CN102083895A - 光学用易粘接性聚酯膜 - Google Patents
光学用易粘接性聚酯膜 Download PDFInfo
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- CN102083895A CN102083895A CN2009801257369A CN200980125736A CN102083895A CN 102083895 A CN102083895 A CN 102083895A CN 2009801257369 A CN2009801257369 A CN 2009801257369A CN 200980125736 A CN200980125736 A CN 200980125736A CN 102083895 A CN102083895 A CN 102083895A
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- polyester film
- optics
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- layer
- film
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
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Abstract
提供与光学功能层在高温高湿下的密合性优良的光学用易粘接性聚酯膜。在聚酯膜的至少一个表面上具有涂布层的光学用易粘接性聚酯膜,其特征在于,所述涂布层以氨基甲酸酯树脂和具有唑啉基的树脂为主要成分,所述氨基甲酸酯树脂以聚碳酸酯多元醇为构成成分。
Description
技术领域
本发明涉及密合性和耐湿热性优良的光学用易粘接性聚酯膜。具体而言,涉及适合作为主要用于显示器等的硬涂膜、防反射膜、光扩散片、棱柱状透镜片、近红外线阻断膜、透明导电膜及防眩膜等光学功能性膜的基材的光学用易粘接性聚酯膜。
背景技术
通常,作为液晶显示器(LCD)的部件使用的光学功能性膜的基材,可以使用由聚对苯二甲酸乙二醇酯(PET)、丙烯酸、聚碳酸酯(PC)、三醋酸纤维素(TAC)、聚烯烃等形成的透明热塑性树脂膜。
在使用上述热塑性树脂膜作为各种光学功能性膜的基材时,层压满足各种用途的功能层。例如,在液晶显示器(LCD)中,可以列举:防止表面损伤的保护膜(硬涂层)、防止外光照入的防反射层(AR层)、聚光或光的扩散所使用的棱柱层、提高亮度的光扩散层等功能层。在上述基材中,特别是聚酯膜,由于透明性、尺寸稳定性、耐化学试剂性优良,且比较廉价,因此被广泛用作各种光学功能性膜的基材。
通常,在使用双轴取向聚酯膜或双轴取向聚酰胺膜这样的双轴取向热塑性膜时,由于膜表面高度的结晶取向,因此存在与各种涂料、粘接剂、油墨等的密合性差的缺点。因此,至今为止提出了通过各种方法赋予双轴取向聚酯膜表面易粘接性的方法。
例如,通常已知有在基材的聚酯膜的表面设置以聚酯、丙烯酸、聚氨酯、丙烯酸接枝聚酯等各种树脂作为主要构成成分的涂布层,由此赋予基材膜易粘接性的方法。在该涂布法中,工业上实施如下方法:对于结晶取向结束前的聚酯膜,将上述树脂的溶液或含有通过分散介质使树脂分散而得到的分散体的水性涂布液涂布在基材膜上,干燥后,至少沿单轴方向拉伸,接着实施热处理,使聚酯膜完成取向的方法(即生产线内涂布(inline coating)法);以及在制造聚酯膜后,在该膜上涂布水系或溶剂系的涂布液,之后进行干燥的方法(即脱生产线涂布(offline coating)法)。
LCD、PDP等显示器、以硬涂膜作为部件的携带用机器等,可在无论室内、室外的各种环境下使用。特别是对于携带用机器而言,有时要求能够耐受浴室、高温高湿地域等的耐湿热性。用于上述用途的光学功能性膜,需要在高温高湿下也不发生层间剥离的高密合性。因此,下述专利文献中公开了通过向涂布液中添加交联剂而在利用生产线内涂布法形成涂布层时使涂布层树脂中形成交联结构,从而赋予耐湿热性的易粘接性聚酯膜。
专利文献1:日本特开2000-141574号公报
专利文献2:日本专利第3900191号公报
专利文献3:日本特开2007-253512号公报
发明内容
为了降低地球环境负荷,期待使具有显示器的家电制品等达到目前以上的长寿命化。因此,需要作为部件使用的光学功能性膜即使在高温高湿下也能长时间地保持密合性。但是,上述专利文献中公开的易粘接性膜,虽然最初显示出良好的密合性,但在高温高湿下长期使用时,无法避免密合强度的降低。由于该密合性降低,因此存在初始性能无法长时间维持的问题。
本发明鉴于上述问题,提供几乎不发生被认为至今无法避免的在高温高湿下的密合性降低的光学用易粘接性聚酯膜。
