CN106232695A - 聚脂薄膜及其制造方法 - Google Patents

聚脂薄膜及其制造方法 Download PDF

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Publication number
CN106232695A
CN106232695A CN201580021716.2A CN201580021716A CN106232695A CN 106232695 A CN106232695 A CN 106232695A CN 201580021716 A CN201580021716 A CN 201580021716A CN 106232695 A CN106232695 A CN 106232695A
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China
Prior art keywords
mylar
coating
particle
water
silane
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CN201580021716.2A
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CN106232695B (zh
Inventor
曹恩惠
朴载奉
白尚铉
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Kolon Industries Inc
Kolon Corp
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Kolon Corp
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Priority claimed from PCT/KR2015/004277 external-priority patent/WO2015167235A1/ko
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
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    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/12—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by mechanical means
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    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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    • B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
    • B05D7/04—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber to surfaces of films or sheets
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Abstract

本发明涉及一种转移聚酯薄膜。更具体地，本发明涉及一种转移聚酯薄膜及其制造方法，其中，所述转移聚酯薄膜包含具有优异剥离性的涂层，使得在涂布和固化硬涂层液体的步骤中，在形成硬涂层以赋予室内产品表面光泽时，涂层可以附着于所述硬涂层的表面，并且在所述硬涂层完全固化之后可以去除，从而使硬涂层的表面光滑。

Description

聚脂薄膜及其制造方法
技术领域
本发明涉及一种转移聚酯薄膜及其制造方法。更具体地，本发明涉及一种转移聚酯薄膜及其制造方法，其中，所述转移聚酯薄膜包含具有优异的剥离性的涂层，使得在形成硬涂层以赋予室内产品(interior product)表面光泽时，所述转移聚酯薄膜可以附着于所述硬涂层的表面，以使硬涂层的表面在涂布和固化硬涂层溶液的步骤中平滑地形成，并且所述转移聚酯薄膜在硬涂层完全固化之后可以易于除去。
背景技术
近来，在室内产品例如家具或地板等中，通过涂布UV固化树脂在印刷层上形成硬涂层，以使印刷层具有光泽。
硬涂层通过如下方法形成：施用UV固化树脂，在硬涂层上层压有转移薄膜的状态下通过UV固化工艺使该硬涂层完全固化，并除去转移薄膜，以使室内产品具有均匀的光滑表面。
在这种情况下，所使用的转移薄膜应当具有与硬涂层剥离的优异性能，并且易于层压和除去。
发明内容
技术问题
