CN101981476B - 用于多层光学膜的底漆层 - Google Patents

用于多层光学膜的底漆层 Download PDF

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CN101981476B
CN101981476B CN200980111535.3A CN200980111535A CN101981476B CN 101981476 B CN101981476 B CN 101981476B CN 200980111535 A CN200980111535 A CN 200980111535A CN 101981476 B CN101981476 B CN 101981476B
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film
optical
layer
prime coat
polyester
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CN101981476A (zh
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詹姆斯·E·洛克里奇
汉·K·洛伊
马克·J·佩莱里蒂
杰弗里·A·彼得森
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3M Innovative Properties Co
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Abstract

本发明公开了一种光学制品，所述光学制品包括多层光学膜和设置在所述多层光学膜上的底漆层。所述底漆层基本上由磺基聚酯和交联剂组成。所述多层光学薄膜可以是反射膜、偏振膜、反射偏振膜、漫射混合反射式偏振膜、漫射膜、增亮膜、转向膜、镜膜或它们的组合。可将微结构化的光学层或非结构化的光学层设置在与所述多层光学膜相对的所述底漆层上。本发明还公开了一种制备所述光学制品的方法。本发明还公开了一种包括所述光学制品的显示装置。

Description

用于多层光学膜的底漆层
技术领域
本发明涉及用于光学膜的涂层，更具体地讲，涉及用于多层光学膜的底漆层。
背景技术
在聚合物膜领域中，通常遇到这样的问题：难以在基底与涂敷到其上的功能性涂层之间提供强粘附力。就聚酯基基底而言，这种情况尤为突出。要解决该问题，通常需要将底漆层或涂层涂敷到聚酯基底上，以改善基底与功能性涂层之间的粘附力。对于具有设置在多层光学膜上的微结构化表面层的光学膜，在其制造过程中，常常遇到尤其难粘附的问题。通过将紫外固化性丙烯酸类树脂涂敷在多层光学膜上，随后再将树脂压在微结构化辊上使其固化，从而形成微结构化表面层。
发明内容
本文公开了一种光学制品，其包括：多层光学膜以及设置在多层光学膜上的底漆层，底漆层基本上由磺基聚酯和交联剂组成。在一些实施例中，多层光学膜包括反射膜、偏振膜、反射偏振膜、漫射混合反射式偏振膜、漫射膜、增亮膜、转向膜、镜膜或它们的组合。在一些实施例中，微结构化层可设置在与多层光学膜相对的底漆层上。本文还公开了一种制备光学制品的方法。本文还公开了一种包括光学制品的显示装置。
本发明的这些方面和其他方面在以下“具体实施方式”中描述。上述发明内容不应理解为是对要求保护的主题的限制，该主题仅受本文所示出的权利要求的限定。
附图说明
结合以下附图和以下具体实施方式可以更加全面地理解本发明。
图1和图2示出了示例性光学制品的示意性剖视图。
具体实施方式
