CN113365743B - 易粘聚酯膜及其制备方法 - Google Patents

易粘聚酯膜及其制备方法 Download PDF

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CN113365743B
CN113365743B CN202080011918.XA CN202080011918A CN113365743B CN 113365743 B CN113365743 B CN 113365743B CN 202080011918 A CN202080011918 A CN 202080011918A CN 113365743 B CN113365743 B CN 113365743B
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film
easy
mass
adhere
resin
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CN113365743A (zh
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山口洋平
多喜博
泷井功
伊藤胜也
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Toyobo Co Ltd
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Toyobo Co Ltd
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    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/22—Plastics; Metallised plastics
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Abstract

[问题]本发明提供了一种易粘聚酯膜和一种用于高效地制备所述易粘聚酯膜的方法，所述易粘聚酯膜具有较少的瑕疵，并且其中不存在由于在卷筒产品储存期间的紧密卷绕引起的外观缺陷。[技术方案]一种易粘聚酯膜，所述易粘聚酯膜包括作为基膜的聚酯膜和在所述基膜的至少一侧上的易粘层，其中相对于所述基膜的质量，所述基膜含有1质量％的量的平均粒径为0.1μm至2μm的粒子，并且所述易粘层是包含以下各项的组合物的固化产物：共聚聚酯树脂(A)、含有封端异氰酸酯基团的聚氨酯树脂(B)和有机硅表面活性剂(C)。此外，本发明还提供了一种用于通过在线涂布法制备易粘聚酯膜的方法。

Description

易粘聚酯膜及其制备方法
技术领域
本发明涉及易粘聚酯膜以及用于制备该易粘聚酯膜的制备方法。更具体地，本发明涉及具有较少的在成膜过程期间出现的瑕疵、较少的由在卷筒产品储存期间的紧密卷绕造成的外观缺陷以及出色的对氧化聚合型墨、UV可固化型墨、硬涂层树脂等的粘附性的易粘聚酯膜，并且涉及用于高效地制备该易粘聚酯膜的方法。
背景技术
近年来，更小且更轻的膝上式个人计算机、平板计算机和手机设备的普及显著增加。例如，具有彩色液晶显示器的产品不仅在膝上式个人计算机中，而且在各种产品比如液晶电视机和便携式通信设备(例如平板计算机)中投入实际使用，同时实现了更高的分辨率。
分辨率的提高增加了黑矩阵面积，因此降低了像素开口率。因此，调整背光单元的亮度变得重要。
作为用于提高背光单元的光学效率的方法，例如，已经提出了这样的一种背光：在该背光的光源的光导出表面侧上包括在一个表面上形成有多个棱镜行镜头单元的镜头片或在其上形成有多个透镜行镜头单元的镜头片。
这些镜头片通过经由折射将从背光发射的光朝显示器正面引导而提高正面亮度。镜头片一般通过使用具有出色成形性的透明塑料树脂比如聚碳酸酯树脂、丙烯酸树脂和聚酯树脂作为基材(基膜)获得。特别地，聚酯树脂从其出色的透明度、尺寸稳定性和耐化学性的观点出发而被广泛采用。然而，随着对亮度调节的需求增加，存在加强对膜缺陷的控制的趋势。