本发明的一个实施方案旨在提供一种用于转移薄膜的聚酯薄膜，在形成用于赋予室内产品表面光泽的硬涂层时，所述聚酯薄膜能够层压在硬涂层上，从而使硬涂层的表面平滑地形成，并且所述聚酯薄膜具有优异的剥离性，以便在硬涂层完全固化之后易于除去。
本发明的另一个实施方案旨在提供一种包含涂层的聚酯薄膜，所述涂层含有粒子，以便平滑地形成硬涂层表面并使所述涂层具有优异的剥离性，并且所述涂层中的粒子具有优异的分散性。
技术方案
在一个总的方面，聚酯薄膜包括：由聚酯树脂组成的基层；以及堆叠在所述基层的一个表面或两个表面上的涂层，
其中，所述涂层使用含有由下面化学式1表示的硅烷偶联剂和粒子的水性涂料组合物形成。
[化学式1]
在化学式1中，X是含有选自乙烯基、环氧基、氨基、甲基丙烯酸基、丙烯酸基和巯基中的一种或至少两种官能团的直链、支链或环状C1-C12烃基，并且R1至R3各自独立的是C1-C5烷基。
在另一个总的方面，聚酯薄膜的制造方法包括：
a)熔融挤出聚酯树脂以制造聚酯片材；
b)沿纵向拉伸该聚酯片材；
c)在所述沿纵向拉伸的聚酯薄膜的一个表面或两个表面上涂布含有由下面化学式1表示的硅烷偶联剂和粒子的水性涂料组合物，并在横向上拉伸所述经涂布的聚酯薄膜；以及
d)热定型经双轴向拉伸的聚酯薄膜。
[化学式1]
在化学式1中，X是含有选自乙烯基、环氧基、氨基、甲基丙烯酸基、丙烯酸基和巯基中的一种或至少两种官能团的直链、支链或环状C1-C12烃基，并且R1至R3各自独立的是C1-C5烷基。
有益效果
根据本发明的聚酯薄膜可以具有优异的转移性和剥离性，从而在用作转移薄膜时易于层压和除去，并形成均匀的光滑涂层。
具体实施方案
下文中，将提供示例性的实施方案以便更详细地描述本发明。然而，本发明不限于所述示例性的实施方案。
在使用聚合物粘合剂树脂和无机粒子形成具有剥离性的涂层的情况下，存在如下问题：即使固体含量较低，也不能完全地进行转移，并且粘合剂树脂对硬涂层具有较高的粘附性，从而会使剥离性劣化。因此，本发明人为了解决这些问题进行了研究，结果发现，通过使用硅烷偶联剂代替聚合物粘合剂树脂来粘合粒子并形成具有聚酯基层的有机-无机混合物，可以形成具有优异的剥离性的涂层，从而完成本发明。
另外，本发明人发现，在使用硅烷偶联剂以在线涂布法形成涂层的情况下，与聚酯基层的粘附性和表面光滑度优异，并且防止了粒子的聚集，使得所述涂层适合于制造所需的用于转移薄膜的聚酯薄膜，从而完成本发明。
另外，本发明人发现，在使用水性组合物制造薄膜以使所述组合物可以在线涂布时，可以通过调节组合物的pH以防止粒子的聚集，以及通过在将pH调节至防止粒子聚集的环境下添加粒子，来提供具有优异的剥离性的薄膜，从而完成本发明。
在本发明的一个方面中，可以使用任何硅烷偶联剂而没有限制，只要其可以进行水解和缩合反应，并且具有充当锚的能够与所用粒子(更具体地，无机粒子)连接的官能团即可。
更详细地，根据本发明的一个方面，聚酯薄膜包括由聚酯树脂组成的基层，以及堆叠在该基层的一个表面或两个表面上的涂层，
其中，所述涂层通过涂布和干燥含有由下面化学式1表示的硅烷偶联剂和粒子的水性涂料组合物而形成。
[化学式1]
在化学式1中，X是含有选自乙烯基、环氧基、氨基、甲基丙烯酸基、丙烯酸基和巯基中的一种或至少两种官能团的直链、支链或环状C1-C12烃基，并且R1至R3各自独立的是C1-C5烷基。
在本发明的一个方面中，所述涂层可以包含10至90wt％的所述粒子。
在本发明的一个方面中，所述粒子可以具有10至200nm的平均粒径，并且是选自二氧化硅、氧化铝、氧化锆和二氧化钛粒子中的任何一种或至少两种无机粒子。
在本发明的一个方面中，所述由化学式1表示的硅烷偶联剂可以是选自[3-(2-氨乙基氨基)丙基]三甲氧基硅烷、N-(2-氨乙基-3-氨丙基)三乙氧基硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、3-丙烯酰氧基丙基三甲氧基硅烷、3-丙烯酰氧基丙基三乙氧基硅烷、3-(甲基)丙烯酰氧基丙基三甲氧基硅烷、3-(甲基)丙烯酰氧基丙基三乙氧基硅烷、3-(甲基)丙烯酰氧基丙基三丙氧基硅烷、3-氨丙基三甲氧基硅烷和3-氨丙基三乙氧基硅烷中的任何一种或至少两种，但不必局限于此。
在本发明的一个方面中，所述水性涂料组合物可以包含用于进行水解或缩合反应的醇类溶剂或水。
在本发明的一个方面中，当粒子的pH为碱性时，水性涂料组合物可以包含用于将整个组合物的pH调节至8以上的pH调节剂，并且当粒子的pH为酸性时，水性涂料组合物可以包含用于将整个组合物的pH调节至5以下的pH调节剂。
在本发明的一个方面中，所述涂层可以通过在线涂布法涂布。
在本发明的一个方面中，所述涂层的干燥涂层厚度可以为10至500nm，但不限于此。
在本发明的一个方面中，所述聚酯薄膜的整体厚度可以为12至250μm，但不限于此。
另外，根据本发明的另一个方面，聚酯薄膜的制造方法包括：
a)熔融挤出聚酯树脂以制造聚酯片材；