另外,本发明所说的在高温高湿下的密合性是指:层压光固化型丙烯酸层后,在80℃、95%RH的环境下放置48小时,使用间隙间隔为2mm的刀具导轨,赋予光固化型丙烯酸层表面100个贯通光固化型丙烯酸层而到达基材膜的网格状的割痕,接着,将玻璃纸胶带贴附在网格状的割痕表面,通过橡皮进行擦蹭而使其完全地密合,再大力将同一部位剥下5次后的密合性。该密合性是比通常所使用的JIS K5600-5-6记载的评价方法更严格的判定标准的密合性,本发明的目的在于,上述在高温高湿下的密合性显示出与初期所显示出的密合性同等或同等以上的密合性。
上述问题能够通过以下的解决方法实现。
(1)一种光学用易粘接性聚酯膜,在聚酯膜的至少一个表面上具有涂布层,所述涂布层以氨基甲酸酯树脂和具有唑啉基的树脂为主要成分,所述氨基甲酸酯树脂以聚碳酸酯多元醇为构成成分。
(2)上述光学用易粘接性聚酯膜,其中,所述氨基甲酸酯树脂具有聚氧化烯基。
(4)一种光学用层压聚酯膜,其通过在所述光学用易粘接性聚酯膜的所述涂布层上层压选自硬涂层、光扩散层、棱柱状透镜层、电磁波吸收层、近红外线阻断层、透明导电层中的至少一层光学功能层而得到。
发明效果
本发明的光学用易粘接聚酯膜与光学功能层在高温高湿下的密合性(耐湿热性)优良。因此,作为优选的实施方式,上述高温、高湿处理下的密合性与最初的密合性相同或提高。作为本发明的优选的实施方式,使用本发明的光学用易粘接聚酯膜作为透镜片的基材时,在高温高湿下与透镜层的密合性良好。
具体实施方式
(聚酯膜)
构成本发明中作为基材使用的聚酯膜的聚酯树脂,可以使用聚对苯二甲酸乙二醇酯、聚对苯二甲酸丁二醇酯、聚2,6-萘二甲酸乙二醇酯、聚对苯二甲酸甲二醇酯、以及使作为共聚成分的、例如二乙二醇、新戊二醇、聚烷撑二醇等二醇成分、和己二酸、癸二酸、邻苯二甲酸、间苯二甲酸、2,6-萘二羧酸等二羧酸成分等共聚而得到的聚酯树脂等。
本发明中优选使用的聚酯树脂主要以聚对苯二甲酸乙二醇酯、聚对苯二甲酸丙二醇酯、聚对苯二甲酸丁二醇酯、聚萘二甲酸乙二醇酯中的至少1种为构成成分。这些聚酯树脂中,从物性和成本的平衡出发,最优选聚对苯二甲酸乙二醇酯。此外,这些聚酯膜通过双轴拉伸能够提高耐化学试剂性、耐热性、机械强度等。
此外,上述双轴拉伸聚酯膜可以是单层或多层。而且,只要在实现本发明效果的范围内,则对上述各层而言,可以根据需要,使聚酯树脂中含有各种添加剂。作为添加剂,可以列举例如:抗氧化剂、耐光剂、防凝胶剂、有机润湿剂、抗静电剂、紫外线吸收剂、表面活性剂等。
此外,为了改善膜的滑动性、卷曲性、抗粘连性等处理性、以及耐磨耗性、耐擦伤性等磨耗特性,有时使聚酯膜中含有惰性粒子。但是,由于本发明的膜作为光学用部件的基材膜使用,因此需要维持高度的透明性且处理性优良。具体而言,作为光学用部件的基材膜使用时,光学用易粘接性聚酯膜的总光线透过率优选为85%以上,更优选为87%以上,进一步优选为88%以上,更进一步优选为89%以上,特别优选为90%以上。
此外,为了得到高的清晰度,优选尽量减少基材膜中的惰性粒子的含量。因此,优选的实施方式为:形成仅使膜的表层中含有粒子的多层结构;或者使膜中实质上不含有粒子,而仅使涂布层中含有微粒。
特别是,从透明性方面出发,在使聚酯膜中实质上不含有惰性粒子的情况下,为了提高膜的处理性,优选使水系涂布液中含有无机和/或耐热性高分子粒子,从而在涂布层表面形成凹凸。
另外,“实质上不含有惰性粒子”是指:例如为无机粒子的情况,在通过X射线荧光分析对来自粒子的元素进行定量分析时,其含量为50ppm以下,优选为10ppm以下,最优选为检出限以下。这是因为,即使不向基材膜中积极地添加粒子,也存在来自外来异物的污染成分、原料树脂或附着在膜制造工序中的生产线或装置上的污染物剥离而混入膜中的情况。
(涂布层)
对于本发明的光学用易粘接性聚酯膜而言,重要的是设置含有氨基甲酸酯树脂和具有唑啉基的树脂作为主要成分的涂布层,其中,上述氨基甲酸酯树脂以聚碳酸酯多元醇作为构成成分。这里,“主要成分”是指含有涂布层所含的总固体成分中的50质量%以上。
如上述专利文献1~3那样,根据现有的技术常识中使涂布层的耐湿热性提高的观点考虑,优选在涂布层的形成中积极地导入交联结构。但是,在本发明中,通过将聚氨酯树脂和具有唑啉基的树脂组合,显示出在湿热条件下密合性提高的显著效果,从而完成了本发明。虽然由于这种结构而在高温高湿下的密合性提高的机制并不明确,但本发明人认为原因如下。
在本发明中,由于将聚氨酯树脂和具有唑啉基的树脂组合,因此在形成涂布层时,未反应的唑啉基残留。在之后的高温高湿环境下,构成基材的聚酯树脂水解,酯键断裂,产生羧酸基末端。这里,涂布层中残留的未反应的唑啉基与产生的羧酸末端反应,形成交联。即,认为是能够通过自我修复来防止由水解引起的密合性降低。而且,在本发明中,通过使用耐久性优良的聚碳酸酯类氨基甲酸酯树脂,能够发挥优良的耐湿热性。
本发明通过上述方式,能够提高与透镜层及其他光学功能层在高温高湿下的密合性(耐湿热性)。进而,以下对本发明的结构进行详述。
(氨基甲酸酯树脂)
