CN1216954A - 高防潮性的以聚丙烯为基的膜 - Google Patents

高防潮性的以聚丙烯为基的膜 Download PDF

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CN1216954A
CN1216954A CN97194232A CN97194232A CN1216954A CN 1216954 A CN1216954 A CN 1216954A CN 97194232 A CN97194232 A CN 97194232A CN 97194232 A CN97194232 A CN 97194232A CN 1216954 A CN1216954 A CN 1216954A
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film
modifier
weight
basic unit
cortex
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J·E·布鲁
J·K·昆
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ExxonMobil Oil Corp
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Abstract

一种具有改善的防潮性和增强的机械性能的高分子膜。该膜具有基层,该基层包含全同立构规整度在93%以上的高结晶度聚丙烯、全同立构规整度为90－93%的常用的全同聚丙烯和可高达9重量%的树脂改性剂的共混料。

Description

高防潮性的以聚丙烯为基的膜
本发明涉及以聚丙烯为基的多层膜，该多层膜具有改进的防潮性和增强的机械性能。
高分子膜使用在许多商业应用中。一个特别重要的应用是食品的包装。食品包装工业中使用的膜是选择和/或设计成能提供适合食品密封度所需的特性。这些特性包括防水汽渗透性、阻隔氧和气体性能和阻隔香味和芳香性能。
聚丙烯是制造食品包装工业中所用膜的过程中常用的聚合物。在多层膜的情况下，聚丙烯通常用作基层即芯层。聚丙烯层往往需改性以得到所需的而未改性的聚丙烯所没有的特性。例如，可将树脂改性剂和/或添加剂与聚丙烯共混。
改变聚丙烯特性的努力往往是在改善所得膜的防潮性方面。迄今为止，已知将聚丙烯与树脂改性剂共混会提供这些改善。通常，必须添加10-20％的树脂改性剂以使膜的水汽透过性达到所需的下降。
然而，在上述范围内添加树脂改性剂也有不利之处。尤其是在本领域通常使用的填充量范围内，聚丙烯的尺寸稳定性会显著下降。这又会影响所得膜的切削性和加工性能，导致制造成本增加和/或膜质量下降。
高分子膜的机械性能是另一个重要的特性，尤其是在烟草产品的包装等方面的应用中。机械性能增强的膜能使操作和包装变得容易，因为这些膜更容易被常用的工业机器适应。已有人试图通过增加取向和/或添加添加剂来提高以聚丙烯为基的膜的机械性能(由膜的刚度和模量测得)。然而，增加取向往往会在膜的制造过程中增加其开裂的可能性，而添加添加剂通常只能有限地提高机械性能，但会对膜的其他特性(如尺寸稳定性和透明度等)产生不良影响。
本专利申请人是共同申请人之一的审理中的美国专利申请No.08/490,081(申请日为1995年6月13日)和08/542,209(申请日为1995年10月12日)公开了具有高结晶度聚丙烯的基层和最高可达8重量％的树脂改性剂的高分子膜结构。皮层可粘附在基层的相反表面上。公开的膜结构具有改善的防潮性和增强的机械性能，并同时保持了尺寸稳定性、切削性、加工性能和透明度。然而，在公开的膜结构中使用高结晶度的聚丙烯增加了结构的制造难度，尤其是在膜的拉伸和切割等制造工序方面。使用高结晶度聚丙烯还增加了膜结构的成本。
因此，本领域仍需要一种树脂改性的以聚丙烯为基的膜，它可容易地以低成本进行制造，且具有改善的防潮性、增强的机械性能、尺寸稳定性、切削性、加工性能和透明度。
本发明即是针对现有技术的需要而涉及一种具有改进的防潮性和增强的机械性能的高分子膜。该膜具有基层，所述基层包含全同立构规整度在93％以上的第一聚丙烯聚合物、全同立构规整度为90-93％的第二聚丙烯聚合物和填充量最高可达基层重量的9％的树脂改性剂的共混料。