b)沿纵向拉伸该聚酯片材；
c)在所述沿纵向拉伸的聚酯薄膜的一个表面或两个表面上涂布含有由下面化学式1表示的硅烷偶联剂和粒子的水性涂料组合物，并在横向上拉伸所述经涂布的聚酯薄膜；以及
d)热定型经双轴向拉伸的聚酯薄膜。
[化学式1]
在化学式1中，X是含有选自乙烯基、环氧基、氨基、甲基丙烯酸基、丙烯酸基和巯基中的一种或至少两种官能团的直链、支链或环状C1-C12烃基，并且R1至R3各自独立的是C1-C5烷基。
下文中，将详细描述本发明的一个方面。
本发明的特征在于，通过在线涂布法形成用于赋予聚酯薄膜的一个表面或两个表面转移性和剥离性的涂层。
在通过离线涂布法在聚酯薄膜上形成涂层的情况下，增加了处理过程，并且涂层厚度变厚，因而与在线涂布法相比会增加成本。因此，本发明人的一个目的是提供一种聚酯薄膜，通过使用在线涂布法涂布在拉伸工艺中经干燥和固化形成涂层的水性涂料组合物，该聚酯薄膜除了具有较薄的涂层厚度和涂层对聚酯薄膜较强的粘附力之外，还能够实现对水和溶剂的优异的耐性。
在本发明中，所述基层可以是由聚酯树脂制成的薄膜。更具体地，所述基层可以由聚对苯二甲酸乙二醇酯或聚萘二甲酸乙二醇酯制成。更优选地，当使用特性粘度为0.6至0.7的聚对苯二甲酸乙二醇酯时，其耐候性和耐水解性会更优异。此外，所述聚酯薄膜的厚度可以为12至250μm。在所述厚度在上述范围内的情况下，可以实现优异的产率和各种堆叠结构。更优选地，在使用具有轻微的粗糙度，更具体地，10nm以下的表面粗糙度的超透明聚酯薄膜的情况下，粗糙度不会转移到涂层。
另外，可以通过在聚酯薄膜的与其上形成有涂层的基层对应的表面的相对表面上进行电晕处理或使用不同的粘合剂组合物来赋予粘合性。
在本发明中，通过涂布和干燥含有由下面化学式1表示的硅烷偶联剂和粒子的水性涂料组合物而形成的涂层，可以通过在线涂布法形成。
[化学式1]
在化学式1中，X是含有选自乙烯基、环氧基、氨基、甲基丙烯酸基、丙烯酸基和巯基中的一种或至少两种官能团的直链、支链或环状C1-C12烃基，并且R1至R3各自独立的是C1-C5烷基。
在本发明的一个方面中，所述粒子可以是无机粒子。具体地，所述粒子可以是选自二氧化硅、氧化铝、氧化锆和二氧化钛粒子中的任何一种或至少两种，但不必局限于此。所述粒子的平均粒径没有特别地限制，但是可以在10至200nm，更优选地50至200nm的范围内，其优选在于，可以形成适合用作转移薄膜的涂层，并且该涂层可以通过在线涂布法形成。
所述粒子在涂层中的含量可以为10至90wt％，更优选地20至50wt％，其它成分可以由硅烷偶联剂和添加剂构成。在粒子的含量小于10wt％的情况下，表面粗糙度非常低，由此可能发生卷绕缺陷和粘连(blocking)问题，并且在所述含量大于90wt％的情况下，雾度会快速增加，或者会产生粒子的聚集。
在化学式1中，X是与各种合成树脂等有机材料化学键合的官能团，并且由OR1至OR3表示的烷氧基部分是与无机材料(例如玻璃或金属等)化学键合的官能团。
将描述由化学式1表示的硅烷偶联剂的反应机理。硅烷偶联剂的烷氧基甲硅烷基(Si-OR)被水或水分水解，由此转化为硅烷醇基(Si-OH)，该硅烷醇基通过缩合反应与无机材料的表面形成Si-O-M键(M指有机材料)。另一个官能团X与有机材料键合或相容，从而使无机材料和有机材料彼此化学结合。
也就是说，水性涂料组合物可以包含用于进行水解或缩合反应的醇类溶剂或水，并且优选地，使用水的情况有利于应用于在线涂布工艺。在使用醇类溶剂的情况下，可以使用具有良好挥发性的快速干燥溶剂，例如异丙醇或正丙醇等。
所述烷基包括直链和支链烷基，更具体地，在化学式1中，R1至R3可以各自独立地是乙基或甲基。
更具体地，所述由化学式1表示的硅烷偶联剂可以是选自[3-(2-氨乙基氨基)丙基]三甲氧基硅烷、N-(2-氨乙基-3-氨丙基)三乙氧基硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、3-丙烯酰氧基丙基三甲氧基硅烷、3-丙烯酰氧基丙基三乙氧基硅烷、3-(甲基)丙烯酰氧基丙基三甲氧基硅烷、3-(甲基)丙烯酰氧基丙基三乙氧基硅烷、3-(甲基)丙烯酰氧基丙基三丙氧基硅烷、3-氨丙基三甲氧基硅烷和3-氨丙基三乙氧基硅烷中的任何一种或至少两种，但不必局限于此。
根据本发明，可以使用硅烷偶联剂将无机粒子附着于由聚酯树脂制成的基层上，并由将要粘附根据本发明的聚酯薄膜的粘附表面实现优异的剥离性。也就是说，在使用粘合剂树脂将无机粒子涂布在基层上的情况下，粘合剂树脂与待粘附所述薄膜的粘附表面(更具体地，硬涂层)之间的粘合性较强，因而会使剥离性劣化，但是在根据本发明的聚酯薄膜中，可以通过使用硅烷偶联剂进一步提高剥离性。
另外，使用包含硅烷偶联剂、无机粒子和水的水性涂料组合物通过在线涂布法形成涂层，以使对聚酯基层的粘附性优异，并且可以形成非常薄的涂层。