本发明的氨基甲酸酯树脂至少含有多元醇成分、多异氰酸酯成分、进而根据需要含有增链剂来作为构成成分。本发明的氨基甲酸酯树脂是以上述构成成分为主、通过氨基甲酸酯键共聚而得到的高分子化合物。在本发明中,特征在于具有聚碳酸酯多元醇作为氨基甲酸酯树脂的构成成分。通过使本发明的涂布层中含有以聚碳酸酯多元醇为构成成分的氨基甲酸酯树脂,能够使耐湿热性提高。另外,这些氨基甲酸酯树脂的构成成分,可以通过核磁共振分析等进行鉴定。
作为本发明的氨基甲酸酯树脂的构成成分的聚碳酸酯多元醇,可以列举聚碳酸酯二醇、聚碳酸酯三醇等,可以优选使用聚碳酸酯二醇。作为本发明的氨基甲酸酯树脂的构成成分的聚碳酸酯二醇,可以列举通过使例如乙二醇、丙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇、3-甲基-1,5-戊二醇、1,6-己二醇、1,9-壬二醇、1,8-壬二醇、新戊二醇、二乙二醇、二丙二醇、1,4-环己二醇、1,4-环己二甲醇、双酚A等二醇类中的1种或2种以上、与例如碳酸二甲酯、碳酸二苯酯、碳酸亚乙酯、碳酰氯等碳酸酯类反应而得到的聚碳酸酯二醇等。作为聚碳酸酯二醇的数均分子量,优选为300~500,更优选为500~3000。
在本发明中,在将氨基甲酸酯树脂的总多异氰酸酯成分设为100摩尔%时,作为氨基甲酸酯树脂的构成成分的聚碳酸酯多元醇的组成摩尔比优选为3~100摩尔%,更优选为5~50摩尔%,进一步优选为6~20摩尔%。上述组成摩尔比低时,有时不能得到由聚碳酸酯多元醇带来的耐久性的效果。此外,上述组成摩尔比高时,初期密合性可能降低。
作为本发明的氨基甲酸酯树脂的构成成分的多异氰酸酯,可以列举例如:甲苯二异氰酸酯的异构体类;4,4-二苯基甲烷二异氰酸酯等芳香族二异氰酸酯类;苯二亚甲基二异氰酸酯等芳香族脂肪族二异氰酸酯类;异佛尔酮二异氰酸酯及4,4-二环己基甲烷二异氰酸酯、1,3-二(异氰酸根合甲基)环己烷等脂环式二异氰酸酯类;六亚甲基二异氰酸酯及2,2,4-三甲基六亚甲基二异氰酸酯等脂肪族二异氰酸酯类;或预先使单一或多种的上述化合物与三羟甲基丙烷等加成而得到的多异氰酸酯类。
作为增链剂,可以列举乙二醇、二乙二醇、1,4-丁二醇、新戊二醇及1,6-己二醇等二醇类;甘油、三羟甲基丙烷及季戊四醇等多元醇类;乙二胺、六亚甲基二胺及哌嗪等二胺类;单乙醇胺及二乙醇胺等氨基醇类;硫代二乙二醇等硫代二甘醇类;或水。
本发明的涂布层优选使用水系的涂布液,并通过后述的生产线内涂布法进行设置。因此,优选本发明的氨基甲酸酯树脂为水溶性的树脂。如果使用水溶性氨基甲酸酯树脂,则与具有唑啉基的树脂的相容性能够增加,透明性能够提高。另外,上述的“水溶性”是指在水、或含有低于50质量%的水溶性有机溶剂的水溶液中溶解。
为了赋予氨基甲酸酯树脂水溶性,可以向氨基甲酸酯分子骨架中导入(共聚)磺酸(盐)基或羧酸(盐)基。磺酸(盐)基为强酸性,存在因其吸湿性能而难以维持耐湿性的情况,因此优选导入弱酸性的羧酸(盐)基。
为了向氨基甲酸酯树脂中导入羧酸(盐)基,例如,将作为多元醇成分的二羟甲基丙酸、二羟甲基丁酸等具有羧酸基的多元醇化合物作为共聚成分导入,并通过盐形成剂进行中和。作为盐形成剂的具体例子,可以列举氨、三甲胺、三乙胺、三异丙胺、三正丙胺、三正丁胺等三烷基胺类;N-甲基吗啉、N-乙基吗啉等N-烷基吗啉类;N-二甲基乙醇胺、N-二乙基乙醇胺等N-二烷基烷醇胺类。这些化合物可以单独使用或并用2种以上。
为了赋予水溶性,在使用具有羧酸(盐)基的多元醇化合物作为共聚成分的情况下,将氨基甲酸酯树脂的总多异氰酸酯成分设为100摩尔%时,氨基甲酸酯树脂中的具有羧酸(盐)基的多元醇化合物的组成摩尔比优选为3~60摩尔%,更优选为10~40摩尔%。上述组成摩尔比小于3摩尔%时,存在水分散性变差的情况。此外,上述组成摩尔比超过60摩尔%时,由于涂布层形成时残留的唑啉基减少,因此耐湿热性可能降低。
但是,如上所述,在使用导入了羧酸的氨基甲酸酯树脂作为氨基甲酸酯树脂的情况下,其在涂布液中与唑啉基反应,存在涂布层形成时未反应的唑啉基降低的情况。因此,优选涂布层中实质上不具有羧酸(盐)基。因此,为了赋予氨基甲酸酯树脂水溶性而导入聚氧化烯基来代替羧酸盐基为本发明的优选实施方式。在使用导入了聚氧化烯基的氨基甲酸酯树脂作为氨基甲酸酯树脂时,涂布层中实质上不具有羧基。因此,未反应的唑啉基稳定地残留,能够发挥更优良的耐湿热性。
作为向氨基甲酸酯树脂中导入的聚氧化烯基(polyoxyalkylene group),可以列举聚氧乙烯基、聚氧丙烯基、聚四甲撑二醇链等,这些可以单独使用或者并用2种以上。其中,可以优选使用聚氧乙烯基。
为了向氨基甲酸酯树脂中导入聚氧乙烯基,例如可以通过如下方法实现:以二异氰酸酯的异氰酸酯基相对于单末端封端的聚氧乙烯二醇(polyoxyethylene glyco1)的羟基达到过量的比例,使多异氰酸酯与单末端封端的聚氧乙烯二醇(通过碳原子数为1~20的烷基进行单末端封端的烷氧基乙二醇(alkoxyethylene glycol))发生氨基甲酸酯化反应,之后,根据需要除去未反应的多异氰酸酯,由此得到含聚氧乙烯链的单异氰酸酯,接着,使所得的含聚氧乙烯链的单异氰酸酯与二异氰酸酯发生脲基甲酸酯化反应。
