CN108884365B - 热塑型粘接膜、粘接方法以及粘接体 - Google Patents

热塑型粘接膜、粘接方法以及粘接体 Download PDF

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CN108884365B
CN108884365B CN201780017574.1A CN201780017574A CN108884365B CN 108884365 B CN108884365 B CN 108884365B CN 201780017574 A CN201780017574 A CN 201780017574A CN 108884365 B CN108884365 B CN 108884365B
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resin
adhesive film
thermoplastics type
polypropylene
weight
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CN108884365A (zh
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齐藤诚法
浅野仁志
松田裕行
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Entrywood Corp
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Entrywood Corp
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Abstract

本发明的问题在于：提供一种热塑型粘接膜，特别是在用于汽车构件、电子构件以及建筑构件等的聚丙烯系树脂材料、聚酰胺系树脂材料以及铝或钢板等金属材料等异种材料层叠体的热粘接工序中，其可防止该树脂材料的变形，防止由成型后的热过程引起的剥离。作为解决方案，提供一种热塑型粘接膜，其包含含有热塑性烯烃弹性体系树脂(A)、酸改性聚丙烯系树脂(B)以及结晶成核剂(C)的树脂组合物(D)。

Description

热塑型粘接膜、粘接方法以及粘接体
技术领域
本发明涉及一种热塑型粘接膜。
背景技术
在将含有聚烯烃等熔点、软化点为较低温的树脂的成型品与其他构件粘接时，通常不使用热熔型粘接剂等在粘接时伴随加热的粘接剂。这是因为：根据粘接时的加热温度，含有聚烯烃树脂等的成型品可能会软化、变形。另外，在想要粘接的构件为重物的情况下，由于加热粘接后的冷却不充分，因此也有可能热熔型粘接剂无法充分地固化，无法承受构件的重量而导致构件剥离。
由此，使用溶液型、反应型的粘接剂来将这些成型品粘接，或者大胆地采用熔敷、粘合剂等方式进行粘接或者粘合。
另外，如专利文献1所述的那样，仅使用聚烯烃、用于加热粘接的膜状粘接剂是公知的。另外，如专利文献2所述的那样，形成含有酸改性聚烯烃树脂的层作为底漆层(primerlayer)，在该层上形成含有烯烃弹性体树脂的粘接剂层，这是公知的。进而，如专利文献3所述的那样，含有乙烯聚合物、α-烯烃系结晶性聚合物、嵌段共聚物以及马来酸接枝聚丙烯的层在聚烯烃层与阻隔层(barrier layer)之间作为粘接剂层发挥功能，这是公知的。
现有技术文献
专利文献
专利文献1：日本特表2000-512683号公报
专利文献2：日本特开2014-69516号公报
专利文献3：日本特表2015-531324号公报
发明内容
发明所要解决的问题
若使用具有通常的软化点的热熔粘接剂，则由于加热温度较高，因此在粘接聚烯烃树脂成型体时，该聚烯烃树脂成型体也可能因软化而变形。
另外，在将酸改性聚烯烃树脂设置为底漆层的情况下，最终需要与粘接剂层一起形成由两层以上的层构成的粘接剂层。
进而，为了制成仅含有酸改性聚丙烯、聚烯烃树脂的粘接膜，需要与被粘接物一起以共挤出等方式在高温下进行粘接。
用于解决问题的方案
本发明人为了解决所述问题而进行了深入的研究，其结果是发现了能通过以下的方案解决上述问题，从而完成了本发明。