本文公开了可用来促进多层光学膜与另一层之间的粘附力的底漆层。例如，底漆层可用于将聚酯基多层光学膜粘附到由辐射固化材料制成的层上。辐射固化材料包括非卤化材料和卤化材料。该底漆层还可以具有其他优势，因为它可以由水基组合物而非溶剂型组合物形成，并且不含有机卤素官能团。
从制造的观点看来，本文所公开的底漆层也具有优势。在多层光学膜的典型制造过程中，可以在一个或两个维度上对膜进行拉幅或拉伸操作，以对膜进行取向。本文所公开的底漆层可以在拉幅或拉伸操作前在多层光学膜上形成。这个拉幅前底漆处理从加工观点来看是合乎需要的，因为它使得不需要单独的涂覆步骤。相比之下，许多用来增强粘附力的已知材料(包括聚合物和粒子)是不容易拉幅的，所述拉幅可包括高温和任何地方的2∶1、4.5∶1或甚至6∶1或更高的拉伸比。
本文所公开的底漆层的另一个优点是可被设计为具有理想的光学性质，例如低雾度和高透光率。例如，在合适的多层光学膜上形成底漆层时，该膜可表现出最低的雾度，例如小于约10％、小于5％、或小于1％。而已知的底漆组合物通常难以实现如此低的雾度，因为在一些情况下，要使粘附力足够强，只能通过使用会带来不可取雾度水平的厚层或在拉伸膜基底时会断裂的涂层来实现。造成不可取雾度的另一个原因是表面粗糙度，它可由与干燥相关的现象(例如起斑和去湿)以及拉幅时的涂层断裂而引起。使用水基涂层配方时，这些问题会特别严重，因为(例如)在干燥过程中会产生表面张力梯度。如果需要，当在合适的多层光学膜上形成底漆层时，该膜可表现出最大的透光率，例如大于90％。一般来讲，经涂覆的多层光学膜有利地为无色的。通过具有这些特性，经涂覆的多层光学制品适用于其中可对光进行管理、增强、操纵、控制、维持、透射、反射、折射、吸收等的光学应用中。下文将对光学应用进行更详细的描述。
图1示出了本文所公开的示例性光学制品的剖视图。光学制品10包括具有第一光学层14和第二光学层16的多个交替层的多层光学膜12。在多层光学膜的外表面上形成底漆层18。底漆层可具有任何适宜的厚度，前提条件是它可以提供所需的粘附力而不会影响光学特性。通常，底漆层足够厚以提供如下所述的所需粘附力，同时又足够薄使得不会影响光学制品的光学性质。在一些实施例中，约30nm至约500nm的厚度是可用的。在一些实施例中，底漆层的厚度为约50nm至约250nm，或约175nm至约225nm。
底漆层可具有至少约50℃的玻璃化转变温度(Tg)。如果底漆层的Tg过低，则底漆层可能会发粘；如果底漆层太软并容易被随后包覆的紫外固化性树脂溶解，则层间粘附力可能不佳。如果底漆层的Tg过高，则可能无法良好地成膜；如果涂层过于呈玻璃态，以至于不能被包覆的紫外固化性树脂渗透或溶胀，则层间粘附力可能不佳。ASTM D 3359是熟知的用来测量两个层之间的粘合力的方法。
底漆层包含磺化聚酯。如本文所用，术语聚酯指由单一一种二羧酸酯单体和单一一种二醇单体制成的聚酯，同时也指由一种以上的二羧酸酯单体和/或一种以上的二醇单体制成的共聚酯。一般来讲，聚酯是由二羧酸酯单体的羧酸酯基团与二醇单体的羟基缩合而制备的。如本文所用，术语“二羧酸酯”和“二羧酸”可互换使用，并且包括具有1至10个碳原子的低级烷基酯。如本文所用，二醇单体包括那些具有两个或更多个羟基的单体，例如二醇、三醇、四醇和五醇。通常，可用的磺化聚酯包括具有水溶性和水分散性的那些。可用的磺化聚酯的分子量足够高，以使得经过如下所述的涂敷、干燥和拉伸后所得的底漆层不易碎裂。可用的分子量可为约8000至约50000。US 4,480,085(Larson)中所述的无定形磺基聚酯会是可用的。US 5,427,835(Morrison等人)中所述的磺基聚酯也是可用的。