在一个优选的实施方式中，基层包含60-94重量％(最好为70-88重量％)的第一聚丙烯、3-37重量％(最好为4-26重量％)的第二聚丙烯和3-9重量％(最好为4-8重量％)的树脂改性剂。树脂改性剂最好是氢化烃。
在另一优选的实施方式中，至少一层皮层粘附在基层上，最好皮层上面有涂层。皮层最好是由乙烯/丙烯无规共聚物或乙烯/丙烯/1-丁烯三元共聚物形成的。在一个特别优选的实施方式中，皮层含有卷绕时防止膜粘连的有效量的防粘剂和在膜露出的表面上有保持低摩擦系数的有效量的硅油。
其结果是，本发明提供一种以聚丙烯为基的膜结构，它具有改善的防潮性和增强的机械性能。这些改善的性能的得到未使尺寸稳定性有所损失，也未对膜的其他特性(如透明度)产生不良影响。因此，该膜结构具有高度的切削性和加工性能，从而能提供较高质量的膜和/或降低制造成本。最后，该膜结构可容易地进行制造。
如在本专利申请人是共同申请人之一的审理中的美国专利申请No.08/490,081(申请日为1995年6月13日)和08/542,209(申请日为1995年10月12日)所公开的，添加少量的树脂改性剂可使由HCPP形成的高分子膜结构的水汽透过性出现出乎意料的大大下降。该防潮性随着树脂改性剂的填充量的增加(树脂改性剂填充量最大可达8％)而增加。即，大于8％的填充量基本上不会使防潮性有进一步地提高。而且，以HCPP为基的膜结构还提供增强的机械性能而不会出现现有技术的膜结构中普遍存在的尺寸稳定性和透明度下降的情况，现有技术的膜结构将需要添加高达20％的树脂改性剂以得到最大的防潮性。然而，在膜结构中使用HCPP会增加制造膜结构的难度，尤其是在拉伸和切割等制造工序方面。
本发明者业已发现，在本专利申请人是共同申请人之一的审理中的美国专利申请No.08/490,081和08/542,209中公开的以HCPP为基的膜结构可通过在其中掺入一定量的常用的全同聚丙烯而进一步地加以改善。更具体地说，本发明是将高结晶度聚丙烯(HCPP)和常用的全同聚丙烯(PP)与树脂改性剂共混而形成基层前体。该HCPP的全同立构规整度在93％以上，最好为94-98％，而PP的全同立构规整度为90-93％。共混的基层在制造效率上有显著提高，并同时保持了在本专利申请人是共同申请人之一的审理中的申请中所公开的结构所达到的增强的性能。而且，共混的基层的成本显著下降，包括材料和制造成本两方面。
HCPP和PP的共混料最好包含有效量的HCPP，这些HCPP能使基层的防潮性对树脂改性剂填充量的曲线在树脂改性剂填充量大于9％时其斜率基本上为零。即，在水汽渗透率(WVTR)对树脂改性剂(％)的图中水汽透过性出现出乎意料的大的初始下降，这种情况持续到树脂改性剂的填充量达到9％为止。当树脂改性剂的填充量大于9％时，曲线的斜率基本上变成零，由此，增加填充量基本上不会使防潮性有进一步的提高。关于曲线斜率，此处定义的斜率基本上为零是指斜率约在10％以下，更好的是约在5％以下，当树脂改性剂的填充量增至9％以上时，可得到额外的防潮性。
基层最好包含60-94重量％，更好的是70-88重量％的HCPP。其余百分数的基层是由PP构成的，PP的量宜有效地使基层增塑，这样，可增加所得挤出膜结构的加工性能，更好的是，PP的量至少与基层中存在的树脂改性剂的量相等。
合适的PP市售品包括Fina 3371(得克萨斯州Dallas市Fina Oil and Chemical公司产品)、Exxon 4612和Exxon 4052(得克萨斯州Houston市Exxon Chemical公司产品)和Amoco 6361(伊利诺伊斯州芝加哥市Amoco Chemical公司产品)。合适的HCPP市售品包括Amoco 9117和Amoco 9119(伊利诺伊斯州芝加哥市Amoco Chemical公司产品)和Chisso HF5010和Chisso XF2805(日本东京ChissoChemical株式会社产品)。合适的HCPP还可从欧洲Solvay公司购得。
HCPP具有很高的全同立构规整度，从而其结晶度比常用的全同聚丙烯更高，即，在93％以上。(此处定义的常用的全同聚丙烯是指其全同立构规整度为90-93％)。HCPP因此而具有较高的刚度、表面硬度、在较高温度下的较低挠度、和比常用的全同聚丙烯更好的蠕变性能。关于HCPP(包括其制备方法)的更详细内容在美国专利No.5,063,264中有揭示。