双轴拉伸聚酯膜一般通过将聚酯树脂熔融并且挤出以形成片材而获得。将片材通过输送辊运输，并且在膜卷绕方向(MD方向)和宽度方向(TD方向)双轴拉伸。一般使用顺序双轴拉伸法和同时双轴拉伸法作为拉伸方法，并且最广泛地使用顺序双轴拉伸法。在顺序双轴拉伸法中，将膜通过利用输送辊之间的速度差在MD方向上拉伸，然后用拉幅机夹子在TD方向上拉伸。
当膜在成膜过程期间通过输送辊时，输送辊上的外来物可能在膜上形成小的划痕。这样的外来物主要由于在成膜过程期间产生的低聚物和其他物质而存在。为了获得高品质的膜，如专利文献(PTL)1所公开的，提出了诸如定期辊清洁和使用低级低聚物原料的措施。
另外，已经研究了通过在膜表面上设置突起来减少小划痕。对划痕的影响一般对应于SRa(中心面平均粗糙度)，所述SRa是一种表面粗糙度指标；已知SRa越高，对划痕的影响越大。可以通过形成具有三层结构的膜并且将惰性粒子添加到膜表面层的方法在膜表面上设置突起。然而，将惰性粒子添加到膜中，由于树脂和钝性粒子之间的折射率差别而增大了雾度，所述雾度是一种膜透明度的指标；这导致透明度损失。
为了解决这些问题，PTL 2和PTL 3提出了使用具有不同粒度的惰性粒子从而同时实现透明度和耐划性。另外，PTL 4提出了通过大幅减小三层结构的表面层的厚度和减少无助于突起的粒子的数量来提高透明度。
通过诸如PTL 1中所公开的那些的提案已经没有问题地解决了作为光学缺陷的划痕和外来物的减少。然而，具有更高清晰度的显示器已经快速发展，并且据信在过去被认为不是问题的小划痕和外来物将可能被认为是光学缺陷。
另外，由于生产率提高，加工过程和成膜过程中的线速度快速提高，这要求甚至在这样的高速加工条件下减少光学缺陷。为了解决这个问题，如PTL 2至PTL 4中所公开的，进行分析以通过在膜表面上设置突起来减少光学缺陷，比如小划痕。然而，如PTL 2和3中所公开的使用平均粒径为1μm以下的多孔微粒导致微粒团聚，并且粒子不能均匀地分散在树脂中。粒子团聚造成鱼眼(fish-eye)状缺陷。因此，不能将光学缺陷减少到可以解决上述问题的水平。
此外，如果如PTL 4所公开树脂层相对于粒子制作得过薄，则粒子将会在高速加工和成膜期间从树脂层脱落；这是令人担心的原因，因为其可能成为新的光学缺陷的原因。PTL 5中公开的方法(其中将加入到膜中的粒径为2μm以上的非晶态块状二氧化硅的量调整为0.030质量％以下，并且将约0.5μm的粒子加入到易粘层中)在成膜线上不造成划痕。然而，当由于卷筒产品随时间的变化而发生辊的紧密卷绕时，膜中出现微小的错位，由此使粒子从易粘层脱落，导致出现作为外观缺陷的白色不均匀性。
考虑到以上内容，揭示了仍没有稳定获得具有较少的光学缺陷并且可以应对更高的清晰度和提高的生产率的高品质光学膜的措施。
引用清单
专利文献
PTL1：JP2007-130984A
PTL2：JPH10-46012A
PTL3：JPH08-73623A
PTL4：JP2003-231229A
PTL5：JP2011-5648A
发明内容
技术问题
鉴于以上描述的常规领域的问题，本发明所解决的问题是提供一种易粘聚酯膜以及提供一种用于高效地制备所述易粘聚酯膜的方法，所述易粘聚酯膜具有较少的瑕疵，并且其中不存在由于在卷筒产品储存期间的紧密卷绕等引起的外观缺陷。
问题的解决方案
更具体地，本发明提供了以下主题。
1.一种易粘聚酯膜，所述易粘聚酯膜包括作为基膜的聚酯膜和在所述基膜的至少一侧上的易粘层，
其中基于所述基膜的质量，所述基膜含有平均粒径为0.1μm以上且2μm以下的粒子，并且所述粒子的量为基于所述基膜质量的1质量％以下，并且
所述易粘层是包含以下各项的组合物的固化产物：共聚聚酯树脂(A)、含有封端异氰酸酯基团的聚氨酯树脂(B)和有机硅表面活性剂(C)。
2.根据项目1所述的易粘聚酯膜，其中所述易粘层含有平均粒径为20nm以上且200nm以下的粒子。
3.根据项目1或2所述的易粘聚酯膜，其中所述共聚聚酯树脂(A)和所述含有封端异氰酸酯基团的聚氨酯树脂(B)以基于固体计为28/72至72/28的(A)/(B)的质量比存在于构成所述易粘层的所述组合物中。