在这种情况下，通过调节水性涂料组合物的pH可以进一步提高硅烷偶联剂和无机粒子之间的分散性，以使无机粒子可以均匀地分散在涂层中。分散性得到提高，这对于进一步提高剥离性是有利的。因此，在根据本发明的聚酯薄膜中，使用含有由化学式1表示的硅烷偶联剂和粒子的水性涂料组合物形成层叠在由聚酯树脂制成的基层的一个表面或两个表面上的涂层，但是粒子与水性涂料组合物之间的pH差可以小于3，更优选地，小于2。
通常，所述粒子以包含该粒子的分散液的形式购买，但是作为本发明人的研究结果，发现通过在制备水性涂料组合物时加入pH调节剂，可以进一步提高粒子分散液的分散性。还发现，当在制备水性涂料组合物时将组合物的pH调节至与粒子分散液的pH一致后稳定地形成酸性或碱性环境时注入粒子，在该情况下，所述粒子的分散性会进一步提高。在这种情况下，通过与其它成分的组合可以实现优异的剥离性和转移性，并且表面可以变得均匀和光滑。
具体地，优选地，当粒子的pH为碱性时，水性涂料组合物含有用于将整个组合物的pH调节至8以上的pH调节剂，并且当粒子的pH为酸性时，水性涂料组合物含有用于将整个组合物的pH调节至5以下的pH调节剂。由于由化学式1表示的硅烷偶联剂的pH是强碱性的，因此只有在组合物的制备过程中在刚要注入粒子之前将pH调节为酸性或碱性环境时，可以制得具有优异的粒子分散性的组合物，并且可以降低涂层的粗糙度。
更具体地，在水性涂料组合物中使用的粒子的pH为碱性的情况下，为了将pH调节至8以上，可以使用四烷基铵盐作为pH调节剂。例如，可以使用四甲基氢氧化铵或四乙基氢氧化铵等，但是pH调节剂不限于此。
另外，在粒子的pH为酸性的情况下，为了将整个组合物的pH调节至5以下，可以使用甲酸、硫酸、硝酸、盐酸、柠檬酸、马来酸、苹果酸、乳酸、草酸、邻苯二甲酸或琥珀酸等作为pH调节剂，但是pH调节剂不限于此。
另外，如有必要，所述水性涂料组合物还可以包含添加剂，例如润湿剂、光滑剂、UV稳定剂或分散剂等。
所述涂层可以通过在线涂布法涂布，从而具有10至500nm的干燥涂层厚度，但是不限于此。在干燥涂层厚度小于10nm的情况下，不会实现滑动性，并且在干燥涂层厚度大于500nm的情况下，薄膜之间可能产生粘连。
更具体地，水性涂料组合物可以包含0.1至0.5wt％的硅烷偶联剂、0.001至0.1wt％的粒子、0.1至2wt％的润湿剂和余量的水。此外，如有必要，还可以包含pH调节剂以制造与所述粒子相同的pH环境，使得所述粒子可以均匀地分散。
优选地，在整个水性涂料组合物中使用的硅烷偶联剂的含量为0.1至0.5wt％，并且在该含量小于0.1wt％的情况下，不能固定粒子，在该含量大于0.5wt％的情况下，涂层外观可能不是优异的。
优选地，在整个水性涂料组合物中使用的粒子的含量为0.001至0.1wt％，并且在该含量小于0.001wt％的情况下，滑动性会劣化并会发生粘连问题，在该含量大于0.1wt％的情况下，雾度会迅速增加。
润湿剂用于使乳液均匀地涂布在聚酯薄膜上，为了显著地提高涂布性，优选使用选自聚乙二醇、聚乙烯酯、改性硅和含氟混合物等中的一种。此外，考虑到优异的粘附性，优选地，在整个水性涂料组合物中使用的润湿剂的含量为0.1至2wt％。
用于提高粒子在水性涂料组合物中的分散性的pH调节剂，可以以形成与粒子相同的pH环境的含量使用。
另外，本发明提供了一种聚酯薄膜的制造方法，包括：
a)熔融挤出聚酯树脂以制造聚酯片材；
b)沿纵向拉伸该聚酯片材；
c)在所述沿纵向拉伸的聚酯薄膜的一个表面或两个表面上涂布含有由下面化学式1表示的硅烷偶联剂和粒子的水性涂料组合物，并在横向上拉伸所述经涂布的聚酯薄膜；以及
d)热定型经双轴向拉伸的聚酯薄膜。
[化学式1]
在化学式1中，X是含有选自乙烯基、环氧基、氨基、甲基丙烯酸基、丙烯酸基和巯基中的一种或至少两种官能团的直链、支链或环状C1-C12烃基，并且R1至R3各自独立的是C1-C5烷基。
另外，聚酯薄膜的制造方法还可以包括在步骤d)之后对与聚酯薄膜的形成有涂层的表面相对的表面上进行电晕处理。该电晕处理是为了进一步提高印刷性能，并且可以使用任何电晕处理方法，只要它是在本领域中通常使用的即可。
步骤a)是通过T型模头从料筒中熔融挤出树脂以制造片材，从而制造聚酯薄膜的过程。
步骤b)是沿双轴向拉伸所述聚酯片材以制造聚酯薄膜的过程，并且沿纵向的拉伸优选使用至少一个辊来进行。
接下来，在步骤c)中，通过在线涂布法形成涂层。在这种情况下，可以优选使用水分散乳液，以用于在线涂布。在这种情况下，用于形成涂层的水性涂料组合物的构成可以与上述相同，并且优选地，在涂布时，可以将水性涂料组合物以拉伸后的干燥涂层厚度为10至500nm来涂布。在通过涂布水性涂料组合物形成涂层之后，可以在横向上拉伸所述经涂布的薄膜。在这种情况下，优选使用拉幅机进行横向上的拉伸。在这种情况下，拉伸速率可以为3至4倍。
然后，除去涂层中使用的水，固化该涂层，并进行干燥和热定形处理以防止薄膜收缩。此时，热定形温度可以为225至235℃。
下文中，将提供实施例以便更详细地描述本发明。然而，本发明不限于下面的实施例。
