CN115697672A - 包装用多层可重复密封的启封易识别薄膜 - Google Patents

包装用多层可重复密封的启封易识别薄膜 Download PDF

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Publication number
CN115697672A
CN115697672A CN202180029004.0A CN202180029004A CN115697672A CN 115697672 A CN115697672 A CN 115697672A CN 202180029004 A CN202180029004 A CN 202180029004A CN 115697672 A CN115697672 A CN 115697672A
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China
Prior art keywords
layer
film
copolymer
corona
block copolymer
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CN202180029004.0A
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埃伦·S·史密斯
卡斯拉·米尔梅斯达
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Bostec
Tefan LLC
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Bostec
Tefan LLC
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Publication of CN115697672A publication Critical patent/CN115697672A/zh
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Abstract

一种多层薄膜，按此顺序包括：(a)双轴取向的聚对苯二甲酸乙二醇酯层，(b)压敏粘合剂层，(c)弹性聚氨酯分散体，和(d)双轴取向的聚对苯二甲酸乙二醇酯层。层(d)优选具有A:B:A:C结构；其中A和B优选包括结晶PET和防粘连颗粒，C优选是无定形的、可热封的共聚酯。

Description

包装用多层可重复密封的启封易识别薄膜
相关申请的交叉引用
本申请要求2020年4月15日提交的美国专利申请号63/010,418的35U.S.C.§119(e)项下的权益。
技术领域
本发明提供了一种聚酯薄膜，可用于为包装提供启封易识别(tamper-evident)、可重复密封的封盖组件。可重复密封的包装已经变得流行，特别是在食品领域，因为它的优点是向消费者提供一个产品容器，无需将剩饭剩菜转移到另一个存储容器。
背景技术
用于可剥离和/或可重复密封包装领域的多层薄膜是已知的，例如，在授权给博斯蒂克股份公司(BOSTIK SA)的美国专利2018/0215522中和在授权给特飞恩有限公司(Terphane,Inc)的美国专利7,413,800中。可重复密封包装用于食品加工业和大众营销，用于包装易腐烂的食品，特别是生鲜产品。这些容器通常包括容器(container)(或储器(receptacle))和形成盖子的密封物，它们通过焊接密封地相互连接在一起。在密封物第一次被打开且容器中容纳的部分食品被消耗后，用户可以复位储器上的密封物，以便基本上密封地重新密封包装，因此，在将其放入冰箱后，酌情储存产品的剩余部分。一系列的重新打开和重新密封也是可能的。
