通常进行0.5~10分钟。
这样得到的改性软质丙烯系共聚物的改性量(极性单体的接枝量)通常希望为0.1~50质量%,优选为0.2~30质量%,进一步优选为0.2~10质量%。
本发明的丙烯系聚合物组合物含有上述的改性软质丙烯系共聚物时,有时与其他的树脂的粘接性、相容性优异,成型体表面的润湿性被改良。
丙烯-α-烯烃无规共聚物(B)例如能够利用国际公开号WO2004/087775号小册子所记载的方法进行制造。
作为上述软质丙烯系共聚物(B)的优选方式,可以列举以下的丙烯-丁烯共聚物(B1)和丙烯-乙烯共聚物(B2)。
关于上述丙烯-丁烯共聚物(B1),在上述的软质丙烯系共聚物(B)中含有70~95摩尔%的量的源自丙烯的结构单元、优选为70~89摩尔%的量的源自丙烯的结构单元。
具有这样的组成的丙烯-丁烯共聚物(B1)具有与上述丙烯系聚合物(A)的良好相容性。
关于丙烯-乙烯共聚物(B2),在上述的软质丙烯系共聚物(B)中含有70~95摩尔%的量的源自丙烯的结构单元、优选为70~93摩尔%的量的源自丙烯的结构单元。
含有来自不饱和羧酸和/或其衍生物的结构单元的聚烯烃(C)
聚烯烃(C)是利用不饱和羧酸和/或其衍生物对聚烯烃进行改性而得到的,含有来自该不饱和羧酸和/或其衍生物的结构单元。
作为接受改性的聚烯烃,例如可以列举聚丙烯(c1)、乙烯-丙烯-α-烯烃共聚物(c2)和乙烯-α-烯烃共聚物(c3)。
聚烯烃(C)可以是单独1种,也可以是2种以上的混合物。例如,可以是聚丙烯(c1)的改性体、乙烯-丙烯-α-烯烃共聚物(c2)的改性体和乙烯-α-烯烃共聚物(c3)的改性体中的任意1种或者它们2种以上的混合物。
聚丙烯(c1)例如是丙烯的均聚物和/或丙烯-α-烯烃共聚物。作为α-烯烃,没有限定,优选列举乙烯和碳原子数4~20的α-烯烃,这些α-烯烃可以是单独1种,也可以是2种以上。作为优选的α-烯烃,为乙烯、碳原子数4~10的α-烯烃,其中特别优选乙烯和碳原子数4~8的α-烯烃。其中,丙烯-α-烯烃共聚物中的源自丙烯的结构单元的含量至少为50摩尔%以上,且少于100%。
聚丙烯(c1)的特性粘度[η]优选为0.1~10dl/g。特性粘度[η]处于该范围时,能够得到成型性和机械强度优异的组合物。
聚丙烯(c1)的制造方法没有特别限定,可以列举使用了齐格勒-纳塔催化剂、茂金属系催化剂等公知催化剂的公知方法。
作为聚丙烯(c1),优选结晶性的聚合物,为共聚物时,可以为无规共聚物,也可以为嵌段共聚物。另外,只要是满足成型性、具有能够耐受形成成型体时的使用的强度的聚合物,对有规立构性、分子量就没有特别限制。也能够直接利用市售的树脂。
聚丙烯(c1)例如为均聚丙烯或丙烯-α-烯烃无规共聚物。另外,也可以含有一些不同的全同立构聚丙烯。
乙烯-丙烯-α-烯烃共聚物(c2)例如由下述的(i)和(ii)规定。
(i)含有来自丙烯的结构单元45~90摩尔%、来自乙烯的结构单元10~25摩尔%、来自碳原子数4~20的α-烯烃的结构单元1~30摩尔%。
(ii)在135℃十氢化萘中的特性粘度[η]处于0.1~10dl/g的范围。
作为上述α-烯烃,可以适当使用碳原子数4~10的α-烯烃,可以是单独1种,也可以是2种以上。关于来自各单体的结构单元的比率,优选丙烯50~85摩尔%、乙烯10~22摩尔%、α-烯烃5~28摩尔%,更优选丙烯55~80摩尔%、乙烯10~20摩尔%、α-烯烃10~28摩尔%。
关于(ii),特性粘度[η]更优选为0.5~8的范围,进一步优选处于0.8~6的范围。特性粘度[η]处于上述的范围时,能够得到柔软性与机械强度的平衡优异且粘接力高的粘接剂。