磺化聚酯包含至少一个具有一个或多个磺酸酯侧基的二羧酸酯单体。磺酸酯侧基是不参与形成聚酯主链的聚合反应的基团。磺化二羧酸酯单体的例子包括以下酸的磺化衍生物：萘二甲酸；对苯二甲酸；邻苯二甲酸；间苯二甲酸；马来酸；衣康酸；壬二酸；己二酸；癸二酸；琥珀酸；谷氨酸；降冰片烯二羧酸；二环辛烷二羧酸；1，6-环己烷二羧酸；叔丁基间苯二甲酸；偏苯三酸；4，4’-二苯基二羧酸；蒽二羧酸；和十六碳二酸。任何磺化二羧酸酯单体都可被分子量小于约80并且在聚合反应中为惰性的基团取代。惰性侧基的例子包括卤素、氰基、硝基、具有1至4个碳原子的低级烷基和烷氧基，以及苯基。其他二羧酸酯单体由Larson进行过描述。磺酸酯侧基可以通过以下方法引入：将磺酸酯侧基接枝到聚酯的侧链上，作为聚酯的端基封端，或在形成聚酯的聚合反应中包括具有磺化侧基的单体。
在水溶液中，每个磺酸酯基团都可以未中和的磺酸形式存在，或与可以为无机或有机抗衡离子的抗衡离子缔合。无机抗衡离子的例子包括铵、钠、钾、锂、锌、镁、钙、钴、铁、铝和锑抗衡离子，以及它们的组合。有机抗衡离子的例子包括含C2-C20-的抗衡离子。优选的有机抗衡离子包括：具有烷基取代基(独立地具有1至8个碳原子)的单烷基铵、二烷基铵、三烷基铵和四烷基铵，取代的鏻
Figure BPA00001232759100041
和未取代的鏻
Figure BPA00001232759100042
以及可任选地被含有1至8个碳原子的烷基取代的杂环含氮阳离子(例如吡啶
Figure BPA00001232759100043
吗啉和咪唑
Figure BPA00001232759100045
)。
可用的磺化聚酯通常含有至少两种二羧酸酯单体：其中一种为上述磺化二羧酸酯单体，另一种为未磺化二羧酸酯单体。可使用的未磺化二羧酸酯单体包括上述用于磺化衍生物的那些中的任一种。
对磺化聚酯中磺化二羧酸酯单体的量并无特别限制。通常，必须使用最小量的磺化二羧酸酯单体，以使得磺化聚酯作为纳米尺度的粒子时为水溶性的或水分散性的。因此，磺化二羧酸酯单体的最小量不仅会取决于磺化聚酯分子量之类的因素，还会取决于构成磺化聚酯的其他单体。要避免底漆溶液在涂覆之前或之后出现不相容问题，需对磺化聚酯中磺化二羧酸酯单体的量进行选择。通常，底漆溶液会需要具有至少24小时的适用期，这意味着在24小时后该溶液不会出现任何肉眼可见的变化。在一个实例中，对应100摩尔的二羧酸酯和二醇单体组合物，磺化聚酯包含0.25至15摩尔的磺化二羧酸酯单体。
磺化聚酯可包含一种或多种二醇单体。通常，可使用脂肪族二醇；例子包括1，3-丙二醇、1，4-丁二醇、1，5-戊二醇、1，6-己二醇、1，10-癸二醇、三羟甲基丙烷、2，3-二羟甲基丙烷、1，4-二羟基-2，3-二甲基丁烷、1，4-环己烷二甲醇、1，4-苯二甲醇、新戊二醇、乙二醇、丙二醇、聚乙二醇、三环癸烷二醇、降莰烷二醇、二环辛二醇、季戊四醇、双酚A和1，3-双(2-羟基乙氧基)苯。还可使用分子量最高为约1000的聚合物二醇，例如聚(己内酯)二醇。其他二醇单体由Larson进行过介绍。
磺化聚酯的具体例子包括EASTEK 1100(Eastman Chemical Co.)以及由间苯二甲酸、和磺基间苯二甲酸钠与乙二醇、二甘醇、和新戊二醇或1，4-环己烷二甲醇的缩聚物合成的那些。例如，可用的磺化聚酯可包含：一种或多种二羧酸单体，其选自磺化间苯二甲酸、间苯二甲酸、和对苯二甲酸；以及一种或多种二醇单体，其选自乙二醇、二甘醇、新戊二醇、和1，4-环己烷二甲醇。在另一个例子中，可用的磺化聚酯可包含5-磺酸钠间苯二甲酸、对苯二甲酸、间苯二甲酸、乙二醇、和新戊二醇。
底漆层包含三聚氰胺-甲醛交联剂，这种交联剂通常为衍生自三聚氰胺和甲醛的树脂。三聚氰胺-甲醛交联剂的具体例子包括CYMEL 301和327(Cytec Industries)。交联剂用于改善丙烯酸酯树脂的机械稳定性和化学耐久性，以及底漆层的粘附性。交联剂的具体选择及其用量取决于多种因素，例如：在涂覆和/或固化底漆层之前或之后底漆层中交联剂与其他组分的相容性、所需的底漆层厚度、聚合反应条件、成本等。