用于可重复密封包装系统的多层薄膜应该允许容易的首次开启和令人满意的重合/重新打开周期。例如，通过施加小于或等于15N/cm的力，优选7N/cm或更小的力来测量初始剥离强度，并且一旦包装打开，使用传播力(propagation force)，优选3-11N/cm，更优选4-11N/cm。该薄膜还优选能使包装容易自粘重合，也就是说，在一系列闭合/重新打开操作之后，薄膜的两部分容易手动复位，重新打开力大于1N/cm，优选大于或等于2N/cm，更优选2-4N/cm。
许多现有的可重复密封的封盖结构或薄膜采用粘附到不可移除的盖子上的可剥离标签，或者在需要移除产品封盖的较大部分时，模切(die-cutting)开口。这些薄膜通常通过将热封双向拉伸的聚对苯二甲酸乙二醇酯(BOPET)薄膜层压到具有水基压敏粘合剂(PSA)涂层的可打印BOPET网上来生产。然后，对可热封层进行激光刻划或模切，以提供进入容器的开口。由于生产这种结构所需的技术，通常需要多个转化步骤才能生产。这导致很长的交货时间和昂贵的包装成本通常会转嫁给消费者。此外，水基PSA具有低防潮性，这可能导致包装失效。激光刻痕在托盘边沿的边缘周围留下一条薄膜带，限制了接触内部食品。
因此，优选将整个盖子用作可剥离的开口进行包装，允许更大程度地接触容器，并且允许避免额外的成本和模切的工艺步骤。
此外，目前很少有可重复密封的盖子提供启封易识别。如果需要启封易识别的可重复密封的包装，可能需要贴上额外的标签封口，该标签封口是破损的或一旦移除无法重新密封，以告知包装已经被打开，需要额外的步骤和成本。
发明内容
本发明提供了一种可用于形成可重复密封包装的多层薄膜。所述薄膜可用于形成托盘的整个盖子，例如，避免了仅需要具有可剥离标签的必要性，并且进一步避免了对模切开口的需要。此外，该薄膜提供了一个启封易识别功能，让消费者知道包装是否已被打开。
本发明提供了一种薄膜，包括(a)双轴取向的聚对苯二甲酸乙二醇酯(BOPET)层，(b)压敏(PSA)层，(c)分散的聚氨酯颗粒层和(d)BOPET层。BOPET层(a)是任选地可打印的，以便可以向消费者提供产品信息。层(a)至(d)按上述顺序排列，并且通常彼此相邻，优选没有额外的内层。
原则上，任何BOPET薄膜都可以用作层(a)。BOPET薄膜是众所周知的，如在例如美国专利2,823,421和美国专利2,884,663中所公开的。层(a)可以接受电晕(corona)和/或共挤(coex)处理以改善油墨和粘合剂的粘附性。所述电晕处理可以是在将薄膜提供给层压设备之前对层(a)的预处理，或者可以是“冲压”电晕处理，其中电晕处理器位于生产线上，并在施加粘合剂和层压之前进行效果处理。电晕处理也可以是预处理和冲压处理的组合。优选BOPET薄膜进行表面处理以增加粘附力。代表性的表面处理薄膜被公开在例如美国专利4,476,189和美国专利5,985,437中。适合作为层(a)的表面处理的BOPET薄膜也可从商业上获得，例如，购自Terphane LLC，包括Terphane 10.21(一面COEX处理)、10.25(一面COEX处理，一面电晕处理)和10.15(一面电晕处理)。例如，层(a)的厚度可以是2-100μm，或5-50μm，或10-40μm。
优选的压敏粘合剂包括由苯乙烯单体和至少一种其他共聚单体(如乙烯、丙烯、异戊二烯、丁二烯和丁烯)得到的苯乙烯嵌段共聚物。所述共聚物可以具有线性、放射状或星形、二嵌段、三嵌段或多嵌段结构，具有至少一种上述共聚单体的中间嵌段。这些PSA进一步包含增粘剂，例如脂肪族树脂，以增强嵌段共聚物的苯乙烯和非苯乙烯嵌段之间相容性的。这类树脂包括多萜类、由C5切割的聚合物，任选地由C9切割改性的聚合物，由部分或完全氢化的C9切割的聚合物，任选地由脂肪族切割改性的聚合物。所述PSA通常包含45至85重量％，优选55至70重量％的共聚物或共聚物共混物，以及15至60重量％，优选30至45重量％的增粘树脂或增粘树脂的共混物。所述粘合剂还可以含有少量增塑剂、稳定剂或填料，这些是热熔粘合剂中常规使用的添加剂。因此，典型的PSA包含至少一种苯乙烯嵌段共聚物和至少一种兼容增粘树脂的共混物。