在为了赋予水溶性而向氨基甲酸酯树脂中导入聚氧乙烯基的情况下,将氨基甲酸酯树脂的总多异氰酸酯成分设为100摩尔%时,氨基甲酸酯树脂中的聚氧乙烯基的组成摩尔比优选为3摩尔%以上,更优选为10摩尔%以上,进一步优选为20摩尔%以上。上述组成摩尔比小于3摩尔%时,水分散性可能变差。
涂布层中优选含有10质量%以上且90质量%以下的上述氨基甲酸酯树脂。特别是,在如透镜层这样需要高密合性的情况下,更优选其含量为20质量%以上且80质量%以下。氨基甲酸酯树脂的含量多时,在高温高湿下的密合性降低,反之,含量少时,初期的密合性降低。
在本发明中,为了使密合性提高,也可以含有氨基甲酸酯树脂以外的树脂。可以列举例如丙烯酸树脂、聚酯树脂等。优选羧酸基含量少的树脂。更优选不含有羧酸基的树脂。羧酸基多时,其与唑啉基反应,导致在高温高湿下与由氨基甲酸酯树脂产生的羧酸基反应的唑啉基减少。
在本发明中,需要含有具有唑啉基的树脂。作为具有唑啉基的树脂,可以列举具有唑啉基的聚合物,例如,根据需要,通过现有公知的方法(例如溶液聚合、乳化聚合等),使具有唑啉基的聚合性不饱和单体与其他的聚合性不饱和单体共聚而得到的聚合物。
作为具有唑啉基的聚合性不饱和单体,可以列举例如:2-乙烯基-2-唑啉、2-乙烯基-4-甲基-2-唑啉、2-乙烯基-5-甲基-2-唑啉、2-异丙烯基-2-唑啉、2-异丙烯基-4-甲基-2-唑啉、2-异丙烯基-5-乙基-2-唑啉等。
作为上述其他的聚合性不饱和单体,可以列举例如:(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸-2-乙基己酯、(甲基)丙烯酸环己酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸异冰片酯等(甲基)丙烯酸的碳原子数为1~24个的烷基酯或环烷基酯;(甲基)丙烯酸-2-羟基乙酯、(甲基)丙烯酸羟基丙酯等(甲基)丙烯酸的碳原子数为2~8个的羟基烷基酯;苯乙烯、乙烯基甲苯等乙烯基芳香族化合物;(甲基)丙烯酰胺、二甲基氨基丙基(甲基)丙烯酰胺、(甲基)丙烯酸二甲基氨基乙酯、(甲基)丙烯酸缩水甘油酯与胺类的加成物;(甲基)丙烯酸聚乙二醇酯;N-乙烯基吡咯烷酮、乙烯、丁二烯、氯丁二烯、丙酸乙烯酯、醋酸乙烯酯、(甲基)丙烯腈等。这些物质可以单独或适当选择2种以上使用。
为了使具有唑啉基的树脂成为水溶性的,优选使其含有亲水性单体作为其他的聚合性不饱和单体。作为亲水性单体,可以列举:(甲基)丙烯酸-2-羟基乙酯、(甲基)丙烯酸甲氧基聚乙二醇酯、(甲基)丙烯酸与聚乙二醇的单酯化合物等具有聚乙二醇链的单体、(甲基)丙烯酸-2-氨基乙酯及其盐、(甲基)丙烯酰胺、N-羟甲基(甲基)丙烯酰胺、N-(2-羟基乙基)(甲基)丙烯酰胺、(甲基)丙烯腈、苯乙烯磺酸钠等。其中,优选含有在水中的溶解性高的(甲基)丙烯酸甲氧基聚乙二醇酯、(甲基)丙烯酸与聚乙二醇的单酯化合物等具有聚乙二醇链的单体。作为导入的聚乙二醇链的分子量,优选为200~900,更优选为300~700。
涂布层中优选含有5质量%以上且90质量%以下的上述具有唑啉基的树脂。特别是,在如透镜层这样需要高密合性的情况下,更优选其含量为10质量%以上且70质量%以下。具有唑啉基的树脂含量多时,与光学功能层的密合性降低,反之,含量少时,高温高湿下的密合性可能降低。
在本发明中,为了使涂膜强度提高,也可以使涂层中含有与具有唑啉基的树脂不同的交联剂、或具有交联基的树脂。作为交联剂,可以列举尿素类、环氧类、三聚氰胺类、异氰酸酯类、硅烷醇类等。此外,为了促进交联反应,可以根据需要适当使用催化剂等。
在本发明中,也可以使涂布层中含有粒子。粒子可以列举:(1)二氧化硅、高岭石、滑石、轻质碳酸钙、重质碳酸钙、沸石、氧化铝、硫酸钡、炭黑、氧化锌、硫酸锌、碳酸锌、二氧化钛、缎光白、硅酸铝、硅藻土、硅酸钙、氢氧化铝、多水高岭土、碳酸镁、氢氧化镁等无机粒子;(2)丙烯酸或甲基丙烯酸类、氯乙烯类、醋酸乙烯酯类、尼龙、苯乙烯/丙烯酸类、苯乙烯/丁二烯类、聚苯乙烯/丙烯酸类、聚苯乙烯/异戊二烯类、聚苯乙烯/异戊二烯类、甲基丙烯酸甲酯/甲基丙烯酸丁酯类、三聚氰胺类、聚碳酸酯类、尿素类、环氧类、氨基甲酸酯类、苯酚类、邻苯二甲酸二烯丙酯类、聚酯类等有机粒子。
上述粒子的平均粒径优选为1~500nm。平均粒径没有特殊限制,但从维持膜的透明性的观点出发,优选1~100nm。
上述粒子也可以含有2种以上平均粒径不同的粒子。
另外,上述平均粒径可以如下求得:使用透射电子显微镜(TEM)在12万倍的倍率下拍摄层压膜的截面,测定涂布层截面上存在的10个以上的粒子的最大粒径,并求出它们的平均值。
作为粒子的含量,优选为0.5质量%以上且20质量%以下。含量少时,不能得到充分的抗粘连性。此外,耐擦伤性变差。含量多时,不仅涂布层的透明性变差,而且涂膜强度降低。
