CN1106424C - 适合于可射频热合的片材和薄膜的聚烯烃组合物 - Google Patents

适合于可射频热合的片材和薄膜的聚烯烃组合物 Download PDF

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CN1106424C
CN1106424C CN95107539A CN95107539A CN1106424C CN 1106424 C CN1106424 C CN 1106424C CN 95107539 A CN95107539 A CN 95107539A CN 95107539 A CN95107539 A CN 95107539A CN 1106424 C CN1106424 C CN 1106424C
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R·马佐拉
L·施坎纳温尼
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Abstract

本发明涉及能产生显著的介电热的聚烯烃组合物，它包含(重量百分数)：(I)85-97%多相烯烃聚合物，它可任选地被所述多相烯烃聚合物的0.3-0.03%的极性单体改性；和(II)3-15%至少一种介电热损耗因子大于或等于0.01的聚合物。

Description

适合于可射频热合的片材和薄膜 的聚烯烃组合物
本发明涉及适合于制备可用射频产生的介电热热合的片材和薄膜的聚烯烃组合物。
已公开的欧洲专利申请472946描述了一种聚烯烃组合物，其特征包括挠性强(挠曲模量低于150MPa)，它包含结晶丙烯均聚物或共聚物和一定量的在环境温度可溶于二甲苯的弹性体型烯烃共聚物，所述弹性体型烯烃共聚物含有低于40％(重量)的乙烯并具有1.5-4dl/g的特性粘度。
美国专利5300365指出上述组合物适于制备基本上无凝胶微粒并且具极佳物理-机械性质的片材和薄膜。
采用射频介电热封合塑性材料例如乙烯基聚合物、聚酰胺、聚酯和聚氨酯的片材或薄膜在本领域是个公知的方法。此方法称为射频热合法，它包括将两片或两片以上上述材料的片材或薄膜的一部分置于被施以电势差而在射频(1-200MHz)下振荡的两个电极之间，同时对欲封合的片材或薄膜部分施加压力。如此产生的热使聚合物片材或薄膜的接触部分熔融，而使这部分粘着并封合。然而该方法不能用于将由烯烃聚合物制得的片材或薄膜相互封合，因为这样的聚合物一般在射频下在电磁场中几乎不产生介电热。
事实上，聚烯烃薄膜或片材一般通过将外部热直接施加到需封合的部分而予以热合。然而与射频设备的热合周期和由此获得的封口相比，此热合周期较长，而且如此获得的封口不均匀且质量差。
因此，获得具有基本上与上述公开的欧洲专利申请472946中所述的组合物相同的物理一机械性质(特别是挠性)并能转变成可用射频产生的介电热封合的片材的薄膜是非常有益的。
本发明提供通过将上述欧洲专利申请472946中所述类型的组合物与少量的至少一种能通过吸收射频电磁辐射发出热的聚合物熔融共混获得的组合物。
本发明聚烯烃组合物包括(重量百分数)：
(I)85-97％、优选90-95％、更优选92-95％的多相烯烃聚合物，包括
A)5-50％的结晶丙烯均聚物、丙烯和乙烯的结晶共聚物、丙烯、乙烯和CH2＝CHRα-烯烃的结晶共聚物或其共混物，其中R是C2-C8烷基，所述共聚物含大于85％的丙烯；
B)0-20％乙烯与丙烯或与CH2＝CHRα-烯烃或与这两者的结晶共聚物部分，其中R是C2-C8烷基，所述部分在环境温度不溶于二甲苯中；
C)40-95％乙烯与丙烯或与CH2＝CHRα-烯烃或与这两者连同可任选的少量二烯烃的弹性体型共聚物部分，其中R是C2-C8烷基，所述共聚物部分中乙烯含量小于40％、优选20-38％，并在环境温度可溶于二甲苯中；
所述的多相烯烃聚合物可任选地用至少一种该多相烯烃聚合物的0.03-0.3％、优选0.05-0.2％的极性单体改性；和
(II)3-15％、优选5-10％、更优选5-8％的至少一种介电热损耗因子至少为0.01的聚合物。
上述聚烯烃组合物可转变成能用射频产生的介电热封合并且尽管存在附加成分(II)仍无凝胶微粒和表面不平整的片材和薄膜。此外，所述组合物具有与公开的欧洲专利申请472946中所述的组合物完全相同的物理-机械性质，特别是挠性。因此，由本发明组合物获得的片材和薄膜特别可用于包装用途以及其它需要高挠性、软度和可介电热合性的用途。
多相烯烃聚合物(I)的实例在公开的欧洲专利申请472946(相应于U.8.申请序号734390，1991年7月23日申请，本文参考引用了其内容)中有述。
乙烯在多相共聚物(I)中的总量例如可以为15-35％(重量)。此外，部分(C)的特性粘度一般为1.5-4dl/g。
部分(B)中乙烯的量优选至少为(B)总重量的75％(重量)，更优选至少为(B)总重量的80％(重量)。
可存在于多相共聚物(I)中的R是C2-C8烷基的CH2＝CHRα烯烃的实例是1-丁烯、1-戊烯、4-甲基-1-戊烯、1-己烯和1-辛烯。