优选地，在-20至+40℃之间，这种共混物的弹性模量G′<5×105Pa(达尔奎斯特(Dahlquist)标准)，在至少130℃的温度下，具有粘度η(根据ISO 11443标准测量)。
·并且对于剪切速率dγ/dt在100和1000s-1之间，位于曲线上方的范围内(见图1)，对于拉伸速率为1ms-1的抗拉强度，位于平均曲线下方的范围内(见图2)，如多项式方程所定义：y＝-2.82×10-16x6+5.92×10-13x5-4.97×10-10x4+2.15×10-7x3-4.99×10-5x2+6.26×10-3x+4.71×10-2，其中y—纵坐标—表示应力，以MPa为单位，x—横坐标—表示变形，以百分比(％)为单位。
特别优选的压敏粘合剂是包括以下物质的共混物的那些：
·40-85重量％的至少一种苯乙烯嵌段共聚物，其由至少一种苯乙烯单体和至少一种其他共聚单体(优选异戊二烯、丁二烯、丁烯或其组合，更优选异戊二烯或丁二烯，最优选形成SIS嵌段共聚物的异戊二烯)形成，并且包括：
ο聚合物中苯乙烯相的质量百分比为10-35％，优选为10-25％；和
ο聚合物中二嵌段的质量百分比大于30％，优选大于40％；和
·15-60重量％的至少一种相容增粘树脂，其软化温度在5至150℃之间。在190℃，使用2.16kg重量时，这样的粘合剂的熔体流动指数在2至70g/10min之间。
特别地，所述PSA具有以下特性:
·在至少130℃的温度下，粘度位于功率曲线η＝22000×(dγ/dt+200)-0.82之上的范围内，其中dγ/dt包括在100和1000s-1之间的剪切速率；
·在拉伸速率为1ms-1下，抗拉强度位于多项式曲线y＝2.82×10-16x6+5.92×10- 13x5-4.97×10-10x4+2.15×10-7x3-4.99×10-5x2+6.26×10-3x+4.71×10-2之下的范围内，其中y包括纵坐标，表示应力，以MPa为单位，x包括横坐标，表示变形，以％为单位；
·在-20至+40℃下，弹性模量G′<5×105Pa；
·调节的冷粘合力，使热挤出压敏粘合剂能够在第一次开启过程中表现出主要的内聚(cohesive)失效。
所述PSA层的厚度优选为5-35μm，更优选为5-22μm
在一个实施方案中，在室温下，粘合剂在挤出之前是以小球或颗粒的形式存在。
美国专利7,622,176中公开了合适的压敏粘合剂。
层(c)作为弹性聚氨酯颗粒的分散体施用，然后干燥或固化。这种分散体被称为触觉涂层，用于薄膜的外表面，以提供柔软的触感。例如，此类涂层在美国专利10,428,237中公开，也可以从市场上购得，例如DSM Coating Resins B.V.的
Figure BDA0003892922230000041
R-1030、AshlandInc.的PurkoteTM23593和Michelman Inc.的
Figure BDA0003892922230000042
聚氨酯层的厚度可以在很大范围内变化，通常为0.1-5μm，优选0.1-3μm。层(c)在本文中可称为弹性聚氨酯分散体。
层(d)优选为“特种”BOPET，包括具有A:B:A:C结构的双轴拉伸聚对苯二甲酸乙二醇酯的多层膜，其中：
ο所述A层和B层由含有无机防粘连颗粒(例如二氧化硅、碳酸钙、玻璃珠、高岭土或这些成分中的两种或多种的混合物，优选为二氧化硅)的结晶PET组成，B层任选地含有重新研磨的PET；