1、一种热塑型粘接膜，其包含含有热塑性烯烃弹性体系树脂(A)、酸改性聚丙烯系树脂(B)以及结晶成核剂(C)的树脂组合物(D)。
2、根据1所述的热塑型粘接膜，其中，从树脂组合物(D)的180℃的熔融状态以应变1％、剪切速率100s-1、3℃/分钟进行冷却时的粘度上升开始温度T1和以应变1％、施加频率为1～100Hz的振动、10℃/分钟进行升温拉伸时的软化开始温度T2满足式(1)。
(T1/T2)≥0.90 式(1)
3、根据1或2所述的热塑型粘接膜，其中，从树脂组合物(D)的180℃的熔融状态以应变1％、剪切速率100s-1、3℃/分钟进行冷却时的150℃、应变1％、剪切速率100s-1时的复数粘度为600Pa·s以上10000Pa·s以下，并且120℃、应变1％、剪切速率100s-1时的复数粘度为4000Pa·s以上。
4、根据1～3中任一项所述的热塑型粘接膜，其中，树脂组合物(D)的由差示扫描量热仪测定的熔融焓为135J/g以下。
5、根据1～4中任一项所述的热塑型粘接膜，其中，树脂组合物(D)含有聚丙烯系树脂(E)。
6、根据1～5中任一项所述的热塑型粘接膜，其中，热塑性烯烃弹性体系树脂(A)与聚丙烯系树脂(E)的重量比[(A)/(E)]为100/0～10/90，[其中，(A)+(E)＝100]，在将(A)与(E)的总重量设为100重量份时，含有20～500重量份的酸改性聚丙烯系树脂(B)。
7、根据1～6中任一项所述的热塑型粘接膜，其中，酸改性聚丙烯系树脂(B)是使不饱和酸酐与无规共聚物聚丙烯共聚而形成的。
8、根据1～7中任一项所述的热塑型粘接膜，其中，树脂组合物(D)含有近红外线吸收性材料。
9、根据1～8中任一项所述的热塑型粘接膜，其中，树脂组合物(D)含有无机填料。
10、根据1～9中任一项所述的热塑型粘接膜，其中，树脂组合物(D)形成多层膜或片材的至少一方的表层面。
11、一种粘接方法，其使用1～10中任一项所述的热塑型粘接膜，使粘接聚丙烯系树脂被粘接体时的加热温度即粘接温度满足式(2)。
(被粘接体的熔融温度)＞(粘接温度)≥(酸改性聚丙烯系树脂(B)的熔融温度)－20 式(2)
其中，熔融温度是由差示扫描量热仪测定的数值。
12、一种粘接体，其是使用1～10中任一项所述的热塑型粘接膜将两个被粘接体相互粘接而成的粘接体，该两个被粘接体中的至少一个被粘接体包含聚丙烯系树脂材料或聚酰胺系树脂材料。
发明效果
根据本发明的热塑型粘接膜，对于聚丙烯系树脂材料或者聚酰胺系树脂材料，可在该树脂材料的变形温度以下进行粘接，也可以将与该树脂材料的性质不同的金属材料之类的异种原材料彼此粘接。
另外，在将被粘接体粘接的工序中，可抑制加热粘接时的热过程(thermalhistory)引起的固化不良导致的剥离，能够可靠地将聚丙烯系树脂材料或者聚酰胺系树脂材料彼此一体化、将所述树脂材料与金属材料之类的异种原材料的被粘接体彼此一体化。
附图说明
图1为表示粘度上升开始温度(T1)的图。
图2为表示软化开始温度(T2)的图。
具体实施方式
本发明的热塑型粘接膜的特征在于，包含含有热塑性烯烃弹性体系树脂(A)、酸改性聚丙烯系树脂(B)以及结晶成核剂(C)的树脂组合物(D)，从树脂组合物(D)的180℃的熔融状态以应变1％、剪切速率100s-1、3℃/分钟进行冷却时的粘度上升开始温度T1与以应变1％、施加频率为1～100Hz的振动、10℃/分钟进行升温拉伸时的软化开始温度T2之比(T1/T2)优选为0.90以上，进一步优选为0.97以上1.05以下。在小于0.90的情况下，可能无法在加热粘接后的冷却工序中充分地固化而发生被粘接体的剥离。
就本发明的热塑型粘接膜而言，优选的是，从树脂组合物(D)的180℃的熔融状态以应变1％、剪切速率100s-1、3℃/分钟进行冷却时的150℃、应变1％、剪切速率100s-1时的复数粘度为600Pa·s以上10000Pa·s以下。进一步优选的是，150℃、应变1％、剪切速率100s-1时的复数粘度为1000Pa·s以上9400Pa·s以下，最优选的是1200Pa·s以上5000Pa·s以下。在150℃、应变1％、剪切速率100s-1时的复数粘度小于600Pa·s的情况下，由于熔融粘度过低，因此有时因在加热粘接时从被粘接体溢出而无法得到充分的粘接强度。在150℃、应变1％、剪切速率100s-1时的复数粘度大于10000Pa·s的情况下，由于熔融粘度过高，因此有时对被粘接体的润湿变差，无法得到充分的粘接强度。