(I)的部分(C)中若存在二烯烃单元，其含量最好为(C)总重量的1-10％(重量)。二烯烃的实例是丁二烯、1，4-己二烯、1，5-己二烯和乙烯-1-降冰片烯。
上述多相烯烃聚合物(I)可通过将部分(A)、(B)和(C)在高于其软化点或熔点的温度以流态熔融共混或者在高度立体专一性的Ziegler-Natta催化剂存在下经两步或多步顺序聚合来制备。
顺序聚合法的实例见公开的欧洲专利申请472946(相应于U.S.申请序号734390，1991年7月23日申请，本文参考引用了其内容)。当多相烯烃聚合物(I)采用顺序聚合法来制备时，部分(B)的含量大于或等于1％(重量)。当所述的部分(B)存在时，(B)/(C)重量比最好小于0.4。还优选的是，部分(C)或部分(B)和(C)之和的重量百分数为多相烯烃聚合物(I)的50-90％，优选65-80％。
多相烯烃聚合物(I)一般在120℃以上的温度例如130-150℃具有至少一个熔融峰(示差扫描量热法(DSC)测定)并在-10--35℃温度具有至少一个与玻璃化转变温度相对应的塑化峰。
此外，所述的多相烯烃聚合物的挠曲模量低于150MPa，而且在-50℃的艾佐德中击试验过程中不断裂。优选存在于多相烯烃聚合物
(I)中的其它性质是屈服点为3-20MPa，拉伸强度为10-20MPa，断裂伸长率大于300％，伸长率为75％时的拉伸变形为20-50％，以及ShoreD硬度为20-35。
多相烯烃聚合物(I)可以采用多种方法用至少一种极性单体予以改性。例如，可通过使用自由基引发剂例如有机过氧化物按照已知方法例如美国专利4350197和4568428中所述的方法将至少一种极性单体接枝到丙烯聚合物主链上。然后将如此获得的改性丙烯聚合物(以下称作“改性聚合物”)在熔融态与多相烯烃聚合物(I)共混。但最好将丙烯聚合物以颗粒形式即粉末、薄片、球形颗粒的形式用极性单体和自由基引发剂按公开的欧洲专利申请572028(相应于U.S.申请序号68012，1993年5月27日申请，本文参考引用了其内容)所述处理。在此情况下，同样将如此获得的改性聚合物在熔融态与多相烯烃聚合物(I)共混。
在这两种情况下，极性单体的量一般均为该改性聚合物总重量的0.05-30％(重量)、优选0.02-10％(重量)，而自由基引发剂(优选有机过氧化物)的量为该改性聚合物总重量的0.008-6％(重量)，优选0.04-2％(重量)。
用于制备所述改性丙烯聚合物的丙烯聚合物可以是关于多相烯烃聚合物(I)所述的部分(A)、(B)和(C)之一或其混合物。但用于制备所述改性丙烯聚合物的丙烯聚合物在改性前不必与含在多相烯烃聚合物(I)中的部分之一相同。最好是，该丙烯聚合物具有与部分(A)相同的类型、或者是与多相烯烃聚合物(I)相同的类型的多相烯烃聚合物，即包含部分(A)、(C)和可任选的(B)。
在任何情况下，通过细心选择加至多相烯烃聚合物(1)中的上述改性聚合物的量，都能获得用极性单体改性的并具有上述组成的多相烯烃聚合物(I)。
还可以将极性聚合物和自由基引发剂直接与多相烯烃聚合物(I)在熔融态混合。所述在熔融态的混合步骤按照任何公知技术进行，最好在惰性气氛中例如在氮气下用常规设备例如密闭式混合机或者单或双螺杆挤出机来进行。混合温度优选180-220℃。
极性单体的实例是马来酸酐、丙烯酸、甲基丙烯酸、丙烯酸酯类、甲基丙烯酸酯类、丙烯腈、甲基丙烯腈、马来酸、富马酸、乙烯基氯或乙酸乙烯酯。优选的极性单体是马来酸酐。
自由基引发剂的实例是过氧化苯甲酰、过氧化二叔丁基、过氧化二枯基、过苯甲酸叔丁酯、2，5-二甲基-2，5-二(过氧化叔丁基)己烷、2，5-二甲基-2，5-二(过氧化叔丁基)-3-己炔和偶氮二异丁腈。
关于组分(II)，介电热损耗因子是个无量纲量，它等于聚合材料的介电常数与所述聚合材料的损耗因子之乘积。聚合物损耗因子是被聚合材料转变成热的吸收能量的部分的函数。
介电热损耗因子至少为0.01的聚合物的实例包括聚酰胺、乙烯基聚合物、聚酯和聚氨酯。优选聚酰胺。特别优选的是选自数均分子量大于或等于1000、最好大于或等于5000、一般为10000-30000的结晶或无定形聚合物的聚酰胺。
所述聚酰胺例如可以由以下方法获得：a)将具有4-12个碳原子的羧酸与具有4-14个碳原子的二胺缩聚；或b)将具有6-12个碳原子的环状内酰胺聚合。
聚酰胺的具体实例包括尼龙6(聚己内酰胺)、66，69、610或612，或六亚甲基二胺，己二酸和邻苯二酸和对苯二酸的缩聚物或其混合物。
一般来讲，聚合物(II)最好以直径为0.05-0.7微米(电子显微镜测定)的分散粒子形式存在于本发明组合物中。所述粒子通常是球状。
除以上成分外，本发明组合物还可含有在聚合材料中常用的添加剂，例如稳定剂，颜料和填充剂。
为获得本发明组合物，将组分(I)和(II)以及可任选使用的添加剂按照任何公知技术熔融共混，即聚合物处于熔融状态，最好在惰性气氛例如在氮气下进行。这样的共混可以通过使用常规设备例如密闭式混合机(例如Banbury)或者单或双螺杆挤出机(例如Buss)来完成。熔融共混的温度最好为190-250℃。