ο所述C层由无定形的可热封共聚酯组成。所述共聚酯优选为无定形聚酯树脂，例如通过由对苯二甲酸二甲酯或对苯二甲酸与下列一种或多种物质的缩合制备的对苯二甲酸乙二醇酯共聚物：壬二酸、壬二酸二甲酯、癸二酸二甲酯、癸二酸、间苯二甲酸、5-磺基间苯二甲酸钠，或者通过由对苯二甲酸二甲酯或对苯二甲酸与乙二醇、二甘醇和/或环己烷二甲醇的缩合制备。共聚酯优选为间苯二甲酸、对苯二甲酸和单乙二醇(MEG)/二甘醇(DEG)。代表性的共聚酯在USP 7,413,800中被公开。
ο所述C层还可以包括一种或多种防雾剂，包括但不限于单硬脂酸甘油酯或十二烷基苯磺酸钠。
在层(d)优选的BOPET中，基于层(d)的总厚度，层(A)的含量优选为10-15％，更优选约13％，并且每层(A)优选含有200-300ppm抗粘连剂；基于层(d)的总厚度，层(B)的含量优选为61-78％，更优选约69％，并且优选包含90-215ppm抗粘连剂；层(C)的含量优选为层(d)总厚度的12-24％，更优选约18％，并且优选包含150-250ppm的抗粘连剂。层(A)和(B)的总厚度优选为2-100μm。层(C)的厚度优选为0.1-10μm。层(d)和层(A)、层(B)及层(C)的总厚度优选为2-110μm，优选为4-15μm，更优选为6-10μm，优选为8μm。
BOPET层(d)的双轴取向可以在该层的共挤出之后通过薄膜的高温拉伸来实现，例如在226-238℃，优选在238℃。薄膜在横向/纵向(TD/MD)上拉伸300-400％，优选350％。
在一个实施方案中，BOPET层(a)和/或可热封BOPET层(d)也可以涂有阻隔涂层，以降低薄膜对气体(如氧气、氮气和其他气体)、以及气体、湿气和/或气味的混合物的渗透性。代表的阻隔涂层可以在有机阻隔聚合物和填充聚合物的组中找到，其包括偏氯乙烯聚合物和共聚物，例如PVDC、PVOH或EVOH基涂层(例如在美国专利10,392,527和美国专利2017/0210867中描述的)、聚氨酯涂层或其他水基、溶剂基或UV/EB固化涂层。所述阻隔涂层可以用纳米尺寸的添加剂(如云母、蛭石、纳米纤维或其它添加剂)来强化，以增强其阻隔性能，如美国专利8,080,297中所述。所述阻隔涂层可以由分散体或溶液制备，然后涂覆到薄膜表面上，并使用任何已知的涂覆方法依次干燥，包括但不限于凹版印刷、柔版印刷、胶版印刷、喷涂和浸涂。其他阻挡涂层可以由金属、陶瓷或有机沉积产生，例如铝、氧化铝、氧化硅、三聚氰胺等。此类涂层可以通过任何已知的涂覆方法沉积，包括但不限于喷涂、热蒸发、溅射、化学气相沉积和原子层沉积。也参见美国专利7,413,800，在第4栏第18-24行讨论阻隔涂层。
附图说明
图1示出了本发明的一个实施方案中，根据粘度(Pa·s)与剪切速率(1/s)的关系，PSA的粘度下限。
图2示出了本发明的一个实施方案中，根据应力与变形百分比的关系，在1m/s的拉伸速率下，PSA的抗拉强度的上限。
图3示出了具有本发明的薄膜作为密封部件的封闭容器的一个代表物。
图4示出了打开后，具有本发明的薄膜作为密封部件的容器。
图5示出了用于制备薄膜的挤压层压工艺。
具体实施方式
本发明的多层膜可以通过共挤出层(d)BOPET，单独共挤出层(a)BOPET，在层(d)BOPET上凹版涂覆层(c)聚氨酯分散体，并用层(b)PSA作为粘合剂将层(d)BOPET挤出层压到层(a)BOPET上来生产。在挤出层压中，如图5所示，通过平模(53)将粘合剂(54)(在这种情况下，PSA层(b)，苯乙烯嵌段共聚物)挤出到移动的基材(在这种情况下，BOPET层(d)和(a)，由(51)和(52)表示)上。所述层(c)聚氨酯分散体可以在平模(53)的上游与挤出层压联机(in-line)涂覆，或者可以脱机涂覆，使得当供给至挤出层压过程时，它已经在BOPET层(d)上(如图5所示)。