另一方面，120℃、应变1％、剪切速率100s-1时的复数粘度优选为4000Pa·s以上，进一步优选为10000Pa·s以上40000Pa·s以下。在120℃、应变1％、剪切速率100s-1时的复数粘度小于4000Pa·s的情况下，由于加热粘接后的冷却时的熔融粘度低，因此可能发生被粘接体的剥离。
为了能够在比聚丙烯系树脂材料或者聚酰胺系树脂材料的变形温度低的温度下进行粘接，需要对热塑型粘接膜的结晶性进行控制，树脂组合物(D)的由差示扫描量热仪测定的熔融焓优选为135J/g以下，进一步优选为100J/g以下，进一步优选为40J/g以下。在熔融焓超过135J/g的情况下，无法在比聚丙烯系树脂材料或者聚酰胺系树脂材料的熔融温度低的温度下得到充分的粘接强度。
以下对构成本发明的热塑型粘接膜的材料进行说明。
(热塑性烯烃弹性体系树脂(A))
作为本发明所使用的热塑性烯烃弹性体系树脂(A)，由差示扫描量热仪测定的熔融焓优选为35J/g以下。
这样的热塑性烯烃弹性体系树脂(A)可列举：在硬链段的聚合时使乙烯-丙烯橡胶、乙烯-丙烯-二烯橡胶的未交联体或者部分交联体作为软链段分散于聚丙烯的均聚体或者无规体的硬链段的类型(反应器型(reactor type))；在混炼时使聚丙烯的均聚体或者无规体的硬链段与乙烯-丙烯橡胶、乙烯-丙烯-二烯橡胶的未交联体或者部分交联体的软链段动态交联的类型；丙烯-丁烯共聚物、丙烯-乙烯-丁烯共聚物、丙烯-丁二烯共聚物、丙烯-乙烯-丁二烯共聚物、间规聚丙烯、α-烯烃共聚物等。作为上述热塑性烯烃弹性体系树脂，例如可列举：PRIME POLYMER制PRIME TPO、三菱化学制THERMORUN等。
作为热塑性烯烃弹性体系树脂(A)的配合量，在树脂组合物(D)中为1.5～90重量份，优选为10～70重量份，进一步优选为20～50重量份。在1.5～90重量份以外时，粘接力有时降低。
(酸改性聚丙烯系树脂(B))
本发明所使用的酸改性聚丙烯系树脂(B)可列举：丙烯或者丙烯-乙烯与马来酸酐、衣康酸、富马酸、油酸、丙烯酸、甲基丙烯酸等不饱和羧酸的共聚物，优选为丙烯-乙烯与马来酸酐的共聚物。作为上述酸改性聚丙烯系树脂(B)，例如可列举：DUPONT制FUSABOND、三洋化成制UMEX等。
作为酸改性聚丙烯系树脂(B)的配合量，相对于热塑性烯烃弹性体系树脂(A)或热塑性烯烃弹性体系树脂(A)与聚丙烯系树脂(E)的总量100重量份，优选为20～500重量份，进一步优选为50～300重量份。在小于20重量份时，粘接力有时降低。
(结晶成核剂(C))
作为本发明所使用的结晶成核剂(C)，可以使用对聚丙烯有效的公知的结晶成核剂，可列举：二亚苄基山梨糖醇衍生物、磷酸酯金属盐、苯甲酸金属盐、庚二酸金属盐、松香金属盐、喹吖啶酮、花青蓝、滑石、碳酸钙等。作为添加量，在树脂组合物(D)100重量份中，优选为0.01～1重量份。在为0.01～1重量份以外的添加量时，粘接力有时降低。作为上述结晶成核剂，可列举：新日本理化制GELALL、ADEKA制ADK STAB等。
就本发明的热塑型粘接膜而言，树脂组合物(D)可含有聚丙烯系树脂(E)，聚丙烯系树脂(E)可为均聚体或者无规体中的任一者。作为如此的聚丙烯系树脂，可列举：住友化学制SUMITOMO NOBLEN、JAPAN POLYPROPYLENE CORPORATION制NOVATEC PP。
在本发明的热塑型粘接膜含有聚丙烯系树脂(E)的情况下，热塑性烯烃弹性体系树脂(A)与聚丙烯系树脂(E)的重量比[(A)/(E)]优选为100/0～10/90[其中，(A)+(E)＝100]，进一步优选为90/10～20/80。在满足该条件的情况下，可在比聚丙烯系树脂材料或者聚酰胺系树脂材料的熔融温度低的温度下得到更高的粘接强度。另外，在将(A)与(E)的总重量设为100重量份时，酸改性聚丙烯系树脂(B)优选为20～500重量份。在为该范围的情况下，对于金属材料，可得到更高的粘接强度。