一般来讲，本发明组合物的挠曲模量小于或等于250MPa，且shoreD硬度小于40。
如前所述，本发明组合物可容易地用于制造片材和薄膜。
这里所说的薄膜是厚度小于100微米的片坯，而片材是指厚度大于或等于100微米的片坯。片材和薄膜均可以是单或多层。多层薄膜和片材通常是指层压制品。所述单层薄膜或片材或者多层薄膜或片材的至少一层包含本发明组合物。在多层片材或薄膜的情况下，不包含本发明组合物的层可以包含烯烃聚合物例如聚乙烯或聚丙烯均聚物。一般来讲，上述片材和薄膜可以采用已知技术例如挤塑和压延来制备。
在将这样的片材和薄膜射频热合时，最好将电极在40-100℃的温度预热。
下列实施例用于举例说明本发明，但对本发明无限制。
为获得实施例和说明书中报告的性质数据所使用的方法见下文。对于需要模塑试样的试验方法，试样得自将待测定组合物用注压机在150-180℃模塑而成的170×70×3mm板材。上述试样是沿平行于板材的聚合物合流线的方向切割的。
 性质                  方法-熔体流动速率(M.F.R.)    ASTM-D1238 Condition L-乙烯重量百分数          I.R.光谱法-特性粘度                在四氢化萘中于135℃测定-二甲苯可溶部分          (下见注)-拉伸强度                ASTM D-638一断裂伸长率             ASTM D-638-维卡(1kg)               ASTM D-1525-硬度(Shore D)           ASTM D-2240-23℃时的挠曲模量        ASTM D-790-压缩变形                ASTM D-395，方法B注：二甲苯可溶部分的百分数的测定
制备浓度为1％(重量)的样品在二甲苯中的溶液并将其于135搅拌1小时。
使溶液冷却至95℃，同时搅拌，然后将其倒至25℃的恒温槽中，静置20分钟，搅拌10分钟。然后将溶液过滤，将丙酮加至等分的滤液中使溶于其中的聚合物沉淀析出。将如此获得的聚合物回收，洗涤、干燥并称重，以测定二甲苯可溶物的重量。
实施例
本实施例举例说明本发明的烯烃聚合物组合物、其制备方法、该组合物的片材和封合该片材的实施方案。
将97％(重量)的未改性的多相烯烃聚合物(I)与3％(重量)的改性聚合物在氮气氛中于200℃在Brabender单螺杆挤出机中熔融共混。
所述多相烯烃聚合物为球状颗粒，平均直径为2.5mm，并具有以下部分(重量百分数)：A)32％含约4％乙烯的结晶丙烯/乙烯共聚物，B)3％基本上是线型的乙烯/丙烯共聚物，在环境温度下不溶于二甲苯中，并含约15％丙烯，C)65℃在环境温度可溶于二甲苯中的无定形丙烯/乙烯共聚物，其特性粘度在135℃的四氢化萘中为2.95dl/g，乙烯含量为30％。
上述多相烯烃共聚物具有下列性质(用上述方法测定)：-M.F.R.(d1/分)         0.6-拉伸强度(MPa)         ＞8-断裂伸长率(％)        ＞350-维卡(℃)              55-Shore D(pts)          30-挠曲模量(MPa)         70-压缩变形(％)          87(22h-70℃)
改性聚合物包括在上述多相烯烃聚合物的粒子上淀积有下列化合物(重量百分数)的烯烃聚合物主链：5％马来酸酐，1％Luperox101 2，5-二甲基-2，5-二(过氧化叔丁基)己烷。
将90重量份如此获得的改性多相烯烃聚合物(I)在氮气氛下于240℃在Brabender单螺杆挤出机中与10重量份分子量为20000(SNIA售)的Ternyl B27聚酰胺(尼龙6)(组分II)共混。
在得到的组合物中的聚酰胺为分散球状粒子形式，直径为约0.07-0.7微米(电子显微镜测定)。此外，得到的组合物具有下列性质：-M.F.R.(dg/分)        1.7-拉伸强度(MPa)        ＞11-断裂伸长率(％)       ＞370-维卡(℃)             59-Shore D(pts)         32-挠曲模量(MPa)        110
将按上述制备的组合物通过使其于230-250℃通过螺杆长度/直径比为20的单螺杆Brabender挤出机的扁平模头挤出而转变为厚度为200微米的片材。
将得到的片材折叠，并用带有在27MHz工作的可加热电极并装备有带运行终止测微停止装置(end-of-run micrometric stop)的加压辊的射频热合设备自身封合。
封合条件如下：-电极电流强度：        0.7A-辊压力：             10-30kg/cm2-可加热电极的温度：   40-60℃-封合时间：           2-5秒。
如此获得的封口是均匀的，而且沿整个封合部分的表面无毛刺。在手工剥离时，该封合的片材的两个边缘在与封口相邻的地方裂开，而不会在封合的地方裂开。