可按照任何相对的量使用磺基聚酯和交联剂，只要所得的底漆层具有所需的性质即可。相对量可取决于具体使用的磺基聚酯和交联剂，以及底漆层的厚度和制品的预期用途。要避免底漆溶液在涂覆前后出现不相容的问题，还需对相对量进行选择。通常，底漆溶液会需要具有至少24小时的适用期，这意味着在24小时的时间段后该溶液不会出现任何肉眼可见的由相分离、沉淀或胶凝作用产生的变化。磺基聚酯和交联剂在底漆层中还必须相容。例如，可以使用1∶1至20∶1的磺基聚酯和交联剂比率。
底漆层还可包含至少一种催化剂或者热活化和/或光活化的潜在催化剂，以促进固化和交联。可用的酸性催化剂和潜在酸性催化剂的例子，特别是可用于基于三聚氰胺-甲醛的可交联体系的催化剂，包括对甲苯磺酸及其衍生物，如CYCAT 4040和4045(Ciba Specialty Chemicals)。其他可用催化剂的例子包括无机酸如盐酸、磷酸和硝酸、它们的胺盐，以及羧酸和它们的胺盐。催化剂还可以是聚合物物质，例如聚丙烯酸及其铵盐。可用的光活化酸性催化剂的例子包括强酸(如三氟甲磺酸)的碘
Figure BPA00001232759100051
盐和锍盐。一般来讲，所用的催化剂或催化剂前体的量小于总涂覆固形物的约4重量％。
底漆层和涂层组合物可以包含其他类型的添加剂。优选地，此类材料应与涂层和涂层配方的主要组分相容，且不应对光学制品的性能属性造成不利影响。这些材料包括涂层助剂，例如表面活性剂和聚结溶剂；消泡剂；用作(例如)增滑剂的颗粒；抗氧化剂；以及pH值控制剂，例如缓冲剂或三烷基胺。对于包含三聚氰胺-甲醛交联剂的涂层配方，使用挥发性相对较高的三烷基胺如三乙胺和二甲基乙醇胺作为pH稳定剂是特别优选的，因为pH偏移到酸性范围会造成不期望的适用期缩短和过早胶凝。
本文还公开了一种制备底漆制品的方法。该方法包括将上述底漆组合物涂覆到基底上，从而形成经涂覆的基底。通常，将底漆组合物中的组分溶解、分散或悬浮于合适的溶剂中，以用于涂覆步骤。具体使用的溶剂取决于具体的组分、所需的组分浓度、所需的层厚度和性质、所采用的涂覆方法等。合适的溶剂包括水。通常，相对于总组合物的重量而言，用来形成底漆层的组合物包含最多约50重量％的固形物。
底漆组合物可用多种涂覆技术来涂覆，如浸涂、辊涂、模涂、刮刀涂布、气刀刮涂、槽式涂布、坡流涂布、缠线棒涂布和帘式涂布。关于涂布技术的综论可见于Cohen，E.and Gutoff，E.Modern Coating andDrying Technology；VCH Publishers：New York，1992；p.122(Cohen，E.和Gutoff，E.，《现代涂布与干燥技术》，VCH Publi shers：NewYork，1992年，第122页)；Tricot，Y-M.Surfactants：Static andDynamic Surface Tension.In Liquid Film Coating；Kistler，S.F.and Schweizer，P.M.，Eds.；Chapman & Hall：London，1997；p.99(Tricot，Y-M.，表面活性剂：静态与动态表面张力；《液体薄膜涂布》，Kistler，S.F.和Schweizer，P.M.编辑，Chapman & Hall：London，1997年，第99页)。
底漆组合物可用热或紫外辐射或任何其他合适的固化技术进行固化。固化的一个优选方法为使用膜拉幅过程的潜热对底漆涂层进行热活化和交联。