就本发明的热塑型粘接膜而言，可在树脂组合物(D)中含有碳黑、石墨烯、石墨、二亚胺(diimmonium)盐、铵盐、花青(cyanine)化合物、酞菁化合物、二硫醇金属络合物、萘醌化合物、偶氮化合物、滑石等近红外线吸收性材料，其结果是，可照射激光等红外线进行加热而进行粘接。
以提高本发明的热塑型粘接膜的刚性为目的，可在树脂组合物(D)中含有滑石、碳酸钙、海泡石、勃姆石、膨润土、二氧化硅、云母、氧化钛、氧化锌、玻璃珠、铝-镍-铜等金属纤维等无机填料。
可在本发明的热塑型粘接膜中添加或不添加增粘剂，在不需要粘合性的情况下，也可不添加。另外，也可添加或不添加各种交联剂、增塑剂。
可在包含本发明的树脂组合物(D)的热塑型粘接膜的单面设置基材层，制成多层膜或多层片材。
以调整本发明的热塑型粘接膜的弯曲强度、刚度(stiffness)、耐热性等物性、厚度为目的而采用该基材层，可以使用聚丙烯系树脂、聚对苯二甲酸乙二醇酯系树脂、聚酰胺系树脂。
(制造方法)
可通过公知的熔融挤出成型得到本发明的热塑型粘接膜，可使树脂组合物(D)从T模头、圆形模(circular die)等挤出/冷却固化来形成膜或片材。另外，以提高热塑型粘接膜的表面润湿性为目的，可在热塑型粘接膜表面上实施电晕放电处理、等离子体放电处理、UV/臭氧处理、火焰处理等。
(粘接方法)
就本发明的热塑型粘接膜而言，在被粘接体例如为聚丙烯系树脂等热塑性树脂的情况下，通过将粘接时的加热温度即粘接温度设为(热塑性树脂的熔融温度)＞(粘接温度)≥(酸改性聚丙烯系树脂的熔融温度)－20(其中，熔融温度是由差示扫描量热仪测定的数值)，可抑制被粘接体的变形而进行粘接。
(用途)
作为本发明的热塑型粘接膜的用途，没有特别限制，可用于将两个被粘接体相互粘接而得到粘接体的用途。
作为此时的被粘接体，可选择包含树脂、木材、金属、纸、玻璃、陶器、陶瓷、纺布以及无纺布等任意材料的被粘接体。
其中，该两个被粘接体的材料的至少一者优选为树脂，在两个材料均为树脂的情况下，可为各种热塑性树脂彼此的组合、各种热/能量射线固化性树脂彼此的组合、热塑性树脂与热/能量射线固化性树脂的组合中的任一者，特别是可以将该两个被粘接体中的至少一方的被粘接体采用聚丙烯系树脂材料或聚酰胺系树脂材料。在一方的被粘接体为树脂的情况下，该树脂可为热塑性树脂以及热/能量射线固化性树脂中的任一者。
另外，可作为用于制作汽车用内饰件、鞋子、凉鞋等鞋类、家具、智能手机/平板终端/PC的壳体、家电壳体等各种用途的成型品的粘接材料进行使用。
实施例
以下，列举实施例来对本发明进行更具体的说明。
需要说明的是，实施例表示发明的一个方案，本发明并不限于此。
(实施例1～4)
以表1所示的比例，将热塑性烯烃弹性体系树脂(TPO1)(PRIME POLYMER制、PRIMETPOR110E、熔融焓6J/g)以及酸改性聚丙烯系树脂(MPP1)(DuPont制、FUSABOND DPA50E806、熔融温度140℃、无规PP)的总重量设为100重量份，通过LABO PLASTO MILL(东洋精机制)将0.2重量份的结晶成核剂(C1)(ADEKA制、ADK STABNA-21、磷酸酯金属盐系)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(实施例5～7)
以表1所示的比例，将热塑性烯烃弹性体系树脂(TPO1)以及酸改性聚丙烯系树脂(MPP2)(三井化学制、ADMER QE060、熔融温度140℃、无规PP)的总重量设为100重量份，通过LABO PLASTO MILL(东洋精机制)将0.2重量份的结晶成核剂(C2)(新日本理化制、GELALL-D、二亚苄基山梨糖醇衍生物系)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(实施例8～13)
以表1所示的比例，将热塑性烯烃弹性体系树脂(TPO2)(三菱化学制、THERMORUN3707N、熔融焓34J/g)、酸改性聚丙烯系树脂(MPP1)以及聚丙烯系树脂(PP1)(住友化学制、NOBLEN S131、无规PP)的总重量设为100重量份，通过LABO PLASTO MILL(东洋精机制)将0.2重量份的结晶成核剂(C1)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(实施例14～19)