在本发明中，立构规整度可根据“Integrated Infrared Band Intensity Measurementof Stereoregularity in Polypropylene”,J.L.Koenig和A.Van Roggen,Journal ofApplied Polymer Science,Vol.9,PP.359-367(1965)和“Chemical Microstructure ofPolymer Chains”,Jack L.Koenig,Wiley-Inerscience Publication,John Wiley and Sons,New York,Chichester,Brisbane,Toronto中叙述的方法用红外光谱学进行测定。立构规整度性还可用十氢化茶(萘烷)溶解度和核磁共振(NMR)谱进行测定。
如上所述，将HCPP和PP组分与树脂改性剂共混，形成基层前体。树脂改性剂的量最高可达9重量％，较好的为4-8重量％，更好的为6重量％。共混可通过将HCPP、PP和树脂改性剂直接加入到膜挤出机中或通过使用母料来进行。一个较佳的共混组分的方法是使用由PP和树脂改性剂形成的母料(例如80％的PP和20％的树脂改性剂)。然后将母料与HCPP共混，HCPP可将PP和树脂改性剂两者的浓度降低至最终所需的含量。
树脂改性剂最好是低分子量的氢化烃，它可与HCPP和PP聚合物相容，能提供所需的增强的膜性能。优选的树脂改性剂的数均分子量在5000以下，较好的是在2000以下，更好的为500-1000。树脂改性剂可以是天然的或合成的，软化点宜为60-180℃。尤其合适的烃(可基本上被氢化的)是烃类树脂。优选的烃类树脂包括石油树脂、萜烯树脂、苯乙烯树脂和环戊二烯树脂。
适合在本发明中使用的氢化烃类树脂市售品的例子有特拉华州的Hercules公司以商品名PICCOLYTE、REGALREZ和REGSLITE销售的产品以及得克萨斯州Houston市Exxon Chemical公司以商品名ESCOREZ销售的产品。
一个尤其优选的树脂改性剂在此处称为饱和的脂环类树脂。饱和的脂环类树脂是通过芳香烃类树脂的氢化而得到的。芳香族树脂本身是通过将含有作为主要成分的芳香烃的活性的不饱和烃(其中，活性的双键一般在侧链上)聚合而得到的。更具体地说，脂环类树脂是通过将后者氢化至所有(或几乎所有)的不饱和键(包括芳香环中的双键)消失而由芳香族树脂得到的。
本发明中所用的饱和的脂环树脂的软化点为85-140℃，较好的为100-140℃，由球环法测得。适合在本发明中使用的市售的饱和脂环类树脂的例子有日本Arakawa Forest Chemical Industrie株式会社以商品名ARKON-P销售的产品。
在一个优选的实施方式中，烯类聚合物的至少一层皮层粘附在基层的至少一个侧面上。该皮层最好与基层共挤出。在另一优选的实施方式中，皮层在基层的两侧同时共挤出。
在又一优选的实施方式中，将涂料施加在皮层的外表面上。可将能提供改善的可印性、切削性和阻隔芳味性能的丙烯酸类涂料施加在其中的一个皮层上。可将热封涂料(如乙烯/丙烯酸甲酯共聚物(EMA)或乙烯/丙烯酸共聚物(EAA))施加在其他皮层上。其他合适的涂料包括聚偏二氯乙烯(PVDC)、聚乙烯醇(PVOH)和低温度热封涂料(如在本专利申请人是共同专利权人之一的美国专利No.5,419,960中所揭示的)。
合适用作皮层的烯类聚合物包括ⅰ)乙烯均聚物、ⅱ)乙烯与丙烯的共聚物、ⅲ)乙烯或丙烯和丁烯或另一种具有5-10个碳原子的α-烯烃的共聚物、ⅳ)乙烯、丙烯和丁烯或另一种具有5-10个碳原子的α-烯烃的三元共聚物、和ⅴ)它们的混合物。
尤其适合用作皮层的烯类聚合物包括丙烯为主要组分、乙烯含量为2-10重量％(相对于共聚物重量)的乙烯/丙烯共聚物、丙烯为主要组分、丁烯含量为0.5-25重量％(相对于共聚物重量)的丙烯/丁烯共聚物、丙烯为主要组分、乙烯含量为0.5-7重量％、1-丁烯含量为5-30重量％(均相对于三元共聚物重量)的乙烯/丙烯/1-丁烯三元共聚物以及这些聚合物的混合物。共聚物和三元共聚物最好是无规聚合物。
为进一步改善所得膜的某些性能，在基层和/或皮层中可加入有效量的添加剂，如防粘剂、抗静电剂和/或增滑剂。
优选的防粘剂包括硅石、滑石粉、粘土、硅酸铝钠和常用的无机防粘剂。其他合适的防粘剂包括无机添加剂，如二氧化硅、碳酸钙、硅酸镁、硅酸铝、磷酸钙等和/或不相容的有机聚合物，如聚酰胺、聚酯、聚碳酸酯等。