多层光学膜可以包含多种材料的任何一种，这些材料包括聚酯，例如聚对苯二甲酸乙二醇酯、聚萘二甲酸乙二醇酯、基于萘二羧酸的共聚酯或聚酯共混物；聚碳酸酯；聚苯乙烯；苯乙烯-丙烯腈；乙酸纤维素；聚醚砜；聚(甲基)丙烯酸酯，例如聚甲基丙烯酸甲酯；聚氨酯；聚氯乙烯；聚环烯烃；聚酰亚胺；玻璃；纸张；或它们的组合物或共混物。具体的实例包括聚对苯二甲酸乙二醇酯、聚甲基丙烯酸甲酯、聚氯乙烯、和三乙酸纤维素。优选的实例包括聚对苯二甲酸乙二醇酯、聚萘二甲酸乙二醇酯、三乙酸纤维素、聚丙烯、聚酯、聚碳酸酯、聚甲基丙烯酸甲酯、聚酰亚胺、聚酰胺、或它们的共混物。优选地，多层光学膜足够耐温度和老化，使得制品的性能不会随时间推移而降低。多层光学膜的厚度通常小于约2.5mm。多层光学膜也可以为可取向膜，例如在拉幅操作中于取向前涂布的浇铸料片基底。
多层光学膜适用于光学应用。可用的多层光学膜被设计用于控制光线流。它们可以具有大于约90％的透射率和小于约5％(例如小于2％或小于1％)的雾度值。选择合适的多层光学膜时要考虑的性质包括机械性能，例如柔韧性、尺寸稳定性、自支承性、和抗冲击性。例如，多层光学膜可能需要具有足够的结构强度，使得可将制品组装成显示装置的一部分。
多层光学膜可用于广泛的应用中，例如图形艺术和光学应用。可用的多层光学薄膜可被描述为反射膜、偏振膜、反射偏振膜、漫射混合反射式偏振膜、漫射膜、增亮膜、转向膜、镜膜、或它们的组合。多层光学膜可以具有10层或更少的层、数百层或甚至数千层，这些层由全部的双折射光学层、一些双折射光学层或全部的各向同性光学层的一些组合构成。在一个实施例中，多层光学膜具有第一光学层和第二光学层的交替层，其中第一光学层和第二光学层具有沿至少一条轴线相差至少0.04的折射率。具有不一致的折射率的多层光学膜在下文所引用的参考文献中有所描述。在另一个实施例中，多层光学膜可以包括上述任何多层光学膜中的一层或多层，使得底漆层埋在其中任何一层中，从而使制品本身成为反射膜、偏振膜、反射偏振膜、漫射混合反射式偏振膜、漫射膜、增亮膜、转向膜、镜膜或它们的组合。
可用的多层光学膜包括均可得自3M公司的、以VikuitiTM双增亮膜(DBEF)、VikuitiTM增亮膜(BEF)、VikuitiTM漫反射式偏振膜(DRPF)、VikuitiTM增强型镜面反射器(ESR)和VikuitiTM高级偏振膜(APF)销售的光学膜。可用的光学膜还在下列专利中有所描述：U.S.5,825,543、5,828,488(Ouderkirk等人)、5,867,316、5,882,774、6,179,948B1(Merrill等人)、6,352,761B1、6,368,699B1、6,927,900B2、6,827,886(Neavin等人)、6,972,813B1(Toyooka)、6,991,695、2006/0084780A1(Hebrink等人)、2006/0216524A1、2006/0226561A1(Merrill等人)、2007/0047080A1(Stover等人)、WO 95/17303、WO95/17691、WO95/17692、WO 95/17699、WO 96/19347、WO 97/01440、WO99/36248和WO99/36262。这些多层光学膜仅为示例性的，并不旨在穷举可用的合适的多层光学膜。在这些实施例的一些中，本发明的底漆层可以为多层膜构造中的内层。