作为乙烯-丙烯-α-烯烃共聚物(C2)的制造方法,没有特别限定,可以利用使用了齐格勒-纳塔催化剂、茂金属系催化剂等公知催化剂的公知方法制造。
乙烯-丙烯-α-烯烃共聚物(C2)只要是满足成型性、具有能够耐受形成成型体时的使用的强度的聚合物,对有规立构性、分子量就没有特别限制。也能够直接利用市售的树脂。
乙烯-α-烯烃共聚物(c3)例如由下述的(iii)和(iv)规定。
(iii)含有来自乙烯的结构单元50~99摩尔%、来自碳原子数3~20的α-烯烃的结构单元1~50摩尔%。
(iv)在135℃十氢化萘中的特性粘度[η]处于0.1~10dl/g的范围。
作为α-烯烃,更优选碳原子数3~10的α-烯烃,可以是单独1种,也可以是2种以上。关于来自各单体的结构单元的比率,优选乙烯55~98摩尔%、α-烯烃2~45摩尔%,更优选乙烯60~95摩尔%、α-烯烃5~40摩尔%。
关于(iv),特性粘度[η]更优选处于0.5~8的范围,进一步优选处于0.8~6的范围。特性粘度[η]处于上述的范围时,能够得到柔软性与机械强度的平衡优异且粘接力高的组合物。
作为乙烯-α-烯烃共聚物(c3)的制造方法,没有特别限定,可以列举使用了齐格勒-纳塔催化剂、茂金属系催化剂等公知催化剂的公知方法。
乙烯-α-烯烃共聚物(c3)只要成型性优异且能够确保能够耐受形成成型体时的使用的强度,对有规立构性、分子量就没有特别限制。乙烯-α-烯烃共聚物(c3)也可以直接利用市售的树脂。
作为对这些聚烯烃进行改性的不饱和羧酸和/或其衍生物,可以列举具有1个以上的羧酸基的不饱和化合物、具有羧酸基的化合物与烷基醇的酯、具有1个以上的羧酸酐基的不饱和化合物等。作为不饱和化合物所具有的不饱和基团,可以列举乙烯基、亚乙烯基、不饱和环状烃基等。不饱和羧酸和/或其衍生物既可以单独使用1种,也可以组合使用2种以上。这些之中优选不饱和二羧酸或其酸酐,特别优选马来酸、纳迪克酸或它们的酸酐。
聚烯烃(C)所含有的来自不饱和羧酸和/或其衍生物的结构单元的量以来自马来酸酐的结构单元换算计优选为0.01~5质量%,更优选为0.05~3.5质量%。来自不饱和羧酸和/或其衍生物的结构单元的量处于上述范围内时,能够得到成型性与粘接性的平衡优异的树脂组合物。
在聚烯烃(C)中,除上述来自不饱和羧酸和/或其衍生物的结构单元以外的结构单元中的来自丙烯的结构单元的含有比率优选为90~100摩尔%,更优选为95~100摩尔%。来自丙烯的结构单元的含有比率处于上述范围内时,能够得到耐热性优异的树脂组合物。
关于使不饱和羧酸和/或其衍生物接枝的方法,没有特别限定,可以采用溶液法、熔融混炼法等目前公知的接枝聚合法。例如有使聚烯烃熔融、向其中添加不饱和羧酸和/或其衍生物而发生接枝反应的方法,或者将聚烯烃溶解于溶剂而形成溶液、向其中添加不饱和羧酸和/或其衍生物而发生接枝反应的方法等。
乙烯系聚合物(D)
本发明所使用的乙烯系聚合物(D)为乙烯均聚物或乙烯与选自碳原子数3~20的α-烯烃的至少1种α-烯烃的共聚物,可以利用下述的(i)所规定的乙烯均聚物和乙烯-α-烯烃共聚物,作为上述共聚物,优选下述的(ii)所规定的乙烯-α-烯烃共聚物。
(i)按照ASTM D-1238、以190℃、2.16kg负荷测得的MFR为0.1~10g/10分钟的范围。
(ii)含有源自乙烯的结构单元50~99mol%、源自选自碳原子数3~20的α-烯烃中的α-烯烃的结构单元1~50mol%。
关于上述共聚物,作为α-烯烃,可以更适合使用碳原子数3~10的α-烯烃,如果处于该范围,则可以单独使用1种,也可以使用2种以上。关于各单体成分的比率,优选乙烯:55~98mol%、α-烯烃:2~45mol%,更优选乙烯:60~95mol%、α-烯烃:5~40mol%。