Claims (4)

1.一种适合于可射频热合的片材和薄膜的聚烯烃组合物，其主要由下列成分组成：(I)90-95重量％的多相共聚物，包括
A)5-50重量％的结晶丙烯均聚物、丙烯和乙烯的结晶共聚物、丙烯、乙烯和CH2＝CHRα-烯烃的结晶共聚物或其共混物，其中R是C2-C8烷基，所述结晶共聚物含大于85％的丙烯；
B)0-20重量％乙烯与丙烯或与CH2＝CHRα-烯烃或与这两者的结晶共聚物部分，其中R是C2-C8烷基，所述部分在环境温度不溶于二甲苯中；
C)40-95％乙烯与丙烯或与CH2＝CHRα-烯烃或与这两者连同可任选的少量二烯烃的弹性体型共聚物部分，其中R是C2-C8烷基，所述共聚物部分中乙烯含量小于40重量％，并在环境温度可溶于二甲苯中；
所述的多相共聚物用用量为该多相共聚物的0.03-0.3重量％的马来酸酐改性；和(II)5-10重量％的介电热损耗因子至少为0.01的聚酰胺。
2.权利要求1的组合物，其中组分(II)为直径为0.05-0.7微米的粒子形式。
3.包含权利要求1的组合物的片材或薄膜。
4.其中至少一层包含权利要求1的组合物的多层片材或多层薄膜。
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