在平模(53)的上游，至少将与(b)PSA接触的层(a)BOPET的一面与挤出层压进行联机电晕处理，以增加(b)PSA对层(a)BOPET的附着力。聚合物熔体通常在高温下离开模具，通常为150-330℃，在一个实施方案中优选为150-190℃。在离开模具后，当聚合物熔体在被称为气隙的距离上与空气接触时被氧化。该距离可以针对每种树脂进行优化，典型范围为5至10英寸。增加空气间隙可以通过更长的氧化时间来提高附着力；然而，过高的空气间隙会由于聚合物的过度冷却而导致粘附力较低。当熔体离开模具时，熔体薄膜被下拉到两个辊(56)和(57)之间的辊隙(55)中，这两个辊分别是位于模具下方的压力辊和冷却辊。以高于熔融薄膜的速度移动的基底将薄膜拉伸到所需的厚度。两个辊之间的压力迫使薄膜压在基底上。进一步地，通过冷却辊的低温，典型地是约50-85°F，将膜冷却和固化。牵伸比是挤出涂覆工艺的特征参数之一，是模具间隙与基材上聚合物薄膜厚度的比率。典型的牵伸比是20-60。然后将层压薄膜通过由(58)和(59)表示的各种附加辊输送，并收集在最终辊(60)上。例如，在R.A.V.Raff和k.w.Doak(Interscience Publishers，1964)的《结晶烯烃聚合物，第二部分》，第478-484页，或在DominickV.Rosato的《塑料加工数据手册》(Chapman&Hall，1997)，第273-277页中给出了代表性的挤出涂覆方法。
本发明的薄膜优点是能够为容器形成可重复密封的盖子，该盖子可以包括容器的整个表面封闭，而不需要模切。此外，所述内部聚氨酯层(c)的存在，不是作为旨在改变膜的表面感觉的触觉或“软接触”涂层，而是提供了启封易识别特征，因为当盖子第一次打开时，膜从透明转变为混浊。层(c)可以进一步包括染料来增强这种效果。
图3和图4示出了符合本发明的容器。图3示出了打开之前(以及重新密封之后)的密封容器。在图3中，本发明的多层膜由(30)表示，由可印刷的BOPET(31)组成，其通过PSA(32)被粘附到弹性聚氨酯层(33)上，与被热封到容器(35)的凸缘(36)上的可热封BOPET(34)相邻。在图4中，所述容器已经通过剥开盖子打开，盖子由(40)表示，可印刷的BOPET(41)、PSA(42)、聚氨酯(43)和BOPET(44)。热封到容器(45)的凸缘(46)的薄膜部分包含保持粘附到其上的盖子的剩余部分、启封易识别的聚氨酯(431)和BOPET(441)。
本发明的方面
1.一种多层薄膜，按此顺序包括
(a)双轴取向的聚对苯二甲酸乙二醇酯层，
(b)压敏粘合剂层，
(c)弹性聚氨酯层，和
(d)双轴取向的聚对苯二甲酸乙二醇酯层。
2.方面1所述的薄膜，其中(d)具有A:B:A:C结构；A和B包括结晶PET和防粘连颗粒，C是无定形的、可热封的共聚酯。
3.方面2所述的薄膜，其中无定型、可热封的共聚物是对苯二甲酸乙二醇酯共聚物。
4.方面2或3所述的薄膜，其中C是(i)对苯二甲酸二甲酯或对苯二甲酸与壬二酸、壬二酸二甲酯、癸二酸二甲酯、癸二酸、间苯二甲酸或5-磺酸钠中的一种或多种的共聚物，或(ii)对苯二甲酸二甲酯或对苯二甲酸与乙二醇、二乙二醇和/或环己烷二甲醇的共聚物。
5.方面2-4中任一方面所述的薄膜，其中防粘连颗粒是二氧化硅、碳酸钙、玻璃珠、高岭土或其至少两种的混合物。
6.方面1-5中任一方面所述的薄膜，其中(d)已在226-238℃下被双轴拉伸TD/MD300-400％。
7.方面2-6中任一方面所述的薄膜，其中层(A)和层(B)的总厚度为2-100μm，层(C)的厚度为0.1-10μm，层(d)的厚度为2-110μm
8.方面1-7中任一方面所述的薄膜，其中层(d)的厚度为8μm。
9.方面1-8中任一方面所述的薄膜，其中层(b)包括至少一种苯乙烯单体和异戊二烯、丁二烯、丁烯或其混合物的至少一种苯乙烯嵌段共聚物。