本发明中的物理性能如下测量。
1)雾度
测量装置：Nippon Denshoku Kogyo Co.LTD.，NDH-5000，ASTM模式(ASTM D-1003)。
测量方法：对涂层样品的雾度测量三次，然后计算平均值。
2)原液稳定性
通过如下方法评价原液稳定性：当原液在室内温度和湿度下保持12小时以上时，测试原液是否变化或是否产生粒子的聚集。
o：在保持原液前、后，涂层外观和粒子的分散性相似。
x：在保持原液前、后，涂层外观和粒子的分散性有变化。
3)粒子的分散性
通过使用扫描电子显微镜(SEM)测量聚集粒子的数量(N数(N＝5))来评价涂层中粒子的分散性。在用肉眼以10,000倍的放大倍率确认聚集粒子时，将粒径为300nm的聚集粒子的数量为5以上的情况评价为产生了聚集粒子，并且将聚集粒子的数量小于5的情况评价为未产生聚集粒子。此处，在粒径为300nm的聚集粒子的数量为5以上的情况下，分散性不好。在这种情况下，剥离性会劣化。
4)剥离性
将丙烯酸硬涂层组合物涂布到聚氯乙烯薄膜上之后，在该聚氯乙烯薄膜上层叠和压制有实施例和比较例中制备的薄膜的状态下，通过固化所述硬涂层组合物来形成硬涂层。然后，除去实施例和比较例中制备的薄膜，从而如下评价剥离性。
o：所述薄膜干净地剥离而不与硬涂层组合物反应。
x：所述薄膜与硬涂层组合物反应，从而不是层压而是粘附于其上。
5)涂层性能
在荧光灯下用肉眼评价涂层外观水平。
o：没有针孔并且涂层表面干净。
x：有针孔并且涂层表面完全不透明。
6)油墨粘附性
使用油性笔在涂层表面上写字之后，将3M胶带贴在其上，并使用橡胶辊(2kg)在其上进行两次摩擦。然后，1分钟后，除去3M胶带，并评价油墨粘附性。
在这种情况下，将油墨转移到3M胶带的情况评价为良好，将油墨未转移的情况评价为差。
实施例1
水性涂料组合物1的制备
通过将0.23wt％的硅烷偶联剂(Dow Corning Korea Ltd.，Z-6020，固体含量：1wt％)、1wt％的润湿剂(3M Ltd.，FC-4432，固体含量：10wt％)、0.05wt％的作为pH调节剂的四乙基氢氧化铵和98.62wt％的水互相混合并将pH调节至10来稳定地形成碱性环境，在这种状态下加入并均匀地分散0.1wt％的二氧化硅粒子(Nalco，Nalco-2329，固体含量：40wt％，粒径：80nm，pH：8.2至8.6)。
聚酯薄膜的制备
将去除水分使含量为100ppm以下的聚对苯二甲酸乙二醇酯片注入熔融挤出机中熔融后，在通过T型模头将所得物挤出的同时用表面温度为20℃的流延鼓使其快速地冷却和固化，从而制备厚度为2,000μm的聚对苯二甲酸乙二醇酯片材。
将制得的聚对苯二甲酸乙二醇酯片材在110℃下沿纵向(MD)拉伸3.5倍，并在室温下冷却。接下来，通过棒涂布法将水性涂料组合物1涂布在所述片材的一个表面上之后，将该拉伸片材预热，干燥，然后在140℃下沿横向(TD)拉伸3.5倍。然后，在235℃下在5阶拉幅机中进行热处理后，将热处理过的薄膜沿纵向和横向松弛10％以在200℃下热定形，由此制备双轴向拉伸的薄膜，该薄膜的厚度为100μm并包含在其一个表面上形成的涂层。所述涂层在拉伸后的干燥涂层厚度为75nm。如上获得的薄膜的物理性能示于下表1中。
实施例2
水性涂料组合物2的制备
通过将0.23wt％的硅烷偶联剂(Dow Corning Korea Ltd.，Z-6020，固体含量：1wt％)、1wt％的润湿剂(3M Ltd.，FC-4432，固体含量：10wt％)、0.05wt％的作为pH调节剂的四乙基氢氧化铵和98.62wt％的水互相混合并将pH调节至10来稳定地形成碱性环境，在这种状态下加入并均匀地分散0.1wt％的二氧化硅粒子(AcenanoChem，AS-80K，固体含量：20wt％，粒径：80nm，pH：10至11.5)。
聚酯薄膜的制备
将去除水分使含量为100ppm以下的聚对苯二甲酸乙二醇酯片注入熔融挤出机中熔融后，在通过T型模头将所得物挤出的同时用表面温度为20℃的流延鼓使其快速地冷却和固化，从而制备厚度为2,000μm的聚对苯二甲酸乙二醇酯片材。
将制得的聚对苯二甲酸乙二醇酯片材在110℃下沿纵向(MD)拉伸3.5倍，并在室温下冷却。接下来，通过棒涂布法将水性涂料组合物2涂布在所述片材的一个表面上之后，将该拉伸片材预热，干燥，然后在140℃下沿横向(TD)拉伸3.5倍。然后，在235℃上在5阶拉幅机中进行热处理后，将热处理过的薄膜沿纵向和横向松弛10％以在200℃下热定形，由此制备双轴向拉伸的薄膜，该薄膜的厚度为100μm并包含在其一个表面上形成的涂层。所述涂层在拉伸后的干燥涂层厚度为75nm。如上获得的薄膜的物理性能示于下表1中。
实施例3
水性涂料组合物3的制备