4.一种用于制备根据项目1至3中任一项所述的易粘聚酯膜的方法，所述方法包括
通过将至少包含共聚聚酯树脂(A)、含有封端异氰酸酯基团的聚氨酯树脂(B)和有机硅表面活性剂(C)的组合物用溶剂稀释来制备涂布液，所述溶剂含有水/醇的质量比为100/0至85/15的水和醇，以及
通过以下方式形成易粘层：在基膜的制备过程期间通过凹面涂布法或棒涂法将所述涂布液涂布到未拉伸膜或单轴拉伸膜的至少一侧，在至少一个未拉伸的单轴方向上拉伸所述膜，以及进行热处理。
发明的有益效果
本发明能够提供一种易粘聚酯膜以及提供一种用于高效地制备所述易粘聚酯膜的方法，所述易粘聚酯膜具有较少的瑕疵，并且其中不存在由于在卷筒产品储存期间的紧密卷绕引起的外观缺陷。
实施方案描述
基膜
构成作为本发明中的基膜的聚酯膜的聚酯树脂的实例包括聚对苯二甲酸乙二醇酯、聚对苯二甲酸丁二醇酯、聚对苯二甲酸丙二醇酯、聚1，2-二苯氧基乙烷-4，4′-二甲酸乙二醇酯和聚2，6-萘二甲酸乙二醇酯。也可以使用通过使作为主要组分的这些树脂的聚合物组分和任何其他酯构成单元共聚获得的共聚聚酯。
基于基膜的质量，基膜优选地含有1质量％以下的量的平均粒径为0.1μm以上且2μm以下的粒子。优选地含有1质量％以下的量的平均粒径在此范围内的粒子以防止在成膜过程中用于进行拉伸和/或干燥的辊上出现瑕疵。优选地含有1质量％以下的量的平均粒径为2μm以下的粒子以降低雾度并且实现出色的透明度。平均粒径优选为1.5μm以下，并且更优选1.0μm以下。粒子含量更优选为0.2质量％以下，特别优选0.1质量％以下，并且最优选0.05质量％以下。粒子含量的下限优选为0.001质量％以上。此下限更优选为但不限于0.005质量％以上。基膜中含有的粒子的类型没有特别限制。实例包括：有机粒子，比如硅氧烷-共聚丙烯酸树脂、交联的聚苯乙烯、聚苯乙烯-二乙烯基苯、聚甲基丙烯酸甲酯、甲基丙烯酸甲酯共聚物、甲基丙烯酸甲酯-共聚交联产物、聚四氟乙烯、聚偏二氟乙烯、聚丙烯腈、苯并胍胺树脂、有机硅树脂和丙烯酸树脂；以及无机粒子，比如二氧化硅、氧化铝、二氧化钛、氧化锆、高岭土、滑石、石墨、碳酸钙、长石、二硫化钼、炭黑和硫酸钡。也可以使用包括由在内部和外部中具有不同性质的材料组成的多层结构的核壳型粒子。二氧化硅粒子由于其作为润滑剂的多种所需性质而是特别优选的。
基膜可以是单轴或双轴拉伸膜。从机械性能等方面考虑，基膜优选为双轴拉伸膜。拉伸方法可以通过同时双轴拉伸进行。然而，优选地使用顺序双轴拉伸膜的制备过程。
本发明的易粘聚酯膜的雾度优选为2％以下。雾度优选为2％以下以在用于光学领域时或在印刷后使用时实现出色的光学特性和外观。雾度更优选为1.5％以下，并且仍更优选1.0％以下。雾度越小越优选；然而，雾度可以是0.1％以上或0.3％以上。
易粘层
在本发明中，在基膜的至少一侧上形成包括共聚聚酯树脂(A)、含有封端异氰酸酯基团的聚氨酯树脂(B)和有机硅表面活性剂(C)的易粘层，以提高对墨、硬涂层材料等的粘附性。在本发明中，使用以下表述：“易粘层是包含以下各项的组合物的固化产物：共聚聚酯树脂(A)、含有封端异氰酸酯基团的聚氨酯树脂(B)和有机硅表面活性剂(C)”。这是因为准确地表达固化后的易粘层的组成非常困难。
在共聚聚酯树脂(A)的聚合中使用的二元醇组分(二醇组分)优选地具有支链结构。支链二元醇组分的实例包括2，2-二甲基-1，3-丙二醇、2-甲基-2-乙基-1，3-丙二醇、2-甲基-2-丙基-1，3-丙二醇、2-甲基-2-异丙基-1，3-丙二醇、2-甲基-2-丁基-1，3-丙二醇、2-甲基-2-正己基-1，3-丙二醇、2，2-二乙基-1，3-丙二醇、2-乙基-2-正丁基-1，3-丙二醇、2-乙基-2-正己基-1，3-丙二醇、2,2-二正丁基-1，3-丙二醇、2-正丁基-2-丙基-1，3-丙二醇和2，2-二正己基-1，3-丙二醇。基于总二元醇组分(总二次组分)，含有优选10摩尔％以上并且更优选20摩尔％以上的比例的上述支链二元醇组分。除了上述化合物以外，共聚聚酯树脂(A)中含有的二元醇组分最优选为乙二醇。也可以组合地使用少量的二甘醇、丙二醇、丁二醇、己二醇、1，4-环己烷二甲醇等。