为了提高涂布时的平整性、使涂布液脱泡,也可以使涂布层中含有表面活性剂。表面活性剂可以是阳离子型、阴离子型、非离子型等中的任意一种,但优选有机硅类、乙炔二醇类或含氟表面活性剂。在不损害与光学功能层的密合性的程度范围内,例如,优选使涂布液中含有0.005~0.5质量%的范围内的上述表面活性剂。
本发明的光学用易粘接性聚酯膜的雾度优选为2.5%以下,更优选为2.0%以下,进一步优选为1.5%以下。通过使上述记载的涂布层中含有的具有唑啉基的树脂为水溶性的,能够提高这种光学用易粘接性聚酯膜与其他的树脂的相容性。
为了赋予涂布层其他的功能性,还可以在不损害与光学功能层的密合性的程度范围内使其含有各种添加剂。作为上述添加剂,可以列举例如:荧光染料、荧光增白剂、增塑剂、紫外线吸收剂、颜料分散剂、抑泡剂、消泡剂、防腐剂、抗静电剂等。
在本发明中,作为在聚酯膜上设置涂布层的方法,可以列举在聚酯膜上涂布含有溶剂、粒子、树脂的涂布液并进行干燥的方法。作为溶剂,可以列举甲苯等有机溶剂、水或者水和水溶性有机溶剂的混合溶剂类,但从环境问题方面出发,优选水、或者在水中混合水溶性有机溶剂而得到的溶剂。
本发明的光学用层压聚酯膜如下得到:在上述聚酯膜的涂布层的至少一个表面上层压选自硬涂层、光扩散层、棱柱状透镜层、电磁波吸收层、近红外线阻断层、透明导电层中的至少一层光学功能层。
上述光学功能层中使用的材料没有特别限制。
(光学用易粘接性聚酯膜的制造)
关于本发明的光学用易粘接性聚酯膜的制造方法,以聚对苯二甲酸乙二醇酯(以下,简记为PET)膜为例进行说明,但本发明并不限于此。
将PET树脂充分真空干燥后,供给至挤出机,从T模将80℃的熔融PET树脂以片状熔融挤出至旋转冷却辊,再通过外加静电法使其冷却固化,从而得到未拉伸PET片。上述未拉伸PET片可以是单层结构,也可以是由共挤出法得到的多层结构。此外,优选使PET树脂中实质上不含有惰性粒子。
通过加热至80~120℃的辊,将所得的未拉伸PET片在长度方向上拉伸至2.5~5.0倍,得到单轴拉伸PET膜。然后,用夹子把持膜的端部,将其导入加热至70~140℃的热风区,在宽度方向上拉伸至2.5~5.0倍。接着,导入160~240℃的热处理区,进行1~60秒的热处理,使结晶取向完成。
在该膜制造工序的任意阶段,在PET膜的至少一个表面涂布涂布液,形成上述涂布层。即使在PET膜的两个表面形成涂布层也没有特殊的问题。涂布液中的树脂组合物的固体成分浓度优选为2~35重量%,特别优选为4~15重量%。
作为用于在PET膜上涂布该涂布液的方法,可以使用公知的任意的方法。可以列举例如:逆转辊涂布法、凹版涂布法、吻合涂布法、模压涂布法、转动刷涂布法、喷涂法、气刀涂布法、环棒涂布法(wire bar coating)、管刮刀涂布法(pipe doctor coating)、浸渍涂布法、帘涂法等。可以单独使用上述方法或将上述方法组合来进行涂布。
在本发明中,涂布层如下形成:在未拉伸或单轴拉伸后的PET膜上涂布涂布液并进行干燥,之后在至少单轴方向上拉伸,接着进行热处理。
在本发明中,最终所得的涂布层的厚度优选为20~350nm,干燥后的涂布量优选为0.02~0.5g/m2。如果涂布层的涂布量小于0.02g/m2,则对粘接性几乎没有效果。另一方面,如果涂布量大于0.5g/m2,则雾度增加。
通过本发明得到的光学用易粘接性热塑性树脂膜的涂布层,相对于硬涂层、光扩散层、棱柱状透镜层、电磁波吸收层、近红外线阻断层、透明导电层具有良好的粘接性。通过层压这些光学功能层,能够提供即使在湿热环境下仍能够长期保持初期功能的光学层压热塑性树脂膜。此外,即使在光学用途以外,也能够得到良好的粘接强度。具体而言,可以列举相片感光层、二偶氮感光层、砑光层、磁性层、喷墨油墨收容层、硬涂层、以及紫外线固化树脂、热固化树脂、印刷油墨或UV油墨、干式层压材料或挤出层压材料等粘接剂通过金属、无机物或它们的氧化物的真空蒸镀、电子束蒸镀、溅射、离子镀、CVD、等离子聚合等而得到的薄膜层、有机阻挡层等。
实施例
下面,使用实施例及比较例对本发明进行详细说明,但本发明并不受到以下的实施例的限制。此外,本发明中使用的评价方法如下。
(1)特性粘度
根据JIS K 7367-5,使用苯酚(60质量%)和1,1,2,2-四氯乙烷(40质量%)的混合溶剂作为溶剂,在30℃下进行测定。
(2)树脂组成
将树脂溶解在氘代氯仿中,使用ヴアリアン公司制造的核磁共振分析仪(NMR)ジエミニ-200进行1H-NMR分析,并根据其积分比,确定将总异氰酸酯成分设为100摩尔%时各组分的摩尔%比。
(3)光学用易粘接性聚酯膜的总光线透过率
按照JIS K 7105,使用浊度计(日本电色制,NDH2000)测定所得的光学用易粘接性聚酯膜的总光线透过率。
(4)光学用易粘接性聚酯膜的雾度
按照JIS K 7136,使用浊度计(日本电色制,NDH2000)测定所得的光学用易粘接性聚酯膜的雾度。