10.方面9所述的薄膜，其中层(b)包括至少一种苯乙烯单体和形成SIS嵌段共聚物的异戊二烯的苯乙烯嵌段共聚物。
11.方面1-10中任一方面所述的薄膜，其中层(b)包含40-85％的苯乙烯嵌段共聚物和10-35％的相容增粘树脂，所述相容增粘树脂的软化温度为5-150℃。
12.方面1-11中的任一方面所述的薄膜，其中在至少130℃的温度下，压敏粘合剂粘度位于功率曲线η＝22000×(dγ/dt+200)-0.82之上的范围内，其中dγ/dt包括在100和1000s-1之间的剪切速率；
在拉伸速率为1ms-1下，抗拉强度位于多项式曲线y＝-2.82×10-16x6+5.92×10- 13x5-4.97×10-10x4+2.15×10-7x3-4.99×10-5x2+6.26×10-3x+4.71×10-2之下的范围内，其中y包括纵坐标，表示应力，以MPa为单位，x包括横坐标，表示变形，以％为单位；
在-20至+40℃下，弹性模量G′<5×105Pa。
13.方面1-12中任一方面所述的薄膜，进一步包括在层(a)和层(b)之间的附加共聚酯层(a’)。
14.方面2-13中任一方面所述的薄膜，其中层(C)包含防雾剂。
15.一种具有可重复密封盖子的容器，其中所述盖子是根据方面1-14中任一方面所述的薄膜。
16.一种制备方面1-14中任一方面所述的薄膜的方法，包括共挤出层(d)，加热至玻璃化转变温度以上，双轴拉伸该层，在层(d)上凹版涂覆层(c)聚氨酯分散体，并用层(b)PSA作为粘合剂将层(d)挤出层压到层(a)上。
17.根据方面16所述的方法，其中在238℃下，层(d)被双轴拉伸。
18.根据方面16或17所述的方法，进一步包括(i)在将层(a)提供给挤出层压设备之前对层(a)进行电晕预处理，(ii)冲击电晕预处理，其中电晕处理器存在于生产线上并在施加粘合剂和层压之前进行效果处理，或者(i)和(ii)的组合。
无需进一步阐述，相信本领域技术人员可以利用前面的描述最大程度地利用本发明。因此，前述优选的具体实施方案应被解释为仅仅是说明性的，而不是以任何方式限制本发明的其余部分。
本文引用的所有申请、专利和出版物的全部公开内容通过引用并入本文。
除非另有明确说明，混合物的所有百分比数据均表示重量百分比，并与相应的混合物整体有关，包括所有固体或液体成分，不包括溶剂。此外，除非另有明确说明，所有温度均以摄氏度(℃)表示。以下实施例旨在解释本发明，而不限制本发明。
实施例
创建了一系列薄膜样品来测试具有这种结构的薄膜作为包装容器的可重复密封盖子薄膜的适用性。
Figure BDA0003892922230000101
顶部薄膜层
薄膜A：92规格(23.3μm)的多层双轴取向PET薄膜，具有一面上电晕处理的表面(“电晕面”)，另一面上共挤出的共聚酯(“共挤面”(“COEX Side”))。
中间层
PSA：可挤出的压敏粘合剂。
底部薄膜层
薄膜B：50规格(12.7μm)的多层双向拉伸PET薄膜，具有共挤出的共聚酯热封层，其包括一面上的滑移包装(“具有滑动的热封面”)和另一面上的电晕处理表面(“电晕面”)。
薄膜C：52规格(13.2μm)的多层双向拉伸PET薄膜，一面上具有触觉(“软触”)哑光涂层(“软触面”)，另一面上具有共挤出的共聚酯热封层(“共挤面”)。
薄膜D：48规格(12.2μm)的多层双向拉伸PET薄膜，一面上具有共挤出的无光泽表面(“哑光面”)，另一面上具有电晕处理面(“电晕面”)。
薄膜E：48规格(12.2μm)的多层双向拉伸PET薄膜，其中一面经过化学处理(“化学处理面”)，另一面上具有共挤出的共聚物(“共挤面”)。
薄膜F：48规格(12.2μm)的多层双向拉伸PET薄膜，一面上具有非常光滑的高摩擦系数表面(“光滑面”)，另一面上具有共挤出的共聚物(“共挤面”)。