以表1所示的比例，将热塑性烯烃弹性体系树脂(TPO2)、酸改性聚丙烯系树脂(MPP1)以及聚丙烯系树脂(PP2)(JAPAN POLYPROPYLENE CORPORATION制、NOVATEC EA9、均聚PP)的总重量设为100重量份，通过LABO PLASTO MILL(东洋精机制)将0.05重量份的结晶成核剂(C2)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(实施例20～25)
以表1所示的比例，将热塑性烯烃弹性体系树脂(TPO1)、酸改性聚丙烯系树脂(MPP1)以及聚丙烯系树脂(PP1)(住友化学制、NOBLEN S131、无规PP)的总重量设为100重量份，通过LABO PLASTO MILL(东洋精机制)将0.2重量份的结晶成核剂(C1)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(实施例26～31)
以表1所示的比例，将热塑性烯烃弹性体系树脂(TPO1)、酸改性聚丙烯系树脂(MPP1)以及聚丙烯系树脂(PP1)(住友化学制、NOBLEN S131、无规PP)的总重量设为100重量份，通过LABO PLASTO MILL(东洋精机制)将0.8重量份的结晶成核剂(C1)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(实施例32～37)
以表1所示的比例，将热塑性烯烃弹性体系树脂(TPO1)、酸改性聚丙烯系树脂(MPP1)以及聚丙烯系树脂(PP2)(JAPAN POLYPROPYLENE CORPORATION制、NOVATEC EA9、均聚PP)的总重量设为100重量份，通过LABO PLASTO MILL(东洋精机制)将0.2重量份的结晶成核剂(C2)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(实施例38)
以表1所示的比例，将热塑性烯烃弹性体系树脂(TPO1)以及酸改性聚丙烯系树脂(MPP1)以及聚丙烯系树脂(PP1)的总重量设为100重量份，通过LABO PLASTO MILL(东洋精机制)将0.2重量份的结晶成核剂(C1)以及0.5重量份的碳黑CB(ASAHI CARBON CO.，LTD.制、ASAHI#15HS)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(实施例39)
以表1所示的比例，将热塑性烯烃弹性体系树脂(TPO1)以及酸改性聚丙烯系树脂(MPP1)以及聚丙烯系树脂(PP1)的总重量设为100重量份，通过LABO PLASTO MILL(东洋精机制)将0.2重量份的结晶成核剂(C1)以及10重量份的滑石(IMERYS SPECIALTIES JAPANCO.,LTD.制、SOAPSTONE A)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(实施例40)
通过热板压力机(神藤金属工业所制)将聚酰胺系树脂(PA1)(BASF制、ULTRAMIDB4、PA6)以300℃、10MPa进行熔融压制，得到了膜1。另外，将热塑性烯烃弹性体系树脂(TPO1)、酸改性聚丙烯系树脂(MPP3)(三菱化学制、MODIC P502、熔融温度165℃、均聚PP)以及聚丙烯系树脂(PP1)的总重量(相对于将TPO1/PP1＝50/50设为100重量份，MPP3设为50重量份)设为100重量份，通过LABO PLASTO MILL(东洋精机制)将0.2重量份的结晶成核剂(C1)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了膜2。通过热板压力机以膜1/膜2＝2/1的方式对膜1以及膜2以170℃、10MPa进行熔融压制，得到了厚度80μm的多层膜。