通过将0.23wt％的硅烷偶联剂(Dow Corning Korea Ltd.，Z-6020，固体含量：1wt％)、1wt％的润湿剂(3M Ltd.，FC-4432，固体含量：10wt％)、0.05wt％的作为pH调节剂的四乙基氢氧化铵和98.62wt％的水互相混合并将pH调节至10来稳定地形成碱性环境，在这种状态下加入并均匀地分散0.1wt％的二氧化硅粒子(Nissan,ST-YL，固体含量：38.2wt％，粒径：50至80nm，pH：9.6)。
聚酯薄膜的制备
将去除水分使含量为100ppm以下的聚对苯二甲酸乙二醇酯片注入熔融挤出机中熔融后，在通过T型模头将所得物挤出的同时用表面温度为20℃的流延鼓使其快速地冷却和固化，从而制备厚度为2,000μm的聚对苯二甲酸乙二醇酯片材。
将制得的聚对苯二甲酸乙二醇酯片材在110℃下沿纵向(MD)拉伸3.5倍，并在室温下冷却。接下来，通过棒涂布法将水性涂料组合物3涂布在所述片材的一个表面上之后，将该拉伸片材预热，干燥，然后在140℃下沿横向(TD)拉伸3.5倍。然后，在235℃下在5阶拉幅机中进行热处理后，将热处理过的薄膜沿纵向和横向松弛10％以在200℃下热定形，由此制备双轴向拉伸的薄膜，该薄膜的厚度为100μm并包含在其一个表面上形成的涂层。所述涂层在拉伸后的干燥涂层厚度为75nm。如上获得的薄膜的物理性能示于下表1中。
实施例4
水性涂料组合物4的制备
通过将0.23wt％的硅烷偶联剂(Dow Corning Korea Ltd.，Z-6020，固体含量：1wt％)、1wt％的润湿剂(3M Ltd.，FC-4432，固体含量：10wt％)、0.05wt％的作为pH调节剂的四乙基氢氧化铵和98.62wt％的水互相混合并将pH调节至10来稳定地形成碱性环境，在这种状态下加入并均匀地分散0.1wt％的二氧化硅粒子(Nissan,ST-ZL，固体含量：38.7wt％，粒径：70至100nm，pH：9.3)。
聚酯薄膜的制备
将去除水分使含量为100ppm以下的聚对苯二甲酸乙二醇酯片注入熔融挤出机中熔融后，在通过T型模头将所得物挤出的同时用表面温度为20℃的流延鼓使其快速地冷却和固化，从而制备厚度为2,000μm的聚对苯二甲酸乙二醇酯片材。
将制得的聚对苯二甲酸乙二醇酯片材在110℃下沿纵向(MD)拉伸3.5倍，并在室温下冷却。接下来，通过棒涂布法将水性涂料组合物4涂布在所述片材的一个表面上之后，将该拉伸片材预热，干燥，然后在140℃下沿横向(TD)拉伸3.5倍。然后，在235℃下在5阶拉幅机中进行热处理后，将热处理过的薄膜沿纵向和横向松弛10％以在200℃下热定形，由此制备双轴向拉伸的薄膜，该薄膜的厚度为100μm并包含在其一个表面上形成的涂层。所述涂层在拉伸后的干燥涂层厚度为75nm。如上获得的薄膜的物理性能示于下表1中。
实施例5
水性涂料组合物5的制备
通过将0.23wt％的硅烷偶联剂(Dow Corning Korea Ltd.，Z-6020，固体含量：1wt％)、1wt％的润湿剂(3M Ltd.，FC-4432，固体含量：10wt％)、0.05wt％的作为pH调节剂的甲酸和98.62wt％的水互相混合并将pH调节至4来稳定地形成酸性环境，在这种状态下加入并均匀地分散0.1wt％的二氧化硅粒子(Nissan,ST-AK-YL，固体含量：30至31wt％，粒径：50至80nm，pH：3至5)。
聚酯薄膜的制备
将去除水分使含量为100ppm以下的聚对苯二甲酸乙二醇酯片注入熔融挤出机中熔融后，在通过T型模头将所得物挤出的同时用表面温度为20℃的流延鼓使其快速地冷却和固化，从而制备厚度为2,000μm的聚对苯二甲酸乙二醇酯片材。
将制得的聚对苯二甲酸乙二醇酯片材在110℃下沿纵向(MD)拉伸3.5倍，并在室温下冷却。接下来，通过棒涂布法将水性涂料组合物5涂布在所述片材的一个表面上之后，将该拉伸片材预热，干燥，然后在140℃下沿横向(TD)拉伸3.5倍。然后，在235℃下在5阶拉幅机中进行热处理后，将热处理过的薄膜沿纵向和横向松弛10％以在200℃下热定形，由此制备双轴向拉伸的薄膜，该薄膜的厚度为100μm并包含在其一个表面上形成的涂层。所述涂层在拉伸后的干燥涂层厚度为75nm。如上获得的薄膜的物理性能示于下表1中。
比较例1
水性涂料组合物6的制备
通过将0.23wt％的硅烷偶联剂(Dow Corning Korea Ltd.，Z-6020，固体含量：1wt％)、1wt％的润湿剂(3M Ltd.，FC-4432，固体含量：10wt％)、0.05wt％的作为pH调节剂的四乙基氢氧化铵和98.62wt％的水互相混合并将pH调节至10来稳定地形成碱性环境，在这种状态下加入并均匀地分散0.1wt％的二氧化硅粒子(Nissan,ST-AK-YL，固体含量：30至31wt％，粒径：50至80nm，pH：3至5)。
聚酯薄膜的制备
将去除水分使含量为100ppm以下的聚对苯二甲酸乙二醇酯片注入熔融挤出机中熔融后，在通过T型模头将所得物挤出的同时用表面温度为20℃的流延鼓使其快速地冷却和固化，从而制备厚度为2,000μm的聚对苯二甲酸乙二醇酯片材。