作为共聚聚酯树脂(A)中的构成组分含有的二羧酸组分最优选为对苯二甲酸和间二甲苯酸。可以加入少量其他二羧酸组分比如脂肪酸二羧酸(例如，己二酸、癸二酸和壬二酸)和芳族二羧酸(例和，二苯基二羧酸和2，6-萘二甲酸)用于共聚。
除了上述二羧酸组分以外，含有磺酸基团的对苯二甲酸或含有磺酸基团的间苯二甲酸以基于总二羧酸组分计在1摩尔％至10摩尔％范围内的量组合使用对于提供水分散性是优选的。例如，可以优选地使用4-磺基间苯二甲酸、磺基对苯二甲酸、5-磺基间苯二甲酸、5-磺基间苯二甲酸钠、4-磺基萘-2，7-二甲酸和5-(4-磺基苯氧基)间苯二甲酸。
含有封端异氰酸酯基团的聚氨酯树脂(B)优选为其中端部异氰酸酯基团被亲水性基团封闭(以下被称为“封端”)的热反应的水溶性聚氨酯。
用于异氰酸酯基团的封端剂的实例包括亚硫酸氢盐、含有磺酸基团的酚、醇、内酰胺、肟和活性亚甲基化合物。封端异氰酸酯基团使聚氨酯预聚物是亲水性或水溶性的。当在成膜过程中的干燥或热定型过程期间将热能施加至含有封端异氰酸酯基团的聚氨酯树脂(B)时，从异氰酸酯基团移除封端剂，由此将混合的共聚聚酯树脂(A)固定在聚氨酯树脂(B)的自交联网络中，同时聚氨酯树脂(B)与共聚聚酯树脂(A)的端基反应。在制备涂布液时的聚氨酯树脂(B)是亲水性的，并且没有足够的耐水性。然而，在涂布、干燥和热定型以完成热反应后，聚氨酯树脂(B)的亲水性基团即封端剂被移除，由此得到具有出色耐水性的涂膜。
上述含有封端异氰酸酯基团的聚氨酯树脂(B)的一个实例是由DKS Co.Ltd.生产的产品名ELASTRON(注册商标)。
当通过将共聚聚酯树脂(A)和含有封端异氰酸酯基团的聚氨酯树脂(B)混合来制备在本发明中使用的涂布液时，共聚聚酯树脂(A)与含有封端异氰酸酯基团的聚氨酯树脂(B)的质量比(A)：(B)优选为28：72至72：28。该质量比优选在此范围内，从而以良好平衡的方式实现例如对墨的易粘附性、对硬涂层材料的易粘附性和雾度。
在本发明中，将有机硅表面活性剂(C)掺入到用于形成易粘层的组合物中。相对于100质量份的共聚聚酯树脂(A)和含有封端异氰酸酯基团的树脂(B)的总固体含量，有机硅表面活性剂(C)的含量可以是例如0.01至0.3质量份。有机硅的结构没有特别限制。可以在本发明的范围内适当地选择加入的有机硅的类型和量，以获得光滑和高度透明的膜表面。由Shin-Etsu Chemical Co.，Ltd.、Dow Corning Toray Co.，Ltd.和Momentive生产的有机硅表面活性剂适合使用。有机硅表面活性剂的使用提高了粒子在涂层中的分散性，并且抑制了粒子聚集。另外，低分子量表面活性剂针对由疏水性粒子或疏水性树脂造成的表面张力变化具有高扩散能力，并且容易保持粒子周围的涂层的厚度。低分子量表面活性剂的这些性质被认为有助于减少粒子的脱落。
有机硅表面活性剂(C)优选为不易受pH变化影响的非离子有机硅表面活性剂。特别地，可以使用聚氧亚烷基改性的有机硅。具体地，有机硅表面活性剂(C)由以下平均组成式(I)表示：
R1xR2ySiO(4-x-y)/2 (I)，
其中
R1是取代或未取代的具有1至10、优选1至8个碳原子并且不含脂族不饱和键的一价烃基，
R2是由通式：-CfH2fO(CgH2gOh)R3(其中R3是氢原子、一价烃基(比如未取代或取代的具有1至8、特别是1至4个碳原子并且不含脂族不饱和基团的烷基)或乙酰基，f是2至12、特别是2至6的整数，g是2至4的整数，并且h是1至200、优选1至100并且仍更优选1至50的整数)表示的有机基团，并且
x和y是各自满足0≤x＜3.0，0＜y＜3.0，以及0＜x+y≤3.0的正值，其中x优选为0.1至2，y优选为0.2至2，并且x+y优选为0.3至3。
另外，聚氧亚烷基改性的有机硅中的聚氧亚乙基含量优选为30质量％至80质量％。
有机硅表面活性剂(C)的实例包括但不限于由以下结构式(1)至(3)表示的那些。
Figure BDA0003188818180000081