薄膜G：53规格(13.5μm)的多层双向拉伸PET薄膜，一面上具有共挤的共聚酯热封层(“热封面”)，一面上具有触觉(“软触”)哑光涂层(“软触面”)。
薄膜H：37规格(9.4μm)的多层双向拉伸PET薄膜，一面上具有共挤出的共聚酯热封层(“热封面”)，另一面上具有电晕处理表面(“电晕面”)，具有多向“易撕”特性。
薄膜I：72规格(18.3μm)的多层双向拉伸PET薄膜，具有死折特性，一面上具有电晕处理表面(“电晕面”)，另一面上具有未经处理的普通PET表面(“普通面”)。
薄膜J：56规格(14.2μm)的多层双向拉伸PET薄膜，具有美国专利7,943,230中所述的多向“易撕”特性。
样品
所有样品的顶膜层都使用了薄膜A，前八(8)个样品的薄膜A的电晕面朝向界面1的中间层，接下来的十七(17)个样品的薄膜A的共挤面朝向界面1的中间层。
同样的PSA用于中间层，但厚度不同。
薄膜B-J用于底部薄膜层，不同侧面朝向界面2的中间层。
对于每个样品，如图5所示，将用于顶部薄膜层的薄膜和用于底部薄膜层的薄膜供给到辊隙中，其中中间层的PSA被挤出。挤出的温度为170℃，空气间隙为7英寸，冷却辊为70°F。
表1总结了用于创建样品的薄膜、薄膜取向和中间层厚度的组合。
表1:样品的总结
Figure BDA0003892922230000111
Figure BDA0003892922230000121
Figure BDA0003892922230000131
评估样品1-14对于可重复密封膜(在容器上)应用的适用性，如通过剥离强度、雾度和透明度确定的。样品3、4、12和13(在界面2处具有柔软触感涂层的那些样品)提供了启封易识别特征(当第一次剥离和重新密封时从透明变为混浊)。表1中列出的柔软触感涂层是层(c)的涂层，即来自弹性聚氨酯分散体的涂层。
样品15-20示出了中间层中PSA用量对剥离强度、雾度和透明度的影响。
样品21和23示出了由于缺乏双轴取向(仅部分取向以使其“可扭曲”)而导致的薄膜I的死折叠性能对底部薄膜层的撕裂能力的影响。
样品22示出了薄膜J的撕裂能力对结构性能的影响，因为期望底部薄膜层在第一次开口时干净地破裂。
样品24和25示出了BOPET层(d)作为底部薄膜层的效果，但是没有层(c)的触觉(软触)涂层。
剥离强度的测试方法
·不具有外部可热封表面的样品(样品1-14)用溶解在1,3-二氧戊环溶剂中的共聚酯可热封树脂涂覆在底部薄膜层的外表面上(约2gsm涂层重量)，并在烘箱中干燥5分钟。
·从薄膜样品和0.5mm的APET盘料上切下1英寸宽的条状物。
·使用Labthink Param Classic 513梯度热封机，在200℃下，以1.5秒的停留时间和40psi的施加压力，将薄膜样品的可热封面热封到APET托盘片上。
·剥离强度是用MTS Insight 1拉伸装置测量的。用上颚夹住薄膜，用下颚夹住托盘片。在180℃下以50mm/min的速度剥离样品。
·剥离后，将薄膜从钳口中取出，用测试员的拇指将薄膜压回托盘片上，重新密封4次。
·然后用同样的方法重新剥离样品。
·这重复了4次。
剥离强度测试的结果总结在下面的表2中。
表2:剥离强度测试的总结
Figure BDA0003892922230000141
Figure BDA0003892922230000151
期望粘合剂失效时，第1次剥离强度大于1140gf/in，期望粘合剂失效时，第2次剥离强度大于285gf/in。
还测试了样品的雾度和透明度。使用BYK Gardner haze-gard plus按照ASTM方法D 1003测试雾度。相同的装置被用于测量透明度。雾度和透明度测试结果总结在下表3中。
表3:雾度和透明度测试的总结
Figure BDA0003892922230000152
Figure BDA0003892922230000161