(比较例1)
以表1所示的比例，通过LABO PLASTO MILL(东洋精机制)将热塑性烯烃弹性体系树脂(TPO1)以及聚丙烯系树脂(PP1)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(比较例2)
以表1所示的比例，将酸改性聚丙烯系树脂(MPP1)设为100重量份，通过LABOPLASTO MILL(东洋精机制)将0.2重量份的结晶成核剂(C1)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(比较例3)
以表1所示的比例，将酸改性聚丙烯系树脂(MPP2)(三井化学制、ADMER QE060)设为100重量份，通过LABO PLASTO MILL(东洋精机制)将0.2重量份的结晶成核剂(C1)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(比较例4以及8)
以表1所示的比例，将聚丙烯系树脂(PP2)以及酸改性聚丙烯系树脂(MPP1)的总重量设为100重量份，通过LABO PLASTO MILL(东洋精机制)将0.2重量份的结晶成核剂(C2)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(比较例5～7)
以表1所示的比例，将聚丙烯系树脂(PP1)以及酸改性聚丙烯系树脂(MPP1)的总重量设为100重量份，通过LABO PLASTO MILL(东洋精机制)将0.2重量份的结晶成核剂(C2)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(比较例9)
以表1所示的比例，通过LABO PLASTO MILL(东洋精机制)将酸改性聚丙烯系树脂(MPP1)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(比较例10)
以表1所示的比例，通过LABO PLASTO MILL(东洋精机制)将酸改性聚丙烯系树脂(MPP2)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(比较例11)
以表1所示的比例，通过LABO PLASTO MILL(东洋精机制)将聚丙烯系树脂(PP1)以及酸改性聚丙烯系树脂(MPP1)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(比较例12)
以表1所示的比例，通过LABO PLASTO MILL(东洋精机制)将聚丙烯系树脂(PP2)以及酸改性聚丙烯系树脂(MPP1)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(比较例13)
以表1所示的比例，通过LABO PLASTO MILL(东洋精机制)将聚丙烯系树脂(PP2)、热塑性烯烃弹性体系树脂(TPO1)以及酸改性聚丙烯系树脂(MPP1)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(比较例14～16)
以表1所示的比例，通过LABO PLASTO MILL(东洋精机制)将聚丙烯系树脂(PP1)、热塑性烯烃弹性体系树脂(TPO1)以及酸改性聚丙烯系树脂(MPP1)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了厚度80μm的热塑型粘接膜。
(比较例17)
通过热板压力机(神藤金属工业所制)将聚酰胺系树脂(PA1)以300℃、10MPa进行熔融压制，得到了膜1。另外，将热塑性烯烃弹性体系树脂(TPO1)以及聚丙烯系树脂(PP1)的总重量设为100重量份，通过LABO PLASTO MILL(东洋精机制)将0.2重量份的结晶成核剂(C1)以200℃、50rpm混炼5分钟，通过热板压力机(神藤金属工业所制)对得到的树脂组合物以200℃、10MPa进行熔融压制，得到了膜2。通过热板压力机以膜1/膜2＝2/1的方式对膜1以及膜2以170℃、10MPa进行熔融压制，得到了厚度80μm的多层膜。
[表1]