聚氧亚乙基含量：47.3质量％
Figure BDA0003188818180000082
聚氧亚乙基含量：54.5质量％
Figure BDA0003188818180000083
聚氧亚乙基含量：55.7质量％
包含上述量的共聚聚酯树脂(A)、含有封端异氰酸酯基团的聚氨酯树脂(B)和有机硅表面活性剂(C)的组合物可以形成没有瑕疵的膜。
在本发明中，易粘层含有平均粒径为20nm以上且200nm以下的粒子，由此容易形成具有较少瑕疵的膜。粒子的平均粒径优选为30nm以上且150nm以下，并且更优选40nm以上且100nm以下。尽管这取决于所形成的易粘层的厚度，但是使用平均粒径为易粘层厚度的三倍以上的粒子是不优选的，因为这由于卷筒产品在紧密卷绕时的周向应力而造成更高的粒子从易粘层脱落的风险。易粘层中含有的粒子的类型没有特别限制。实例包括：有机粒子，比如硅氧烷-共聚丙烯酸树脂、交联的聚苯乙烯、聚苯乙烯-二乙烯基苯、聚甲基丙烯酸甲酯、甲基丙烯酸甲酯共聚物、甲基丙烯酸甲酯-共聚交联产物、聚四氟乙烯、聚偏二氟乙烯、聚丙烯腈、苯并胍胺树脂、有机硅树脂和丙烯酸树脂；以及无机粒子，比如二氧化硅、氧化铝、二氧化钛、氧化锆、高岭土、滑石、石墨、碳酸钙、长石、二硫化钼、炭黑和硫酸钡。也可以使用包括由在内部和外部中具有不同性质的材料组成的多层结构的核壳型粒子。二氧化硅粒子由于其作为润滑剂的各种所需性质而是特别优选的；并且从分散性的观点出发，球形粒子形式的胶体二氧化硅是最理想的。
在本发明中，通过以下方式确定基膜和易粘层中的粒子的平均粒径：用扫描电子显微镜观察膜横截面中的30个粒子，并且获得平均值作为平均粒径。
只要实现了本发明的目的，不规则形状粒子的粒径可以作为具有圆等效直径计算。圆等效直径是通过以下方式得到的值：将所观察的粒子的面积除以π，计算平方根，并且乘以2。
相对于共聚聚酯树脂(A)和含有封端异氰酸酯基团的聚氨酯树脂(B)的100质量份总固体含量，易粘层中含有的粒子的固体含量优选为0.3质量份以上，更优选0.5质量份以上，并且仍更优选1.0质量份以上。固体含量优选为0.3质量份以上，以提高滑溜性(slipperiness)并且容易减少瑕疵。相对于共聚聚酯树脂(A)和含有封端异氰酸酯基团的聚氨酯树脂(B)的100质量份总固体含量，易粘层中的粒子的含量优选为18质量份以下，更优选15质量份以下，并且仍更优选8质量份以下。粒子的含量优选为18质量份以下，以降低雾度并且提供透明度。
易粘层的厚度可以是例如5nm至500nm，优选10nm至300nm，并且更优选20nm至150nm。
在本发明的聚酯系层压膜中，用于堆叠易粘层的方法没有特别限制；可以使用在线涂布或离线涂布，其中使用双轴拉伸聚酯膜进行加工。任何涂布方法都是适用的，只要其是已知的。优选地使用在线涂布法，通过所述在线涂布法，通过以下方式高效地获得膜：通过用溶剂稀释包含共聚聚酯树脂(A)、含有封端异氰酸酯基团的聚氨酯树脂(B)和有机硅表面活性剂(C)的组合物得到涂布液，在基础聚酯膜的制备过程期间用凹面涂布法或棒涂法将所得到的涂布液涂布至未拉伸膜或单轴拉伸膜；并且在至少一个未拉伸的单轴方向上拉伸膜，然后热定型。所得易粘聚酯膜具有出色的对各种墨、特别是UV可固化墨和氧化聚合型(或溶剂型)墨的粘附性，并且还适用于二次加工，比如标记。
用于涂布液的溶剂可以是水或水与醇的混合溶剂。水与醇的质量比即水/醇优选地选自100/0至85/15的范围。当醇的质量基于水和醇的总质量为15质量份以下时，可以容易地通过使用通用双轴拉伸成膜装置制备膜。水/醇的质量比理想地在98/2至90/10的范围内，以通过加入醇来控制涂布液的表面张力，并且由此容易地调整易粘层的外观。
在本发明中，如上适合使用所述凹面涂布法或棒涂法，并且可以用通用双轴拉伸成膜装置制备具有较少瑕疵的高透明度易粘膜。
为了减少在成膜期间形成划痕，理想的是使从涂布到卷绕所使用的辊的数量最小化。因此，理想的是在不使用辊的情况下从涂布过程转向干燥过程，并且在干燥炉中连续地进行干燥过程到热定型过程。
实施例
以下参照具体实施例描述本发明。然而，本发明不限于这些实施例。首先，描述本发明中使用的评价方法。