Figure BDA0003892922230000171
期望雾度值≤13.0％，透明度值≥88.2％。

Claims (18)

1.一种多层薄膜，按此顺序包括
(a)双轴取向的聚对苯二甲酸乙二醇酯层，
(b)压敏粘合剂层，
(c)弹性聚氨酯层，和
(d)双轴取向的聚对苯二甲酸乙二醇酯层。
2.根据权利要求1所述的薄膜，其中(d)具有A:B:A:C结构；A和B包括结晶PET和防粘连颗粒，C为无定形的、可热封的共聚酯。
3.根据权利要求2所述的薄膜，其中所述无定型、可热封的共聚物是对苯二甲酸乙二醇酯共聚物。
4.根据权利要求3所述的薄膜，其中所述C是(i)对苯二甲酸二甲酯或对苯二甲酸与壬二酸、壬二酸二甲酯、癸二酸二甲酯、癸二酸、间苯二甲酸或5-磺酸钠中的一种或多种的共聚物，或(ii)对苯二甲酸二甲酯或对苯二甲酸与乙二醇、二乙二醇和/或环己烷二甲醇的共聚物。
5.根据权利要求2所述的薄膜，其中所述防粘连颗粒是二氧化硅、碳酸钙、玻璃珠、高岭土或其至少两种的混合物。
6.根据权利要求1所述的薄膜，其中(d)已在226-238℃下被双轴拉伸TD/MD 300-400％。
7.根据权利要求2所述的薄膜，其中层(A)和层(B)的总厚度为2-100μm，层(C)的厚度为0.1-10μm，层(d)的厚度为2-110μm。
8.根据权利要求7所述的薄膜，其中所述层(d)的厚度为8μm。
9.根据权利要求1所述的薄膜，其中层(b)包括至少一种苯乙烯单体和异戊二烯、丁二烯、丁烯或其混合物的至少一种苯乙烯嵌段共聚物。
10.根据权利要求9所述的薄膜，其中所述层(b)包括至少一种苯乙烯单体和形成SIS嵌段共聚物的异戊二烯的苯乙烯嵌段共聚物。
11.根据权利要求9所述的薄膜，其中所述层(b)包含40-85％的苯乙烯嵌段共聚物和10-35％的相容增粘树脂，所述相容增粘树脂的软化温度为5-150℃。
12.根据根据权利要求11所述的薄膜，其中在至少130℃的温度下，所述压敏粘合剂的粘度位于功率曲线η＝22000×(dγ/dt+200)-0.82之上的范围内，其中dγ/dt包括在100和1000s-1之间的剪切速率；
在拉伸速率为1ms-1下，抗拉强度位于多项式曲线y＝-2.82×10-16x6+5.92×10-13x5-4.97×10-10x4+2.15×10-7x3-4.99×10-5x2+6.26×10-3x+4.71×10-2之下的范围内，其中y包括纵坐标，表示应力，以MPa为单位，x包括横坐标，表示变形，以％为单位；
在-20℃至+40℃下，弹性模量G′<5×105Pa。
13.根据权利要求1所述的薄膜，进一步包括在所述层(a)和所述层(b)之间的附加共聚酯层(a’)。
14.根据权利要求2所述的薄膜，其中所述层(C)包含防雾剂。
15.一种具有可重复密封盖子的容器，其中所述盖子是根据权利要求1所述的薄膜。
16.一种制备权利要求1所述薄膜的方法，包括共挤出层(d)，加热至玻璃化转变温度以上，双轴拉伸所述层，在所述层(d)上凹版涂覆层(c)聚氨酯分散体，并用层(b)PSA作为粘合剂将所述层(d)挤出层压到层(a)上。
17.根据权利要求16所述的方法，其中在238℃下，所述层(d)被双轴拉伸。
18.根据权利要求16所述的方法，进一步包括(i)在将所述层(a)提供给挤出层压设备之前对所述层(a)进行电晕预处理，(ii)冲击电晕预处理，其中电晕处理器存在于生产线上并在施加粘合剂和层压之前进行效果处理，或者(i)和(ii)的组合。
CN202180029004.0A 2020-04-15 2021-04-14 包装用多层可重复密封的启封易识别薄膜 Pending CN115697672A (zh)

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