将制得的聚对苯二甲酸乙二醇酯片材在110℃下沿纵向(MD)拉伸3.5倍，并在室温下冷却。接下来，通过棒涂布法将水性涂料组合物6涂布在所述片材的一个表面上之后，将该拉伸片材预热，干燥，然后在140℃下沿横向(TD)拉伸3.5倍。然后，在235℃下在5阶拉幅机中进行热处理后，将热处理过的薄膜沿纵向和横向松弛10％以在200℃下热定形，由此制备双轴向拉伸的薄膜，该薄膜的厚度为100μm并包含在其一个表面上形成的涂层。所述涂层在拉伸后的干燥涂层厚度为75nm。如上获得的薄膜的物理性能示于下表1中。
比较例2
水性涂料组合物7的制备
将0.23wt％的硅烷偶联剂(Dow Corning Korea Ltd.，Z-6020，固体含量：1wt％)、1wt％的润湿剂(3M Ltd.，FC-4432，固体含量：10wt％)和98.67wt％的水互相混合之后，当pH为8时，加入并均匀地分散0.1wt％的二氧化硅粒子(Nissan,ST-AK-YL，固体含量：30至31wt％，粒径：50至80nm，pH：3至5)。
聚酯薄膜的制备
将去除水分使含量为100ppm以下的聚对苯二甲酸乙二醇酯片注入熔融挤出机中熔融后，在通过T型模头将所得物挤出的同时用表面温度为20℃的流延鼓使其快速地冷却和固化，从而制备厚度为2,000μm的聚对苯二甲酸乙二醇酯片材。
将制得的聚对苯二甲酸乙二醇酯片材在110℃下沿纵向(MD)拉伸3.5倍，并在室温下冷却。接下来，通过棒涂布法将水性涂料组合物7涂布在所述片材的一个表面上之后，将该拉伸片材预热，干燥，然后在140℃下沿横向(TD)拉伸3.5倍。然后，在235℃下在5阶拉幅机中进行热处理后，将热处理过的薄膜沿纵向和横向松弛10％以在200℃下热定形，由此制备双轴向拉伸的薄膜，该薄膜的厚度为100μm并包含在其一个表面上形成的涂层。所述涂层在拉伸后的干燥涂层厚度为75nm。如上获得的薄膜的物理性能示于下表1中。
比较例3
水性涂料组合物8的制备
通过将0.23wt％的硅烷偶联剂(Dow Corning Korea Ltd.，Z-6020，固体含量：1wt％)、1wt％的润湿剂(3M Ltd.，FC-4432，固体含量：10wt％)、0.05wt％的作为pH调节剂的甲酸和98.62wt％的水互相混合并将pH调节至4来稳定地形成酸性环境，在这种状态下加入并均匀地分散0.1wt％的二氧化硅粒子(Nalco,Nalco-2329，固体含量：40wt％，粒径：80nm，pH：8.2至8.6)。
聚酯薄膜的制备
将去除水分使含量为100ppm以下的聚对苯二甲酸乙二醇酯片注入熔融挤出机中熔融后，在通过T型模头将所得物挤出的同时用表面温度为20℃的流延鼓使其快速地冷却和固化，从而制备厚度为2,000μm的聚对苯二甲酸乙二醇酯片材。
将制得的聚对苯二甲酸乙二醇酯片材在110℃下沿纵向(MD)拉伸3.5倍，并在室温下冷却。接下来，通过棒涂布法将水性涂料组合物8涂布在所述片材的一个表面上之后，将该拉伸片材预热，干燥，然后在140℃下沿横向(TD)拉伸3.5倍。然后，在235℃下在5阶拉幅机中进行热处理后，将热处理过的薄膜沿纵向和横向松弛10％以在200℃下热定形，由此制备双轴向拉伸的薄膜，该薄膜的厚度为100μm并包含在其一个表面上形成的涂层。所述涂层在拉伸后的干燥涂层厚度为75nm。如上获得的薄膜的物理性能示于下表1中。
比较例4
水性涂料组合物9的制备
将4wt％的尿烷粘合剂(DKS，H-3，固体含量：1wt％)、1wt％的润湿剂(3M Ltd.，FC-4432，固体含量：10wt％)和94.9wt％的水互相混合之后，加入并均匀地分散0.1wt％的二氧化硅粒子(Nissan,ST-AK-YL，固体含量：30至31wt％，粒径：50至80nm，pH：3至5)。
聚酯薄膜的制备
将去除水分使含量为100ppm以下的聚对苯二甲酸乙二醇酯片注入熔融挤出机中熔融后，在通过T型模头将所得物挤出的同时用表面温度为20℃的流延鼓使其快速地冷却和固化，从而制备厚度为2,000μm的聚对苯二甲酸乙二醇酯片材。
将制得的聚对苯二甲酸乙二醇酯片材在110℃下沿纵向(MD)拉伸3.5倍，并在室温下冷却。接下来，通过棒涂布法将水性涂料组合物9涂布在所述片材的一个表面上之后，将该拉伸片材预热，干燥，然后在140℃下沿横向(TD)拉伸3.5倍。然后，在235℃下在5阶拉幅机中进行热处理后，将热处理过的薄膜沿纵向和横向松弛10％以在200℃下热定形，由此制备双轴向拉伸的薄膜，该薄膜的厚度为100μm并包含在其一个表面上形成的涂层。所述涂层在拉伸后的干燥涂层厚度为90nm。
如上获得的薄膜的物理性能示于下表1中。
比较例5
水性涂料组合物10的制备
将2.27wt％的丙烯酸粘合剂(Rohm&Haas,P-3208，固体含量：1wt％)、1wt％的润湿剂(3M Ltd.，FC-4432，固体含量：10wt％)和96.63wt％的水互相混合之后，加入并均匀地分散0.1wt％的二氧化硅粒子(Nissan,ST-AK-YL，固体含量：30至31wt％，粒径：50至80nm，pH：3至5)。