在多层光学膜上形成底漆层后，接着可以在一个或两个维度上对涂覆的膜进行拉幅或拉伸操作，以对膜进行取向。对膜(特别是聚酯膜)进行取向的方法见述于第2版“The Encyclopedia of Polymer Science andEngineering”(聚合物科学与工程百科全书)的第12卷第193至216页。制造双轴取向的聚酯膜的典型方法包括以下四个主要步骤：(1)熔融挤出聚酯树脂并将其骤冷以形成幅材，(2)在纵向方向上拉伸该幅材，(3)随后或者同时在横向方向上拉伸该幅材以产生膜；和(4)将该膜进行热定型。如果需要双轴取向，可在多层光学膜已在纵向上拉伸之后但在随后在横向方向上拉伸之前，将底漆组合物涂覆到多层光学膜上。有关聚合物膜的取向的更多讨论可见于WO 2006/130142和前面引述的关于光学膜的参考文献中。在制备多层光学膜的过程中，拉伸比通常在6∶1或更高的范围内，明显高于在制备一体化聚对苯二甲酸乙二醇酯膜时常用的3.5∶1-4∶1。本发明的底漆不同于本领域中使用的许多底漆，据发现，使用这种底漆后，即便以6∶1的比率拉伸后，也可得到具有极佳透明性、美观度和粘附性的涂层。
在一些实施例中，光学制品包括增亮膜。在该实施例中，将微结构化层设置在与多层光学膜相对的底漆层上，其中该微结构化层包括具有多个微结构的结构化表面，而该结构化表面包括制品的外表面。图2示出了这样的示例性光学制品20的横截面示意图，其中该光学制品20具有设置在底漆层18上的微结构化层22。微结构化层具有微结构化表面24，微结构化表面24包括用于导光的棱镜阵列。关于光在增亮薄膜中的行为的综论可见于(例如)US 2007/0115407A1(Richard等人)。
在一些实施例中，光学制品包括设置在与多层光学膜相对的底漆层上的基底。基底的例子包括那些可用于光学应用的任何基底，例如聚酯、聚碳酸酯、聚(甲基)丙烯酸酯基底，其中任何一个都可以为取向的或未取向的。
多个微结构可以包括如图2所示的棱镜阵列，或可具有一系列形状，包括脊、柱、棱锥、半球和圆锥；和/或可为具有平坦、尖状、截平或圆形部分的凸起或凹陷；以上任何一种结构都可具有与表面平面成角度或垂直的侧面。任何透镜状微结构都可使用，例如微结构化的表面可包括立体角元件，每个元件具有三个基本上互相垂直的、通常在单一基准点或顶点相交的光学面。微结构化的表面可以具有规则重复的图案、可以为无规的或它们的组合。通常，每个微结构均具有至少两个小于2mm的横向尺寸(即在膜平面内的尺寸)。微结构化层的厚度可为约10微米至约200微米。
可使用可聚合的组合物、具有微结构化负成型表面的母板和在其上具有底漆层的多层光学膜制备微结构化层。可将可聚合的组合物沉积在母板和底漆层之间，移动组合物珠粒使得该组合物填充母板的微结构。可聚合组合物发生聚合以形成层，然后脱离母板。母板可以是金属的，如镍、镀镍铜或黄铜，或者可以是在聚合条件下稳定且优选具有能让聚合而成的层干净利落地脱离母板的表面能的热塑性材料。母板在US 4,542,449、U.S.5,771,328和US 6,354,709中有进一步的描述。作为另外一种选择，可以制备预成形的微结构化层，并将其层合至涂底漆的多层光学膜上，使得底漆层设置在微结构化层和多层光学膜之间。
用于形成微结构化层的可聚合组合物可包括单体(包括单官能度、双官能度或更高官能度的单体)和/或低聚物，优选地是具有高折射率(例如大于约1.4或大于约1.5)的那些。可使用紫外线辐射使这些单体和/或低聚物聚合。合适的材料包括(甲基)丙烯酸酯，例如U.S.4,568,445、4,721,377、4,812,032、5,424,339和6,355,754中所述的那些。
可将光学制品用于图形艺术应用，例如用于背光标牌、告示板等。光学制品也可以用于至少具有一个或多个光源和显示面板的显示装置中。显示面板可以是任何能够产生图像、图形、文本等的类型，且可以是单色或多色的或者透射或反射的。实例包括液晶显示面板、等离子显示面板、或触摸屏。光源可包括荧光灯、磷光灯、发光二极管、或它们的组合。显示装置的例子包括电视、监测器、膝上型计算机和诸如手机、PDA、计算器之类的手持装置等。