(5)粘接性
使用间隙间隔为2mm的刀具导轨,对所得的光学用层压聚酯膜的光固化型丙烯酸层表面,赋予100个贯通光固化型丙烯酸层而到达基材膜的网格状的割痕。接着,将玻璃纸胶带(ニチバン公司制,405号,宽24mm)贴附在网格状的割痕表面,通过橡皮进行擦蹭而使其完全地密合。然后,进行5次将玻璃纸胶带垂直地从光学用层压聚酯膜的光固化型丙烯酸层表面剥离的操作,之后,目视计数从光学用层压聚酯膜的光固化型丙烯酸层表面剥离的网格的数量,由下式求得光固化型丙烯酸层与基材膜的密合性。另外,将网格中部分剥离的网格视为被剥离的网格来进行计数,并按照下述标准划分等级。
密合性(%)=(1-被剥离的网格数/100)×100
◎:100%、或光固化型丙烯酸层的材料破裂
○:99~90%
△:89~70%
×:69~0%
(6)耐湿热性
在高温高湿槽中,于80℃、95%RH的环境下将所得的光学用层压聚酯膜放置48小时。接着,取出光学用层压聚酯膜,在室温常湿下放置12小时。然后,进行5次将玻璃纸胶带垂直地从光学用层压聚酯膜的光固化型丙烯酸层表面剥离的操作,除此之外,通过与上述(5)同样的方法求得光固化型丙烯酸层与基材膜的密合性,并按照下述标准划分等级。
◎:100%、或光固化型丙烯酸层的材料破裂
○:99~90%
△:89~70%
×:69~0%
(以聚碳酸酯多元醇作为构成成分的氨基甲酸酯树脂的聚合)
在具备搅拌机、蛇形冷凝管(Dimroth condenser)、氮气导入管、硅胶干燥管及温度计的四口烧瓶中加入1,3-二(异氰酸根合甲基)环己烷72.96质量份、二羟甲基丙酸12.60质量份、新戊二醇11.74质量份、数均分子量2000的聚碳酸酯二醇112.70质量份、以及作为溶剂的乙腈85.00质量份、N-甲基吡咯烷酮5.00质量份,在氮气气氛下,于75℃下搅拌3小时,确认反应液达到了预定的胺当量。接着,使该反应液降温至40℃后,添加三乙胺9.03质量份,得到聚氨酯预聚物D溶液。接着,向具有可高速搅拌的搅拌器(ホモデイスパ一)的反应容器中添加水450g,调节至25℃,以2000分钟-1进行搅拌混合,同时添加异氰酸酯基封端的预聚物并进行水分散。之后,在减压下,除去部分乙腈和水,由此制备固体成分为35%的水溶性聚氨酯树脂(A-1)。
通过同样的方法,得到其他组成的水溶性聚氨酯树脂(A-2)~(A-3)。对于这些水溶性聚氨酯树脂,将通过1H-NMR测定的组成(摩尔%比)及其他特性示于表1。
表1
(以聚碳酸酯多元醇作为构成成分、具有聚氧乙烯基的氨基甲酸酯树脂的聚合)
在具备温度计、氮气导入管及搅拌机的反应容器中,导入氮气的同时加入六亚甲基二异氰酸酯627.1质量份、加热至50℃的数均分子量为1000的甲氧基聚乙二醇372.9质量份,在80℃下反应6小时。在达到预定的异氰酸酯基含量后,通过史密斯式薄膜蒸馏器除去未反应的六亚甲基二异氰酸酯,得到含聚氧乙烯基的单异氰酸酯(A)。该含聚氧乙烯链的单异氰酸酯(A)的计算上的数均分子量为1168g/摩尔。
接着,在具备温度计、氮气导入管、搅拌机的反应容器中,于室温下导入氮气,同时加入二乙醇胺83.9质量份。在冷却的同时,添加含有聚氧乙烯链的单异氰酸酯A 916.1质量份,在60℃下反应3小时。通过红外光谱确认脲键的生成,得到含有聚氧乙烯基的多元醇(A)。
在具备回流冷凝管、氮气导入管、温度计、搅拌机的四口烧瓶中加入作为多异氰酸酯的1,3-二(异氰酸根合甲基)环己烷53.69质量份、作为疏水性大分子多元醇的数均分子量为2000的聚碳酸酯二醇88.6质量份、新戊二醇14.97质量份、上述含聚氧乙烯基的多元醇(A)52.87质量份、作为有机溶剂的乙腈60质量份、N-甲基吡咯烷酮30质量份,在氮气气氛下,将反应液温度调节至75~78℃,添加辛酸亚锡0.06质量份作为反应催化剂,反应7小时,直至反应率达到99%以上。接着,将反应液冷却至30℃,得到异氰酸酯基封端的预聚物。接着,向具有可高速搅拌的搅拌器的反应容器中添加水450g,调节至25℃,以2000分钟-1进行搅拌混合,同时添加异氰酸酯基封端的预聚物并进行水分散。之后,在减压下,除去部分乙腈和水,由此制备固体成分为35%的水溶性聚氨酯树脂(A-4)。
(以聚酯多元醇作为构成成分的氨基甲酸酯树脂的聚合)
在具备搅拌机、蛇形冷凝管、氮气导入管、硅胶干燥管及温度计的四口烧瓶中加入1,3-二(异氰酸根合甲基)环己烷72.96质量份、二羟甲基丙酸12.60质量份、新戊二醇11.74质量份、数均分子量为2000的聚酯多元醇112.70质量份、以及作为溶剂的乙腈85.00质量份、N-甲基吡咯烷酮5.00质量份,在氮气气氛下,于75℃下搅拌3小时,确认反应液达到了预定的胺当量。接着,使该反应液降温至40℃后,添加三乙胺9.03质量份,得到聚氨酯预聚物溶液。接着,向具有可高速搅拌的搅拌器的反应容器中添加水450g,调节至25℃,以2000分钟-1进行搅拌混合,同时添加异氰酸酯基封端的预聚物并进行水分散。之后,在减压下,除去部分乙腈和水,由此制备固体成分为35%的水溶性聚氨酯树脂(A-5)。