＜粘度上升开始温度测定＞
针对实施例1～40以及比较例1～17的各样品，使用粘弹性测定装置(ANTON PAAR公司制)，以应变1％、剪切速率100s-1、冷却速度3℃/分钟的条件，将180℃设为开始温度，对冷却至100℃时的复数粘度进行了测定。将复数粘度急剧上升的点设为粘度上升开始温度(T1)(图1)。
＜软化开始温度测定＞
针对实施例1～40以及比较例1～17的各样品，使用动态粘弹性测定装置(ITKeisoku Seigyo CO.,LTD.制)，以应变1％、频率1以及100Hz、升温速度10℃/分钟的条件，将25℃设为开始温度，对储能模量进行了测定。将储能模量急剧减少的点设为软化开始温度(T2)(图2)。
＜复数粘度测定＞
针对实施例1～40以及比较例1～17的各样品，使用粘弹性测定装置(ANTON PAAR公司制)，以应变1％、剪切速率100s-1、冷却速度3℃/分钟的条件，将180℃设为开始温度，对120℃以及150℃的复数粘度进行测定。
＜差示扫描量热仪＞
针对实施例1～40、比较例1～17以及热塑性烯烃弹性体系树脂(TPO1以及TPO2)的各样品，通过差示扫描量热仪(TA Instruments制)以升温速度10℃/分钟、冷却速度10℃/分钟的条件实施了升温-冷却-再升温，根据在实施升温-冷却-再升温时的再升温时的吸热峰的面积求出熔融焓。另外，针对酸改性聚丙烯系材料(MPP1、MPP2以及MPP3)，根据以所述条件实施再升温时的吸热峰求出熔融温度。
＜粘接剥离试验＞
参照JIS K 6850的试验片制作方法，对于厚度1.6mm、宽度20mm的电镀锌钢板(SEHC)和厚度3mm、宽度20mm的聚丙烯板(PP)，在各自的材料之间插入实施例1～39以及比较例1～16的各样品，使用热板压力机(神藤金属工业所制)，以压制温度150℃、压制载荷0.27kN、压制时间120s、粘接面积70以及40mm2的条件进行粘接，分别制作了试验片。实施例40以及比较例17的样品以上述条件进行粘接，以使膜2侧与SEHC侧相接，制作了试验片。在载荷解除30s后，将SEHC面设为下侧，以可动距离50mm进行往复上下运动，对自重引起的SEHC与PP之间的剥离进行观察。
○：在往复上下运动10次以内不剥离
×：在往复上下运动10次以内剥离
＜粘接强度测定1＞
参照JIS K 6850，对拉伸剪切粘接强度进行了测定。详细条件如下所示。
被粘接体：聚丙烯板(PP)(厚度3.0mm、宽度20mm、熔融温度165℃)
聚酰胺66板(PA66)(厚度3.0mm、宽度20mm、熔融温度265℃)
粘接构成：1-1PP/实施例1～39以及比较例1～16的样品/PP
1-2PA66/实施例40以及比较例17的样品(膜2侧为PA66侧)
粘接方法：使用热板压力机(神藤金属工业所制)，以压制温度130℃、150℃以及170℃、压制载荷0.27kN、压制时间120s、粘接面积150mm2进行粘接。
测定：在23℃环境下静置一天后，对通过拉伸试验机(岛津制作所制)以500mm2/分钟的速度进行拉伸时的拉伸剪切粘接强度进行评价。
粘接性评价
粘接构成1-1：○被粘接体破坏或者热塑型粘接膜内聚破坏(cohesive failure)
×界面剥离
粘接构成1-2：○无膜1/膜2的界面剥离，被粘接体破坏或者热塑型粘接膜内聚破坏
×膜1/膜2的界面剥离或者热塑型粘接膜/PA66的界面剥离
被粘接体的变形评价
粘接构成1-1：目测观察PP的变形
○无变形 ×有变形
粘接构成1-2：目测观察PA66或膜1侧的变形
○无变形×有变形
＜粘接强度测定2＞
参照JIS K 6850，对拉伸剪切粘接强度进行了测定。详细条件如下所示。
被粘接体：电镀锌钢板(SEHC)(厚度1.6mm、宽度20mm)
聚丙烯板(PP)(厚度3.0mm、宽度20mm、熔融温度165℃)
粘接构成：2-1SEHC/实施例1～39以及比较例1～16的样品/PP
2-2SEHC/实施例40以及比较例17的样品(膜2侧为SEHC侧)
粘接方法：使用热板压力机(神藤金属工业所制)，以压制温度150℃、压制载荷0.27kN、压制时间120s、粘接面积150mm2进行粘接。