关于上述(i),优选MFR处于0.5~8g/10分钟的范围,更优选处于1~6g/10分钟的范围。MFR处于上述的范围时,能够得到柔软性与机械強度的平衡优异、粘接力高的粘接剂。
作为乙烯系聚合物(D)的制造方法,没有特别限定,可以利用使用了高压法、齐格勒-纳塔催化剂、茂金属系催化剂等公知催化剂的公知方法进行制造。另外,只要是满足成型性、具有能够耐受形成成型体时的使用的强度的聚合物,对有规立构性、分子量就没有特别限制。也能够直接利用市售的树脂。乙烯系聚合物(D)只要满足上述条件,也可以是接枝了少量的马来酸酐等的聚合物。另外,只要满足上述条件,可以是在接枝了少量的马来酸酐等之后,进一步利用二胺、碳二亚胺等对接枝单体进行修饰而成的聚合物。
其他的成分
在本发明的树脂组合物中,在不损害本发明的效果的范围内,可以适当含有与本发明组成不同的丙烯-乙烯嵌段共聚物、丙烯均聚物、丙烯-乙烯无规共聚物、丙烯-乙烯-丁烯无规共聚物、苯乙烯系弹性体、聚乙烯等其他成分。其他成分在本发明的树脂组合物中所占的的比率优选为20质量%以下。
此外,根据需要,还可以含有抗氧化剂、紫外线吸收剂、中和剂、成核剂、光稳定剂、抗静电剂、防粘连剂、润滑剂、臭味吸附剂、抗菌剂、颜料、无机质和有机质的填充剂以及各种合成树脂等公知的添加剂。
树脂组合物
本发明的树脂组合物可以采用现有公知的方法进行制造。例如,可以通过将上述的各成分熔融混炼而制造。
关于本发明的树脂组合物中的丙烯系聚合物(A)、软质丙烯系共聚物(B)、聚烯烃(C)、乙烯系聚合物(D)的含量,将丙烯系聚合物(A)、软质丙烯系共聚物(B)、聚烯烃(C)、乙烯系聚合物(D)的含量的合计设为100质量份时,优选丙烯系聚合物(A)为35~59.9质量份、软质丙烯系共聚物(B)为25~40质量份、聚烯烃(C)为0.1~10质量份、乙烯系聚合物(D)为15~30质量份,更优选丙烯系聚合物(A)为35~55质量份、软质丙烯系共聚物(B)为25~35质量份、聚烯烃(C)为1~7质量份、乙烯系聚合物(D)为20~30。本发明的树脂组合物中的上述成分的含量为上述范围内时,粘接性、特别是低热量下的粘接性高,另外包含由本组合物得到的层的膜在变形加工时更不容易发生白化。
本发明的树脂组合物按照ASTM D-1238、以230℃、2.16kg负荷测得的MFR为7g/10分钟以上25g/10分钟以下,优选为8g/10分钟以上15g/10分钟以下。MFR为上述范围内时,即使在高速成型条件下进行膜成型,分子链的取向也容易得到松弛,能够抑制之后的变形加工时的白化。
在产生微细裂纹时,会引起变形加工时的白化。认为若在膜上产生微细裂纹,则在作为电池包装材料时绝缘性变差。
单层或多层膜
本发明的单层和多层膜是包含至少1层含有上述树脂组合物的层的单层或多层膜。即,本发明的单层膜为由含有上述树脂组合物的层构成的膜,多层膜为包含至少1层含有上述树脂组合物的层的多层膜。
本发明的单层和多层膜在变形加工时的耐白化性优异。因此,使用本发明的单层和多层膜作为食品包装材料或建筑用材料、锂离子电池的外装材料等时,在拉深加工、弯折等膜的二次加工时不容易发生白化。因此,本发明的单层和多层膜能够适合用作食品包装材料和建筑用材料、电池包装用膜。
特别而言,作为形成锂离子电池的外包装体的包装材料,虽然一直都在使用聚丙烯系树脂,但本发明通过使用前述的丙烯系聚合物(A)、软质丙烯系共聚物(B)、聚烯烃(C)和乙烯系聚合物(D)这样的特定的组合,实现了防止用现有的聚丙烯系树脂时一直没能避免的白化。