(以聚醚多元醇为构成成分的氨基甲酸酯树脂的聚合)
在具备搅拌机、蛇形冷凝管、氮气导入管、硅胶干燥管及温度计的四口烧瓶中加入1,3-二(异氰酸根合甲基)环己烷72.96质量份、二羟甲基丙酸12.60质量份、新戊二醇11.74质量份、数均分子量2000的聚醚二醇112.70质量份、以及作为溶剂的乙腈85.00质量份、N-甲基吡咯烷酮5.00质量份,在氮气气氛下,于75℃下搅拌3小时,确认反应液达到了预定的胺当量。接着,使该反应液降温至40℃后,添加三乙胺9.03质量份,得到聚氨酯预聚物溶液。接着,在具有可高速搅拌的搅拌器的反应容器中添加水450g,调节至25℃,以2000分钟-1进行搅拌混合,同时添加异氰酸酯基封端的预聚物并进行水分散。之后,在减压下,除去部分乙腈和水,由此制备固体成分为35%的水溶性聚氨酯树脂(A-6)。
在具有温度计、氮气导入管、回流冷凝器、滴液漏斗以及搅拌机的烧瓶中加入作为水性介质的离子交换水58质量份和异丙醇58质量份的混合物、以及聚合引发剂(2,2-偶氮二(2-脒基丙烷)二盐酸盐)4质量份。另一方面,在滴液漏斗中加入作为具有唑啉基的聚合性不饱和单体的2-异丙烯基-2-唑啉16质量份、甲氧基聚乙二醇丙烯酸酯(乙二醇的平均加成摩尔数为9摩尔;新中村化学株式会社制)32质量份、及甲基丙烯酸甲酯32质量份的混合物,在氮气气氛下,在70℃下滴液1小时。滴液结束后,搅拌反应溶液9小时,冷却,由此得到固体成分为40质量%的具有唑啉基的水溶性树脂(B)。
实施例1
(1)涂布液的调节
混合下述涂剂,制成涂布液。
水 51.00质量%
异丙醇 30.00质量%
聚氨酯树脂(A-1) 12.58质量%
粒子 1.57质量%
(平均粒径为40nm的硅溶胶,固体成分浓度40质量%)
粒子 0.08质量%
(平均粒径为450nm的硅溶胶,固体成分浓度40质量%)
表面活性剂 0.05质量%
(有机硅类,固体成分浓度100质量%)
(2)光学用易粘接性聚酯膜的制造
将作为膜原料聚合物的、特性粘度为0.62dl/g且实质上不含有粒子的PET树脂颗粒,在133Pa的减压下,于135℃下干燥6小时。之后,供给至挤出机,在约280℃下熔融挤出成片状,使其在表面温度保持在20℃的旋转冷却金属辊上急冷密合固化,得到未拉伸PET片。
通过被加热的轧辊组及红外线加热器将该未拉伸PET片加热至100℃,之后,通过具有圆周速度差的轧辊组在长度方向上拉伸3.5倍,得到单轴拉伸PET膜。
接着,通过辊涂法将上述涂布液涂布在PET膜的一个表面上,之后在80℃下干燥20秒。另外,进行调整以使最终(双轴拉伸后)的干燥后的涂布量为0.15g/m2。接着,通过拉幅机在120℃下在宽度方向上拉伸至4.0倍,并在固定了膜的宽度方向的长度的状态下,于230℃下加热0.5秒,然后在230℃下进行10秒钟3%的宽度方向的松弛处理,得到厚度为100μm的光学用易粘接性聚酯膜。将评价结果示于表2。
(3)光学用层压聚酯膜的制造
在保持清洁的厚度为1mm的SUS板上(SUS304)放置约5g的下述光固化型丙烯酸类涂布液,以膜试样的涂布层表面与光固化型丙烯酸类涂布液接触的方式进行重叠,从膜试样的上方通过宽10cm、直径4cm的手动式载荷胶辊进行压合,使光固化型丙烯酸类涂布液延展。接着,使用高压水银灯从膜表面侧照射800mJ/cm2的紫外线,使光固化型丙烯酸树脂固化。从SUS板上将厚度为20μm的具有光固化型丙烯酸层的膜试样剥离,得到光学用层压聚酯膜。
光固化型丙烯酸类涂布液
光固化型丙烯酸树脂 54.00质量%
(荒川化学工业制ビ一ムセツト505A-6)
光固化型丙烯酸树脂 36.00质量%
(荒川化学工业制ビ一ムセツト550)
光聚合引发剂 10.00质量%
(チバスペシヤリテイ一ケミカルズ公司制イルガキユア184)
比较例1
除了将聚氨酯树脂变更为以聚酯多元醇为构成成分的聚氨酯树脂(A-5)之外,与实施例1同样地操作,得到光学用易粘接性聚酯膜及光学用层压聚酯膜。
比较例2
除了将聚氨酯树脂变更为以聚醚多元醇为构成成分的聚氨酯树脂(A-6)之外,与实施例1同样地操作,得到光学用易粘接性聚酯膜及光学用层压聚酯膜。
实施例2
除了将聚氨酯树脂变更为以聚碳酸酯多元醇为构成成分的聚氨酯树脂(A-2)之外,与实施例1同样地操作,得到光学用易粘接性聚酯膜及光学用层压聚酯膜。
实施例3
除了将聚氨酯树脂变更为以聚碳酸酯多元醇为构成成分的聚氨酯树脂(A-3)之外,与实施例1同样地操作,得到光学用易粘接性聚酯膜及光学用层压聚酯膜。
实施例4
除了将聚氨酯树脂变更为以聚碳酸酯多元醇为构成成分、且侧链具有聚氧乙烯二醇链的氨基甲酸酯树脂(A-4)之外,与实施例1同样地操作,得到光学用易粘接性聚酯膜及光学用层压聚酯膜。
实施例5
除了对涂布液进行如下变更之外,与实施例1同样地操作,得到光学用易粘接性聚酯膜及光学用层压聚酯膜。
水 50.44质量%