测定：在23℃环境下静置一天后，对通过拉伸试验机(岛津制作所制)以500mm2/分钟的速度进行拉伸时的拉伸剪切粘接强度进行评价。
粘接性评价
粘接构成2-1：○被粘接体破坏或者热塑型粘接膜内聚破坏
×界面剥离
粘接构成2-2：○无膜1/膜2的界面剥离，被粘接体破坏或者热塑型粘接膜内聚破坏
×膜1/膜2的界面剥离或者热塑型粘接膜/SEHC的界面剥离
被粘接体的变形评价
粘接构成2-1：目测观察PP的变形
○无变形 ×有变形
粘接构成2-2：目测观察膜1侧的变形
○无变形 ×有变形
＜评价结果＞
将针对实施例1～40以及比较例1～17的各样品的各评价结果示于表2以及表3。
[表2]
[表3]
本发明的热塑型粘接膜示出：可将聚丙烯系材料与金属材料粘接，可在刚进行热压粘接后抑制自重引起的剥离，此时的粘接破坏形态为内聚破坏或者被粘接体破坏。根据表2的结果示出：将对每单位粘接面积施加的重量换算为每1m2时，可耐受高达1500kg的自重。另外，示出：即使在比聚丙烯被粘接体的熔融温度低35℃的130℃，也不会使被粘接体变形，可进行粘接破坏形态为热塑型粘接膜的内聚破坏或者被粘接体破坏的粘接。
产业上的可利用性
特别是，本发明的热塑型粘接膜可通过热板压制、超声波、高频、激光等的加热/加压，以不损害聚丙烯、聚酰胺等树脂材料的形状的方式，与钢板、铝等金属材料进行粘接，另外，即使在刚进行热压、注塑成型等加热/加压成型后取出粘接体，也可抑制自重引起的剥离。因此，不需要加热/加压后的冷却工序，可利用于汽车、汽车用内饰件/外饰件(automotive interior and exterior parts)、建材零件、智能手机/家电壳体以及零件的粘接成型。

Claims (9)

1.一种热塑型粘接膜，其包含含有热塑性烯烃弹性体系树脂(A)、酸改性聚丙烯系树脂(B)、结晶成核剂(C)以及聚丙烯系树脂(E)的树脂组合物(D)，
结晶成核剂(C)从二亚苄基山梨糖醇衍生物、磷酸酯金属盐、苯甲酸金属盐、松香金属盐、花青蓝、滑石、碳酸钙中选择，
热塑性烯烃弹性体系树脂(A)与聚丙烯系树脂(E)的重量比(A)/(E)为100/0～10/90，其中，(A)+(E)＝100，在将(A)与(E)的总重量设为100重量份时，含有20～500重量份的酸改性聚丙烯系树脂(B)，
从树脂组合物(D)的180℃的熔融状态以应变1％、剪切速率100s-1、3℃/分钟进行冷却时的粘度上升开始温度T1和以应变1％、施加频率为1～100Hz的振动、10℃/分钟进行升温拉伸时的软化开始温度T2满足式(1)，
(T1/T2)≥0.90 式(1)。
2.根据权利要求1所述的热塑型粘接膜，其中，
从树脂组合物(D)的180℃的熔融状态以应变1％、剪切速率100s-1、3℃/分钟进行冷却时的150℃、应变1％、剪切速率100s-1时的复数粘度为600Pa·s以上10000Pa·s以下，并且120℃、应变1％、剪切速率100s-1时的复数粘度为4000Pa·s以上。
3.根据权利要求1所述的热塑型粘接膜，其中，
树脂组合物(D)的由差示扫描量热仪测定的熔融焓为135J/g以下。
4.根据权利要求1所述的热塑型粘接膜，其中，
酸改性聚丙烯系树脂(B)是使不饱和酸酐与无规共聚物聚丙烯共聚而形成的。
5.根据权利要求1所述的热塑型粘接膜，其中，
树脂组合物(D)含有近红外线吸收性材料。
6.根据权利要求1所述的热塑型粘接膜，其中，
树脂组合物(D)含有无机填料。
7.根据权利要求1～6中任一项所述的热塑型粘接膜，其中，
树脂组合物(D)形成多层膜或片材的至少一方的表层面。
8.一种粘接方法，其使用权利要求1～7中任一项所述的热塑型粘接膜，使粘接聚丙烯系树脂被粘接体时的加热温度即粘接温度满足式(2)，
(被粘接体的熔融温度)＞(粘接温度)≥(酸改性聚丙烯系树脂(B)的熔融温度)－20 式(2)
其中，熔融温度是由差示扫描量热仪测定的数值。
9.一种粘接体，其是使用权利要求1～7中任一项所述的热塑型粘接膜将两个被粘接体相互粘接而成的粘接体，该两个被粘接体中的至少一个被粘接体包含聚丙烯系树脂材料或聚酰胺系树脂材料。
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