本发明的多层膜例如包含至少1层含有上述树脂组合物的层,另外,含有上述组合物的层的一面或两面与该多层膜所含的其他层相接触。作为与含有上述组合物的层相接触的其他层,例如可以列举含金属层、聚烯烃层和极性树脂层。作为含金属层,可以列举铝层、铜层、不锈钢层等,作为聚烯烃层,可以列举聚丙烯层、聚4-甲基戊烯层、聚乙烯层等,作为极性树脂层,可以列举聚酰胺层、EVOH层、PET层、PBT层等。
本发明的单层和多层膜能够通过熔融挤出成型而得到,能够利用通常在工业上进行的浇铸法、吹胀法、挤出层压法等制造。
实施例
以下,列举实施例和比较例,更具体地说明本发明,但是,本发明只要不超出其要点,就不受这些实施例的任何限制。
(各种测定方法)
本实施例等中,按照以下的方法实施测定。
[熔体流动速率(MFR)]
按照ASTM D1238,在230℃、2.16kg负荷下实施熔体流动速率测定。
[特性粘度[η]]
特性粘度[η]按照ASTM D1601测定。
[拉深成型后的耐白化性评价]
(拉深成型)
使用啮合深度5mm的模具,以速度200mm/min对实施例和比较例中得到的通常成型时和高速成型时的耐白化性评价用多层膜(聚丙烯层/粘接剂层/铝层)进行拉深成型。通过目测,依照下述基准对所得到的成型体的壁面所产生的白化的程度进行评价。
A:没有白化
B:稍微白化
C:明显白化
[粘接力]
将实施例和比较例中得到的粘接力测定用多层膜(铝层/粘接剂层/铝层)切成20mm宽度,使用拉伸试验机,利用180°剥离法,在室温23℃测定铝层与粘接剂层的粘接力(单位:N/20mm)。十字头速度设为200mm/min。
[聚合物的组成]
丙烯系共聚物中的源自丙烯的结构单元、源自α-烯烃的结构单元的含量通过13C-NMR、利用以下的装置和条件测定。
关于丙烯、α-烯烃含量的定量和全同立构三单元组分率(mm分率),使用日本电子株式会社制造的JECX400P型核磁共振装置,将氘代邻二氯苯/氘代苯(80/20容量%)混合溶剂作为溶剂,试样浓度为60mg/0.6mL,测定温度为120℃,观测核为13C(100MHz),序列(sequence)为单脉冲质子去偶(single pulse proton decoupling),脉冲宽度为4.62μ秒(45°脉冲),重复时间为5.5秒,累计次数为8000次,将29.73ppm作为化学位移的基准值而测定。
[熔点(Tm)、玻璃化转变温度(Tg)]
使用Seiko Instruments公司制造的DSC220C装置作为差示扫描量热计(DSC),测定熔点(Tm)、玻璃化转变温度(Tg)。将试样5~10mg密封于铝皿中而作为试样。关于温度曲线,以50℃/分钟从室温升温至230℃后,在230℃保持5分钟,接着以10℃/min降温至-80℃,在-80℃保持5分钟,再以10℃/min升温至230℃。从其第二次升温时的图得到熔点(Tm)和玻璃化转变温度(Tg)。
[分子量(Mn、Mw)、分子量分布(Mw/Mn)]
使用串联连接有东曹株式会社制造的TSKgelGMH6-HT×2根和TSKgelGMH6-HTL×2根(柱尺寸均为直径7.5mm、长度300mm)作为色谱柱的液相色谱(Waters制造的Alliance/GPC2000型),测定聚合物的分子量和分子量分布。流动相介质使用邻二氯苯和作为抗氧化剂的BHT(武田药品)0.025质量%,以试样浓度0.15%(V/W)、流速1.0mL/分钟、140℃进行测定。关于标准聚苯乙烯,对于分子量为500~20,600,000的标准聚苯乙烯,使用东曹公司制造的标准聚苯乙烯。使用Waters制造的数据处理软件Empower2,按照公知的方法,利用使用标准聚苯乙烯样品得到的标准曲线,解析所得到的色谱图,从而算出Mn、Mw和Mw/Mn。
(所使用的聚烯烃)