优选的抗静电剂包括烷烃磺酸碱金属盐和具有10-20个碳原子并且脂族基团被2-羟烷基-(C1-C4)基团取代的、基本上直链的、饱和的脂族叔胺。优选的胺有其烷基上有10-20个，最好是12-18个碳原子的N,N-二(2-羟乙基)-烷基胺。抗静电剂的有效量在0.05-3重量％(相对于层重量)之间。
优选的增滑剂包括高级脂族酸酰胺、高级脂族酸酯、蜡、金属皂和硅油(如聚二甲基硅氧烷)。润滑剂的有效添加量在0.1-2重量％之间。
在本发明的一个实施方式中，膜结构包括一对粘附在芯层反面的皮层。各皮层含减少卷绕的膜粘连的有效量的防粘剂(例如硅石)且至少一层皮层含在皮层的暴露面上保持低摩擦系数的有效量的硅油(例如，聚二甲基硅氧烷)。防粘剂的量最好在0.1-0.3重量％之间。硅油的量在0.5-2.0重量％之间，最好在0.8-1.2重量％之间，粘度为350-1,000,000厘沲，最好为10,000-60,000厘沲。若将硅油添加至两层皮层中，则可制得ABA结构。在硅油仅加在一层皮层中(由此产生ABC结构)的那些实施方式中，在膜卷绕后仍可将一定量的油移至反面的皮层上。在这独特的ABC结构中，可在卷绕之前将不含油的一面进行火焰处理或电晕处理。
本发明的多层膜可用市售的共挤出树脂体系进行制备。如上所述，较好的是，将共混的PP、HCPP和树脂改性剂与至少一种形成皮层的第二聚合物共挤出。可将聚合物加热至熔融状态并通过平片模头从常用的挤出机共挤出，在从模头挤出之前，将熔化的物流在模头接套中混合。离开模孔后，将多层膜结构骤冷。
本发明的膜结构最好是双轴取向的。在一个优选的实施方式中，将膜结构在纵向(MD)上拉伸4.5-6倍，在横向(TD)上拉伸6-13倍。总取向倍率(MD×TD)在25-80之间。取向后，可切去膜的边缘并将膜卷绕在卷芯上。
本发明的膜结构还具有比现有的具有以全同聚丙烯为基的芯层的膜结构出乎意料地增大的刚度和模量(MD和TD)。增大的刚度和模量使膜结构具有增强的机械性能，这又使后续的操作和包装变得容易。而且，MD和TD模量的增加是在取向较低的情况下实现的，因此，可降低制造成本和相关的开裂可能性。
本发明的共混的基层还提高了作业线的操作性和作业线的正常运行时间百分率，这些改善可在本发明的膜结构的制造过程中观察到。例如，共混的基层降低了拉伸膜所需的拉力，此外，与本专利申请人为共同申请人之一的审理中的美国专利申请No.08/490,081(申请日为1995年6月13日)和08/542,209(申请日为1995年10月12日)所公开的膜相比，挤出膜的边切除变得更容易。这些改善还进一步地降低了制造成本。值得注意的是，这些改善的性能是在同时保持了下面的实施例所示的改善的防潮性且不对膜的其他特性(如尺寸稳定性和透明度)产生不良影响的情况下得到的。最后，共混的基层还可节约材料成本。
在本发明中，所形成的膜结构的厚度在10-60微米之间，较好的是在15-50微米之间。
                            实施例
在下面的各实施例中，水汽渗透率(WVTR)是在37.8℃(100°F)和90％相对湿度的条件下(ASTMF-372)测得的，以g/645.16cm2(100英寸2)/日/密耳为单位进行表示。
                          实施例1
制造试样1以显示现有的以全同聚丙烯为基的膜结构的防潮性。将厚度为23.75微米的全同聚丙烯(Fina 3371)芯层与厚度均为0.6微米的乙烯/丙烯无规共聚物(Fina 8573HB)的各皮层共挤出，制造ABA挤出物。将ABA挤出物在纵向上拉伸4.3倍，在横向上拉伸9倍。
试样 芯层 树脂改性剂(％)     WVTR
大气条件下 老化条件下
    1  Fina 3371     0     0.311     0.311
                          实施例2
制造试样2a-2c以显示现有的以全同聚丙烯为基的、树脂改性剂含量不同的膜结构的防潮性。将厚度为18.8微米、通过熔融共混而加入了不同量的萜烯聚合物(PICCOLYTEC-115)的全同聚丙烯(Fina 3371)芯层与厚度均为0.6微米的乙烯/丙烯无规共聚物(Fina 8573)的各皮层共挤出，制造ABA挤出物。将ABA挤出物在纵向上拉伸4.3倍，在横向上拉伸9倍。
试样 芯层 树脂改性剂(％)     WVTR
大气条件下 老化条件下