由以下实例可更完全地理解本发明。
实例
材料
所有化学品均商购获得，并直接使用(除非另外指明)。表面活性剂TOMADOL 25-9得自Tomah Chemical Co.。交联剂CYMEL 301、CYMEL327、和催化剂CYCAT 4040得自Cytec Industries Inc.。聚乙烯亚胺交联剂EPOMIN SP012得自Aceto Corp.。多异氰酸酯交联剂STAHL XR5305和碳二亚胺交联剂STAHL XR5577得自Stahl International。氮丙啶交联剂CX-100得自DSM Neoresins。丙烯酸酯/三聚氰胺-甲醛分散体RHOPLEX3208得自Rohm and Haas Co.；该分散体包含约34-35重量％的丙烯酸粘合剂和约8-9重量％的甲醛-三聚氰胺交联剂。双酚A环氧二丙烯酸酯(CN120)购自Sartomer。除了CYMEL 301以20重量％的稀释度溶于异丙醇使用外，其他的交联剂均以20重量％的稀释度溶于水使用。CYTEC 4045以10重量％的稀释度溶于水使用。
磺基聚酯A(SPA)
按下述步骤制备磺基聚酯A：将111.9g(5.5摩尔％)的5-磺酸钠间苯二甲酸、592.1g(47.0摩尔％)的对苯二甲酸、598.4g(47.5摩尔％)的间苯二甲酸、705.8g的乙二醇、599g的新戊二醇、0.7g的氧化锑、和2.5g的醋酸钠加入一加仑聚酯反应釜中。向反应釜中通入氮气，使压力保持在345kPa(50psi)，在搅拌下将混合物加热到230℃，保持2小时，在此期间观察水的演变。将温度升至250℃，随后降低气压，施加真空(0.2托)，再将温度升至270℃。材料的粘度在45分钟内逐渐升高，之后，排出透明、粘稠的高分子量磺基聚酯。通过DSC测得磺基聚酯的Tg为70.3℃。磺酸酯的理论当量为每摩尔磺酸酯3847g聚合物。将500g聚合物在80℃下溶于2000g水和450g异丙醇的混合物中。然后将温度升至95℃，以除去异丙醇(以及一部分水)。最后得到的分散体包括12重量％固含量的磺基聚酯A水性分散体。
磺基聚酯B(SPB)
得自Eastman Chemical Co.的EASTEK 1100包括大约30重量％的磺基聚酯B水性分散体。
磺基聚酯C(SPC)
磺基聚酯C包括12重量％的磺基聚酯A与B的混合物(其中A与B的重量比为91∶9)的水性分散体。
实例1
实例1制备了由12重量％的磺基聚酯C、3.6重量％的CYMEL 301(相对于磺基聚酯固体为30重量％)、0.05重量％的CYCAT 4045(相对于CYMEL 301为1.5重量％)、和0.15重量％的TOMADOL 25-9组成的水溶液，其中括号外的所有重量比均是相对于水溶液的总量。混合顺序如下：水、表面活性剂、粘合剂、交联剂和催化剂。每加入一种物质后都充分混匀溶液。
使用#3缠线棒将溶液涂布到浇铸聚酯多层光学膜上。完成涂布后，将膜在80℃下干燥2分钟。按照US 2001/0013668(Neavin等人)中所述制备多层光学膜。然后，将涂布的多层光学膜在160℃下预热，随后，按6.5∶1的横向拉伸比、以50％/秒的恒定速率进行拉伸。
使用辐射固化性组合物在经涂布的多层光学膜的底漆层上形成微结构化层。该辐射固化性组合物由25重量％的苯氧基乙基丙烯酸酯、75重量％的双酚A环氧二：丙烯酸酯(CN120)、0.5重量％的LUCIRIN TPO和0.5重量％的DAROCUR 1173组成。使用下述工序涂布该组合物，并使其固化，以形成微结构化层：
1)将经涂覆的膜在140℃下加热1分钟。
2)将平坦的微结构化不锈钢印模在140℃的热板上加热。