评价方法
(1)墨粘附性的评价
在之后描述的实施例和比较例中获得的各易粘聚酯膜的易粘层上，使用250目丝网对氧化聚合(或溶剂)型墨进行丝网印刷，并且将其风干一天；或者使用300目丝网对UV固化型墨进行丝网印刷，并且通过利用UV暴光机的500mj/em2的UV暴光进行固化。接下来，使用切割刀横切各个带墨表面以形成具有100个方形(2mm×2mm)的网格，并且将Cellophane(注册商标，Nichiban Co.，Ltd.)胶带(宽度：25mm)粘附至表面，使得在胶带下不出现气泡。另外，摩擦胶带表面以充分粘贴。然后，在用手按压未粘附Cellophane(注册商标)胶带的带墨表面的前端和后端的同时，在从胶带向上的方向(90度角的方向)上将胶带快速剥离。观察剥离后的带墨表面，以基于墨残留百分比评价粘附性。
使用的墨品牌
1)氧化聚合(或溶剂)型墨
(a)RAM，黑色，由Seiko advance Ltd.生产
(b)用于PVC的SS-8，白色，由Toyo Ink Co.，Ltd.生产
2)UV固化型墨
(c)FDSS，黑色，由Toyo Ink Co.，Ltd.生产
(d)UVA，黑色，由Seiko advance Ltd.生产
评价：
在剥离横切表面后，根据以下四种标准来评价墨残留百分比。
A：残留百分比为100％；完全没有剥离
B：残留百分比为90％以上；实际使用中没有问题
C：残留百分比为80％以上；可以通过调整条件来使用
D：残留百分比低于80％；不能使用
(2)对硬涂层材料树脂的粘附性的评价
将以下描述的硬涂层涂布液A用线-棒涂布机涂布至各易粘聚酯膜的易粘层，使得干燥后的涂层厚度为2μm，用在80℃温度的热空气干燥60秒，并且使其以10m/min的速度通过在输出为120W/cm2的高压汞灯下方20cm的位置，由此得到硬涂层膜。硬涂层膜的折射率为1.48。
通过以下方式获得涂布液：将以下所示质量比的以下材料混合，并且将所得混合物搅拌30分钟以上以进行溶解。
然后，使用标称过滤精度为1μm的过滤器移除未溶解的物质以制备硬涂层涂布液A。
涂布液A
-甲乙酮：64.48质量％
-季戊四醇三丙烯酸酯：11.45质量％(由Shin-Nakamura Chemical Co.，Ltd.生产，NK Ester A-TMM-3LM-N，官能团数量：3)
-三丙二醇二丙烯酸酯：5.73质量％(由Shin-Nakamura Chemical Co.，Ltd.生产，NK Ester APG-200，官能团数量：2)
-甲基丙烯酸二甲基氨基乙酯：5.72质量％(由Kyoeisha Chemical Co.，Ltd.生产，Light Ester DM，官能团数量：1)
-二氧化硅粒子：11.45质量％(由Nissan Chemical Corporation生产，MEK-ST-L，固体含量：30质量％，平均粒径：50nm)
-光聚合引发剂：1.14质量％(由Ciba Specialty Chemicals生产，Irgacure184)
-有机硅表面活性剂：0.03质量％(由Dow Coming Toray Co.，Ltd.生产，DC57)
具体地，使用空隙间隔为2mm的刀具引导件制作通过硬涂层到达基膜的切口，以在得到的硬涂层上形成具有100个方形的网格。接下来，将Cellophane胶带(Nichiban Co.，Ltd.，No.405，宽度：24mm)施加至网格形式的切割表面，并且用橡皮擦进行摩擦以确保完全粘附。然后，将Cellophane胶带垂直地从硬涂层膜的硬涂层表面剥离，并且对从基膜的硬涂层表面剥离的方形的数量进行目视计数以根据下式确定硬涂层和基膜之间的粘附性。部分剥离的方形也作为剥离进行计数，并且根据以下标准将结果分类为四种等级。
粘附性(％)＝(1-剥离掉的方形数量/100)×100
A：100％
B：90％以上且低于100％
C：80％以上且低于90％
D：低于80％
(3)易粘聚酯膜的雾度
根据JIS K 7136：2000使用浊度计(由Nippon Denshoku Industries Co.Ltd.制造，NDH2000)测量各易粘聚酯膜的雾度。