    2a     Fina 3371     0    ---     0.325
    2b     Fina 3371     10    ---     0.27
    2c     Fina 3371     20    ---     0.25
                      实施例3
制造试样3以显示以HCPP为基的膜结构的防潮性。用高结晶度聚丙烯(Amoco 9117)芯层重复实施例1。
试样 芯层 树脂改性剂(％)     WVTR
大气条件下 老化条件下
Amoco     9117     0     0.246     0.218
                        实施例4
制造试样4a-4j以显示以HCPP为基的、树脂改性剂含量不同的膜结构的防潮性。将80％HCPP(Amoco 9218)和20％树脂改性剂(ARKONP-115)的母料与另外的HCPP(Amoco 9218)共混，然后与乙烯/丙烯无规共聚物(Fina8573HB)的皮层共挤出，制造ABA挤出物。将ABA挤出物在纵向上拉伸4.3倍，在横向上拉伸9倍。
试样 膜厚度(微米)     HCPP(％) 树脂改性剂(％)     WVTR
大气条件下 老化条件下
    4a     19.8     94     6     0.230     0.202
    4b     19.8     94     6     0.234     0.205
    4c     19.8     94     6     0.235     0.222
    4d     19.8     94     6     0.231     0.217
    4e     19.8     94     6     0.229     0.215
    4f     19.8     94     6     0.235     0.215
    4g     26.8     94     6     0.219     0.208
    4h     26.8     94     6     0.226     0.212
    4i     26.8     90     10     0.216     0.210
    4j     26.8     90     10     0.218     0.209
                        实施例5
制造试样5a-5i以显示以HCPP/PP为基的、树脂改性剂含量不同的膜结构的防潮性。将85％PP和15％树脂改性剂(ESCOREZ)的母料与HCPP(Amoco9218)共混，然后与乙烯/丙烯无规共聚物(Fina 8573HB)的皮层共挤出，制造厚度为27微米的ABA挤出物。将ABA挤出物在纵向上拉伸4.3倍，在横向上拉伸9倍。
试样     HCPP(％)     PP(％) 树脂改性剂(％)     WVTR
大气条件下 老化条件下
    5a     60     34     6     0.220     0.203
    5b     60     34     6     0.215     0.208
    5c     60     34     6     0.224     0.213
    5d     60     34     6     0.221     0.217
    5e     60     34     6     0.249     0.220
    5f     33     57     10     0.216     0.210
    5g     33     57     10     0.229     0.206
    5h     0     85     15     0.233     0.223
    5i     0     85     15     0.239     0.219
                    实施例6试样6a-6g具有实施例1、4和5的相同膜的刚度和模量的平均值。
试样 试样的平均 刚度(g/4英寸)     模量(ksi)
    MD     TD     MD     TD
    6a     1     7.5     12.3     369.0     703.0