实施例和比较例中使用的聚烯烃如下所示。另外,只要没有特别限定,聚烯烃均利用通常方法进行聚合而制备。
丙烯系聚合物(A)
PP-1:无规聚丙烯
(丙烯96mol%、乙烯4mol%、Tm 140℃)
软质丙烯系共聚物(B)
PR-1:下述合成例1中合成的丙烯-α-烯烃共聚物
(源自1-丁烯的结构单元26mol%、源自丙烯的结构单元74mol%)
PR-2:下述合成例2中合成的丙烯-α-烯烃共聚物
(源自乙烯的结构单元14mol%、源自丙烯的结构单元86mol%)
聚烯烃(C)
改性PP-1:改性均聚丙烯
(马来酸酐接枝量3.0质量%、[η]0.4)
乙烯系聚合物(D)
EPR:乙烯-丙烯共聚物
(源自乙烯的结构单元80mol%、源自丙烯的结构单元20mol%、MFR3.0g/10分钟)
PE:低密度聚乙烯
(MFR2.8g/10分钟、密度0.92g/cm3)
(合成例1)[丙烯-α-烯烃共聚物(PR-1)的合成]
在常温向充分氮置换后的20L的聚合装置中加入8.7L的干燥己烷、1-丁烯900g和三异丁基铝(1.0mmol)后,将聚合装置内温升温至65℃,用丙烯加压至0.7MPa。接着将使二甲基亚甲基(3-叔丁基-5-甲基环戊二烯基)芴基二氯化锆0.002mmol与以铝换算计为0.6mmol的甲基铝氧烷(Tosoh Finechem制造)接触的甲苯溶液添加到聚合器内,一边保持内温65℃、丙烯压0.7MPa一边聚合30分钟后,添加20mL的甲醇,停止聚合。
在脱压后,在20L的甲醇中,使聚合物(丙烯-α-烯烃共聚物(PR-1))从聚合溶液析出,在真空下130℃干燥12小时。
丙烯-α-烯烃共聚物(PR-1)的质量为130g,丙烯含量为74摩尔%,丁烯含量为26摩尔%,熔点(Tm)为75℃,MFR(温度230℃、负荷2.16kg)为7g/10分钟,分子量分布(Mw/Mn)为2.1,全同立构三单元组分率(mm分率)为93%。重复进行上述操作,得到需要量的聚合物。
(合成例2)[丙烯-α-烯烃共聚物(PR-2)的合成]
利用与合成例1同样的方法,使用乙烯代替1-丁烯,除此以外,利用同样的方法进行合成,得到丙烯-乙烯共聚物(丙烯-α-烯烃共聚物(PR-2))。
丙烯-α-烯烃共聚物(PR-2)的丙烯含量为86mol%,乙烯含量为14mol%,熔点(Tm)为80℃,MFR(温度230℃、负荷2.16kg)为8g/10分钟,分子量分布(Mw/Mn)为2.2,全同立构三单元组分率(mm分率)为88%。
[实施例1]
使用单螺杆挤出机,以230℃对40质量份PP-1、30质量份PR-1、5质量份改性PP-1、15质量份EPR和10质量份PE进行熔融混炼,制备树脂组合物。将该组合物作为粘接剂1。
使用直径50mm、有效长度L/D为28的螺杆,以290℃将市售的聚丙烯(普瑞曼聚合物株式会社制造的F329RA、MFR:24)和粘接剂1共挤出。将挤出后的聚丙烯和粘接剂在供料块内以聚丙烯为外层、粘接剂为内层的方式进行叠层,制作外层和内层均为20μm的厚度约40μm的膜状的叠层体。模具温度为290℃。使该叠层体以溶融状态与铝箔(厚度20μm)表面接触后,一边利用带夹紧辊的冷却辊进行冷却,一边以50m/分钟的速度进行牵拉,得到通常成型时的耐白化性评价用多层膜(聚丙烯层/粘接剂层/铝层)。同样地,将上述叠层体以100m/分钟的速度进行牵拉,得到高速成型时的耐白化性评价用多层膜(聚丙烯层/粘接剂层/铝层)。
另外,利用带T模的挤出成型机,由粘接剂1成型为厚度50μm的膜。将所得到的膜夹在厚度300μm的2片铝箔中,利用热封机,在160℃、0.1MPa的条件下热封5秒钟,得到低热量粘接的粘接力测定用多层膜(铝层/粘接剂层/铝层)。同样地,在180℃、0.1MPa的条件下热封5秒钟,得到通常粘接的粘接力测定用多层膜(铝层/粘接剂层/铝层)。