(4)瑕疵的评价
将具有易粘层的膜切割为A4尺寸，并且用溴光(brom light)照射。之后，对0.5mm以上的划痕进行计数。评价基于以下标准。
A：0
B：1至5
D：6以上
(5)白色不均匀性的评价
为了再现卷芯的加压状态，将具有易粘层的膜切割为10-cm见方的片；并且将一组10个片材的顶部和底部夹在5-mm厚的SUS板之间，并且在50kg/cm2的加压压机中保持24小时。然后，评价膜外观。评价基于以下标准。
A：与处理前相比没有变化
B：在5％以下的面积中观察到发白(白色不均匀性)
C：在10％以下的面积中观察到发白(白色不均匀性)
D：在超过10％的面积中观察到发白(白色不均匀性)
实施例1
(1)涂布液的制备
根据以下方法制备本发明中使用的涂布液。具体地，将95质量份的对苯二甲酸二甲酯、95质量份的间苯二甲酸二甲酯、35质量份的乙二醇、145质量份的新戊二醇、0.1质量份的乙酸锌和0.1质量份的三氧化锑放入反应容器中以在180℃进行酯交换反应3小时。接下来，将6.0质量份的5-磺基间苯二甲酸钠加入其中以在240℃进行酯化反应1小时，然后在250℃在减压(10至0.2mmHg)下进行缩聚反应2小时，由此得到数均分子量为19,500并且软化点为60℃的共聚聚酯树脂(A)。
将64质量份的所得共聚聚酯树脂、144质量份的丁基溶纤剂和114质量份的水在加热下搅拌6小时以上，得到固体浓度为30％的均匀的淡白色水分散体。
将如上所述得到的共聚聚酯树脂(A)、含有封端异氰酸酯基团的可自交联聚氨酯树脂(由DKS Co.Ltd.生产，ELASTRON(注册商标)H-3DF)(B)、有机硅表面活性剂(由DowCorning Toray Co.，Ltd.生产，67 Additive)(C1)和胶体二氧化硅(由Nissan ChemicalCorporation生产，SNOWTEX OL，平均粒径：40nm)(P1)以基于固体计50/50/0.1/5的(A)/(B)/(C1)/(P1)的质量比分散在溶剂中，以形成固体含量为7质量％的涂布液(X)。此处使用的溶剂通过将水和异丙醇以95/5的比率混合得到。
(2)层压聚酯膜的制备
作为原料聚合物，将不含粒子且特性粘度为0.62dl/g的聚对苯二甲酸乙二醇酯树脂粒料在减压(133.3Pa)下在135℃干燥6小时。然后，将聚对苯二甲酸乙二醇酯树脂放入挤出机I中，同时将通过将0.10％的平均粒径为1.5μm的二氧化硅粒子加入到相同聚对苯二甲酸乙二醇酯中得到的树脂粒料放入挤出机II中，将它们在285℃熔融挤出，使得II/I/II的厚度比＝5/90/5。将膜在金属辊上在25℃的表面温度淬火并且凝固以得到流延膜。
将所得流延膜用热辊组和红外加热器加热至95℃，并且使用凹面涂布机将涂布液X涂布至以40m/min的速度行进的单轴拉伸PET膜的一侧。将所涂布的涂布液X的量调整至0.08g/m2的最终固体含量。随后，将所得产物在拉幅机中在120℃在横向上拉伸4倍，然后在相同拉幅机中在220℃进行热处理，同时在横向上松弛(3％)，由此得到整体膜厚度为50μm的易粘聚酯膜。易粘层的厚度为80nm。
实施例2至5
除了如表1所示将共聚聚酯树脂(A)与含有封端异氰酸酯基团的聚氨酯树脂(B)的基于固体计的质量比改变为30/70、70/30、25/75或75/25以外，以与实施例1中相同的方式来获得易粘聚酯膜。
实施例6至8和比较例1
除了如表1所示将涂布液中的有机硅表面活性剂(C1)改变为由Shin-EtsuChemical Co.，Ltd.生产的KF-6012(C2)、由Momentive生产的L-77(C3)或由Dow CorningToray Co.，Ltd.生产的502 Additive(C4)，或者不使用表面活性剂以外，以与实施例1中相同的方式来获得易粘聚酯膜。
比较例2和实施例9
除了如表1所示将涂布液中的有机硅表面活性剂(C1)改变为由DIC生产的氟表面活性剂F-470(C5)并且改变其量以外，或者除了将相同有机硅表面活性剂(C1)的量提高5倍以外，以与实施例1中相同的方式来获得易粘聚酯膜。