    6b     4a-4f     7.6     12.1     435.0     780.8
    6c     4g-4h     16.1     25.5     452.0     803.0
    6d     4i-4j     16.7     26.7     444.5     814.5
    6e     5a-5e     15.4     24.6     421.1     796.8
    6f     5f-5g     15.9     24.0     420.5     769.5
    6g     5h-5I     15.2     22.0     415.0     692.0
                        实施例7
制造试样7a-7f以显示以HCPP/PP为基的、树脂改性剂含量不同的膜结构的尺寸稳定性。将80％PP和20％树脂改性剂(ESCOREZ)的母料与HCPP(Amoco 9218)共混，然后与乙烯/丙烯无规共聚物的皮层共挤出，制造厚度为25微米的ABA挤出物。将ABA挤出物在纵向上拉伸4.3倍。
试样     TD(×)     HCPP(％) PP(％) 树脂改性剂(％) 纵向尺寸稳定性(-％@275°F) 横向尺寸稳定性(-％@275°F)
    7a     9     100     0     0     2.5     3.7
    7b     9     50     40     10     3.3     3.3
    7c     9     0     80     20     4.7     6
    7d     12     100     0     0     1.9     4.2
    7e     12     50     40     10     5.9     7.9
    7f     12     0     80     20     7.3     6.9
从上面的数据可很容易地看出，与实施例1的现有技术的膜相比，本发明的膜结构具有改善的WVTR，与实施例6a的现有技术的膜相比，刚度和模量也有改善，如实施例7所示，保持了尺寸稳定性并且如在本发明膜结构的制造过程中所观察到的，其制造变得容易，例如，提高了作业线的操作性和作业线的正常运行时间百分率。

Claims (10)

1．一种高分子膜，具有改善的防潮性和增强的机械性能，它包括基层，所述基层包含全同立构规整度在93％以上的第一聚丙烯聚合物、全同立构规整度为90-93％的第二聚丙烯聚合物和填充量最高可达基层重量的9％的树脂改性剂的共混料。
2．如权利要求所述的膜，其特征在于，所述基层包含有效量的第一聚丙烯，这些聚丙烯可使该基层的防潮性对树脂改性剂填充量的曲线在树脂改性剂填充量大于9％时其斜率基本上为零。
3．如权利要求1或2所述的膜，其特征在于，所述基层包含60-94重量％的第一聚丙烯、3-37重量％的第二聚丙烯和3-9重量％的树脂改性剂。
4．如权利要求1、2或3所述的膜，其特征在于，所述第一聚丙烯的全同立构规整度为94-98％。
5．如权利要求1、2、3或4所述的膜，其特征在于，所述树脂改性剂是氢化烃。
6．如权利要求5所述的膜，其特征在于，所述混合物还包含添加剂，所述添加剂选自防粘剂、抗静电剂和增滑剂。
7．如权利要求1、2、3或4所述的膜，其特征在于，它还包含至少一层粘附在基层的至少一面的皮层；所述皮层选自乙烯/丙烯无规共聚物和乙烯/丙烯/1-丁烯三元共聚物。
8．如权利要求7所述的膜，其特征在于，所述皮层还包含添加剂，所述添加剂选自防粘剂、抗静电剂、增滑剂和硅油。
9．如权利要求8所述的膜，其特征在于，所述皮层包含1000-3000ppm(重量)的防粘剂、0.5-2.0重量％的硅油，所述硅油的粘度为10,000-60,000厘沲。
10．如权利要求7所述的膜，其特征在于，其皮层的外表面上还有一涂层，所述涂层选自聚丙烯酸类、乙烯/丙烯酸甲酯共聚物、乙烯/丙烯酸共聚物、聚偏二氯乙烯和聚乙烯醇。
CN97194232A 1996-04-30 1997-03-28 高防潮性的以聚丙烯为基的膜 Pending CN1216954A (zh)

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