异丙醇 30.00质量%
聚氨酯树脂(A-1) 17.07质量%
粒子 1.57质量%
(平均粒径为40nm的硅溶胶,固体成分浓度40质量%)
粒子 0.08质量%
(平均粒径为450nm的硅溶胶,固体成分浓度40质量%)
表面活性剂 0.05质量%
(有机硅类,固体成分浓度100质量%)
实施例6
除了对涂布液进行如下变更之外,与实施例1同样地操作,得到光学用易粘接性聚酯膜及光学用层压聚酯膜。
水 51.90质量%
异丙醇 30.00质量%
聚氨酯树脂(A-1) 5.39质量%
具有唑啉基的树脂(B) 1.01质量%
粒子 1.57质量%
(平均粒径为40nm的硅溶胶,固体成分浓度40质量%)
粒子 0.08质量%
(平均粒径为450nm的硅溶胶,固体成分浓度40质量%)
表面活性剂 0.05质量%
(有机硅类,固体成分浓度100质量%)
实施例7
除了对涂布液进行如下变更之外,与实施例1同样地操作,得到光学用易粘接性聚酯膜及光学用层压聚酯膜。
水 50.78质量%
异丙醇 30.00质量%
聚氨酯树脂(A-1) 14.38质量%
粒子 1.57质量%
(平均粒径为40nm的硅溶胶,固体成分浓度40质量%)
粒子 0.08质量%
(平均粒径为450nm的硅溶胶,固体成分浓度40质量%)
表面活性剂 0.05质量%
(有机硅类,固体成分浓度100质量%)
表2
产业上的利用可能性
本发明的光学用易粘接性聚酯膜与光学功能层的密合性及在高温高湿下的密合性(耐湿热性)优良,因此适合作为主要用于显示器等的硬涂膜及使用该膜的防反射膜、光扩散片、棱柱状透镜片、近红外线阻断膜、透明导电膜及防眩膜等光学功能性膜的基材膜。
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JP3125410B2 (ja) * | 1992-01-27 | 2001-01-15 | 旭化成工業株式会社 | コーティング剤組成物 |
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JP2005082671A (ja) * | 2003-09-08 | 2005-03-31 | Toppan Printing Co Ltd | 塗工フィルム及び反射用シート |
JP2008013606A (ja) * | 2006-07-03 | 2008-01-24 | Toyobo Co Ltd | ポリウレタン樹脂組成物およびこれを用いた積層体 |
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CN103619925A (zh) * | 2011-06-30 | 2014-03-05 | 三菱树脂株式会社 | 涂布膜 |
CN103619588A (zh) * | 2011-06-30 | 2014-03-05 | 三菱树脂株式会社 | 涂布膜 |
CN105037772A (zh) * | 2011-06-30 | 2015-11-11 | 三菱树脂株式会社 | 涂布膜 |
CN103619588B (zh) * | 2011-06-30 | 2016-03-09 | 三菱树脂株式会社 | 涂布膜 |
CN105037772B (zh) * | 2011-06-30 | 2018-01-02 | 三菱化学株式会社 | 涂布膜 |
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CN112724807A (zh) * | 2020-12-31 | 2021-04-30 | 宁波长阳科技股份有限公司 | 树脂组合物、光学涂布液、光学涂布层及光学聚酯保护膜 |
CN115139596A (zh) * | 2022-07-14 | 2022-10-04 | 道恩周氏(青岛)复合包装材料有限公司 | 一种高透明醋酸纤维素生物降解复合膜及其制备方法 |
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Also Published As
Publication number | Publication date |
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KR20110009736A (ko) | 2011-01-28 |
JP4457322B2 (ja) | 2010-04-28 |
WO2010001750A1 (ja) | 2010-01-07 |
KR101084403B1 (ko) | 2011-11-18 |
JP2010013550A (ja) | 2010-01-21 |
CN102083895B (zh) | 2013-01-16 |
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