实施例10和11
除了如表1所示将涂布液中的胶体二氧化硅(P1)改变为由Nissan ChemicalCorporation生产的SNOWTEX ZL(P2，平均粒径：100nm)或由Nissan Chemical Corporation生产的MP2040(P3，平均粒径：200nm)并且改变其量以外，以与实施例1中相同的方式来获得易粘聚酯膜。P2和P3如同P1一样均为二氧化硅粒子。
实施例12和13
除了如表1所示将涂布液中的胶体二氧化硅(P1)的量改变为基于共聚聚酯树脂(A)和含有封端异氰酸酯基团的聚氨酯树脂(B)的总固体含量的质量的20质量份或0.2质量份以外，以与实施例1中相同的方式来获得易粘聚酯膜。
实施例14至17和比较例3
除了如表1所示改变基膜中的聚对苯二甲酸乙二醇酯中含有的粒子的平均粒径和量以外，以与实施例1中相同的方式来获得易粘聚酯膜。
实施例18和19以及比较例4
除了如表1所示将基膜改变为仅有挤出机II(其中放有通过将0.10％的平均粒径为0.5μm的二氧化硅粒子加入到聚对苯二甲酸乙二醇酯中得到的树脂粒料)所获得的层的单层、仅有挤出机II(其中放有通过加入0.02％的平均粒径为0.8μm的二氧化硅粒子得到的树脂粒料)所获得的层的单层或者仅有挤出机I(其中仅放有聚对苯二甲酸乙二醇酯树脂)所获得的层的单层以外，以与实施例1中相同的方式来获得易粘聚酯膜。
以下表1和2示出了实施例和比较例的成膜条件和评价结果。
表1
Figure BDA0003188818180000161
/>
Figure BDA0003188818180000171
-共聚聚酯树脂(A)的含量(质量份)和含有封端异氰酸酯基团的聚氨酯树脂(B)的含量各自按固体且相对于(A)和(B)的100质量份总固体含量计算。
-易粘层中的有机硅表面活性剂(C)的含量(质量份)和粒子(P)的含量各自按固体且相对于共聚聚酯树脂(A)和含有封端异氰酸酯基团的聚氨酯树脂(B)的100质量份总固体含量计算。
表2
Figure BDA0003188818180000181
工业实用性
本发明能够提供一种易粘聚酯膜以及提供一种用于高效地制备所述易粘聚酯膜的方法，所述易粘聚酯膜具有较少的瑕疵，并且其中不存在由于在卷筒产品储存期间的紧密卷绕引起的外观缺陷。

Claims (3)

1.一种易粘聚酯膜，所述易粘聚酯膜包括作为基膜的聚酯膜和在所述基膜的至少一侧上的易粘层，
其中基于所述基膜的质量，所述基膜含有平均粒径为0.1μm以上且1.5μm以下的粒子，并且所述粒子的量为基于所述基膜质量的0.001质量％以上且1质量％以下，
所述易粘层是包含以下各项的组合物的固化产物：共聚聚酯树脂(A)、含有封端异氰酸酯基团的聚氨酯树脂(B)和有机硅表面活性剂(C)，
所述有机硅表面活性剂(C)是聚氧亚烷基改性的有机硅并且在所述聚氧亚烷基改性的有机硅中的聚氧亚烷基含量为30-80质量％，并且
所述共聚聚酯树脂(A)和所述含有封端异氰酸酯基团的聚氨酯树脂(B)以基于固体计为28/72至72/28的(A)/(B)的质量比存在于构成所述易粘层的所述组合物中，并且相对于100质量份的所述共聚聚酯树脂(A)和所述含有封端异氰酸酯基团的树脂(B)的总固体含量，所述有机硅表面活性剂(C)的含量为0.01至0.3质量份。
2.根据权利要求1所述的易粘聚酯膜，其中所述易粘层含有平均粒径为20nm以上且200nm以下的粒子。
3.一种用于制备根据权利要求1或2所述的易粘聚酯膜的方法，所述方法包括
通过将至少包含共聚聚酯树脂(A)、含有封端异氰酸酯基团的聚氨酯树脂(B)和有机硅表面活性剂(C)的组合物用溶剂稀释来制备涂布液，所述溶剂含有水/醇的质量比为100/0至85/15的水和醇，以及
通过以下方式形成易粘层：在基膜的制备过程期间通过凹面涂布法或棒涂法将所述涂布液涂布到未拉伸膜或单轴拉伸膜的至少一侧，在至少一个未拉伸的单轴方向上拉伸所述膜，以及进行热处理。
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