[实施例2~4、比较例1~3]
在实施例2~4、比较例1~3中,分别按照表1所示的配方,利用与实施例1相同的方法制造了树脂组合物。将实施例2中得到的组合物作为粘接剂2,将实施例3中得到的组合物作为粘接剂3,将实施例4中得到的组合物作为粘接剂4,将比较例1中得到的组合物作为粘接剂5,将比较例2中得到的组合物作为粘接剂6,将比较例3中得到的组合物作为粘接剂7。使用各粘接剂,与实施例1同样地制造耐白化性评价用多层膜和粘接力测定用多层膜。
将实施例和比较例中得到的粘接剂的MFR和关于由该粘接剂制作的多层膜的粘接力以及耐白化性评价结果示于表1。
[表1]
Claims (9)
1.一种树脂组合物,其特征在于,含有:
满足下述(a)的丙烯系聚合物(A)35~59.9质量份,
满足下述(b)的软质丙烯系共聚物(B)25~40质量份,
含有来自不饱和羧酸和/或其衍生物的结构单元的聚烯烃(C)0.1~10质量份,和
满足下述(d)的乙烯系聚合物(D)15~30质量份,
其中,将(A)、(B)、(C)和(D)的合计设为100质量份,
所述树脂组合物按照ASTM D-1238、以230℃、2.16kg负荷测得的MFR为7g/10分钟以上25g/10分钟以下;
(a)在差示扫描量热测定中观测到的熔点(Tm)为120℃以上,
(b)按照ASTM D-1238、以230℃、2.16kg负荷测得的MFR处于0.01~100g/10分钟的范围,并且满足下述条件(b-1)和(b-2),
(b-1)在差示扫描量热测定中观测到的熔点(Tm)为110℃以下,或者观测不到熔点,
(b-2)具有源自丙烯的结构单元以及源自选自乙烯和碳原子数4~20的α-烯烃中的至少1种烯烃的结构单元,源自选自乙烯和碳原子数4~20的至少1种α-烯烃的结构单元的含量为30mol%以下,利用13C-NMR测得的全同立构三单元组分率(mm分率)为80%以上,
(d)为乙烯均聚物或乙烯与选自碳原子数3~20的α-烯烃中的至少1种α-烯烃的共聚物,其按照ASTM D-1238、以190℃、2.16kg负荷测得的MFR为0.1~10g/10分钟的范围。
2.如权利要求1所述的树脂组合物,其特征在于:
聚烯烃(C)含有以来自马来酸酐的结构单元换算计为0.01~5质量%的来自不饱和羧酸和/或其衍生物的结构单元,
并且,在聚烯烃(C)中,除所述来自不饱和羧酸和/或其衍生物的结构单元以外的结构单元中的来自丙烯的结构单元的含有比率为90~100摩尔%。
3.一种单层或多层膜,其特征在于:
包含至少1层含有权利要求1或2所述的树脂组合物的层。
4.一种多层膜,其特征在于:
包含至少1层含有权利要求1或2所述的树脂组合物的层和至少2层含有所述组合物的层以外的其他层,
含有所述组合物的层的两面与所述其他层相接触。
5.一种多层膜,其特征在于:
包含至少1层含有权利要求1或2所述的树脂组合物的层和至少1层选自含金属层、聚烯烃层和极性树脂层的层,
含有所述组合物的层与所述含金属层、聚烯烃层和极性树脂层中的至少1层相接触。
6.如权利要求3~5中任一项所述的单层或多层膜,其特征在于:
其是食品包装用膜。
7.如权利要求3~5中任一项所述的单层或多层膜,其特征在于:
其是建筑材料用膜。
8.如权利要求3~5中任一项所述的单层或多层膜,其特征在于:
其是电池包装用膜。
9.一种单层或多层膜的制造方法,其特征在于:
将权利要求1或2所述的树脂组合物熔融挤出成型。
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