3)将PL1200层合机(Professional Laminating Systems，Inc.)加热至140℃，并将运行速度设置为5.1mm/s(10英寸/分钟)。
4)将预热到140℃的辐射固化性组合物的珠线施加到印模上。
5)使用手压滚筒，将PET膜的经涂覆一侧轻轻压向该印模并滚动，以粘住就位。
6)将印模+膜样品夹在两张更大片的未涂底漆PET膜之间，以保护层合机滚筒。
7)使样品运行通过层合机。这产生出25微米(1密耳)的总树脂膜厚度。
8)使样品通过紫外处理器(紫外融合Lighthammer，配有300W的D灯泡，在氮气吹扫下，以100％的功率和15cm/s(30英尺/分钟)的线速度操作)。
9)将膜样品轻轻从印模上剥下来。
实例2至4和比较例1至8(C1至C8)
实例2至4和C1至C8的制备与实例1所述相同，区别在于使用表1中列出的材料。
测试方法
适用期：24小时后，对涂层溶液的不稳定指征进行评估。
拉伸后观察：对样品的缺陷和表面雾度进行评估。数字越小表示性能越好。
印模移除：从平坦的印模上剥离固化的微结构化表面，通过这种方式进行定性评估。与基底的良好粘附力使得能够在不在基底与印模之间残留粘附的固化树脂线丝的情况下从印模上拉开结构。在表1中，0表示存在一些线丝，1表示不存在线丝(印模上未残留任何固化树脂)。
粘附力按照ASTM D 3359测量，这是采用3M公司的3MTM 610玻璃纸带进行的交叉排线带拉拔试验。对粘附于基底上的残余树脂的量进行测定。
表1
Figure BPA00001232759100121
1.NC＝无肉眼可见的变化
2.相对于磺基聚酯固体为10重量％的CX100

Claims (8)

1.一种光学制品，包括：
多层光学膜，和
设置在所述多层光学膜上的底漆层，所述底漆层基本上由磺基聚酯和交联剂组成，
其中，所述交联剂包括三聚氰胺-甲醛树脂，
其中所述磺基聚酯与所述交联剂的比率为1∶1至20∶1。
2.根据权利要求1所述的光学制品，所述磺基聚酯包括水溶性磺基聚酯或水分散性磺基聚酯。
3.根据权利要求1所述的光学制品，所述磺基聚酯包含：
一种或多种二羧酸单体，所述二羧酸单体选自磺化间苯二甲酸、间苯二甲酸和对苯二甲酸；以及
一种或多种二醇单体，所述二醇单体选自乙二醇、二甘醇、新戊二醇和1，4-环己烷二甲醇。
4.根据权利要求1所述的光学制品，所述底漆层具有30nm至500nm的厚度。
5.根据权利要求1所述的光学制品，所述底漆层的Tg至少为50℃。
6.根据权利要求1所述的光学制品，所述多层光学膜具有第一光学层和第二光学层的交替层，所述第一光学层和所述第二光学层分别包含第一聚合物和第二聚合物，所述第一聚合物和所述第二聚合物选自聚对苯二甲酸乙二醇酯、聚萘二甲酸乙二醇酯、三乙酸纤维素、聚丙烯、聚酯、聚碳酸酯、聚甲基丙烯酸甲酯、聚酰亚胺、聚酰胺以及它们的共混物。
7.根据权利要求1所述的光学制品，还包括设置在所述底漆层上的微结构化层，其中所述微结构化层包括具有多个微结构的结构化表面，所述结构化表面包括所述光学制品的外表面。
8.根据权利要求7所述的光学制品，所述微结构化层不含卤素。
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EP2260340B1 (en) 2014-08-27
JP2011523379A (ja) 2011-08-11
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JP2014222364A (ja) 2014-11-27
JP5628789B2 (ja) 2014-11-19
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