聚酯薄膜的制备
将去除水分使含量为100ppm以下的聚对苯二甲酸乙二醇酯片注入熔融挤出机中熔融后，在通过T型模头将所得物挤出的同时用表面温度为20℃的流延鼓使其快速地冷却和固化，从而制备厚度为2,000μm的聚对苯二甲酸乙二醇酯片材。
将制得的聚对苯二甲酸乙二醇酯片材在110℃下沿纵向(MD)拉伸3.5倍，并在室温下冷却。接下来，通过棒涂布法将水性涂料组合物10涂布在所述片材的一个表面上之后，将该拉伸片材预热，干燥，然后在140℃下沿横向(TD)拉伸3.5倍。然后，在235℃下在5阶拉幅机中进行热处理后，将热处理过的薄膜沿纵向和横向松弛10％以在200℃下热定形，由此制备双轴向拉伸的薄膜，该薄膜的厚度为100μm并包含在其一个表面上形成的涂层。所述涂层在拉伸后的干燥涂层厚度为90nm。如上获得的薄膜的物理性能示于下表1中。
[表1]
如表1所示，在比较例1至3中，水性涂料组合物的pH与粒子的pH不同，从而产生粒子的聚集。反之，在实施例1至5中证实，通过将水性涂料组合物的pH和粒子的pH调节为彼此相等则不产生粒子的聚集，并且剥离性也较优异。同时，在比较例4和5中证实，在使用尿烷粘合剂或丙烯酸粘合剂代替硅烷偶联剂的情况下，粒子的分散度良好，但是与使用硅烷偶联剂的情况相比，涂层厚度增加20％，使得雾度较高，剥离性降低，反而产生粘附力。
上文中，尽管通过示例性的实施方案描述了本发明，但是提供它们只是为了帮助对本发明的整体理解。因此，本发明不限于所述示例性的实施方案。本发明所属领域的技术人员根据本说明书可以进行各种修改和改变。
因此，本发明的精神不应局限于上述示例性的实施方案，并且所附权利要求以及等同或等效于所附权利要求的所有修改都旨在落入本发明的范围和精神内。

Claims (16)

1.一种聚酯薄膜，包括：
由聚酯树脂组成的基层；以及
堆叠在所述基层的一个表面或两个表面上的涂层，
其中，所述涂层通过涂布和干燥含有由下面化学式1表示的硅烷偶联剂和粒子的水性涂料组合物而形成，并且
所述水性涂料组合物与所述粒子之间的pH差小于3，
[化学式1]
在化学式1中，X是含有选自乙烯基、环氧基、氨基、甲基丙烯酸基、丙烯酸基和巯基中的一种或至少两种官能团的直链、支链或环状C1-C12烃基，并且R1至R3各自独立的是C1-C5烷基。
2.根据权利要求1所述的聚酯薄膜，其中，所述涂层包含10至90wt％的所述粒子。
3.根据权利要求1所述的聚酯薄膜，其中，所述粒子具有10至200nm的平均粒径，并且是选自二氧化硅、氧化铝、氧化锆和二氧化钛粒子中的任何一种或至少两种无机粒子。
4.根据权利要求1所述的聚酯薄膜，其中，所述由化学式1表示的硅烷偶联剂为选自[3-(2-氨乙基氨基)丙基]三甲氧基硅烷、N-(2-氨乙基-3-氨丙基)三乙氧基硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、3-丙烯酰氧基丙基三甲氧基硅烷、3-丙烯酰氧基丙基三乙氧基硅烷、3-(甲基)丙烯酰氧基丙基三甲氧基硅烷、3-(甲基)丙烯酰氧基丙基三乙氧基硅烷、3-(甲基)丙烯酰氧基丙基三丙氧基硅烷、3-氨丙基三甲氧基硅烷和3-氨丙基三乙氧基硅烷中的任何一种或至少两种。
5.根据权利要求1所述的聚酯薄膜，其中，所述水性涂料组合物还包含醇类溶剂或水。
6.根据权利要求1所述的聚酯薄膜，其中，当所述粒子的pH为碱性时，所述水性涂料组合物含有用于将整个组合物的pH调节至8以上的pH调节剂，并且当所述粒子的pH为酸性时，所述水性涂料组合物含有用于将整个组合物的pH调节至5以下的pH调节剂。
7.根据权利要求1所述的聚酯薄膜，其中，所述涂层通过在线涂布法形成。
8.根据权利要求1所述的聚酯薄膜，其中，所述涂层的干燥涂层厚度为10至500nm。
9.根据权利要求1所述的聚酯薄膜，其中，所述聚酯薄膜的整体厚度为12至250μm。
10.根据权利要求1所述的聚酯薄膜，其中，所述聚酯薄膜中粒径为300nm以上的聚集粒子的数量小于5。
11.一种聚酯薄膜的制造方法，该制造方法包括：
a)熔融挤出聚酯树脂以制造聚酯片材；
b)沿纵向拉伸所述聚酯片材；
c)在所述沿纵向拉伸的聚酯薄膜的一个表面或两个表面上涂布含有由下面化学式1表示的硅烷偶联剂和粒子的水性涂料组合物，并沿横向拉伸所述经涂布的聚酯薄膜；以及
d)热定型经双轴向拉伸的聚酯薄膜，
[化学式1]
在化学式1中，X是含有选自乙烯基、环氧基、氨基、甲基丙烯酸基、丙烯酸基和巯基中的一种或至少两种官能团的直链、支链或环状C1-C12烃基，并且R1至R3各自独立的是C1-C5烷基。
12.根据权利要求11所述的制造方法，其中，所述粒子具有10至200nm的平均粒径，并且是选自二氧化硅、氧化铝、氧化锆和二氧化钛粒子中的任何一种或至少两种无机粒子。
13.根据权利要求11所述的制造方法，其中，所述由化学式1表示的硅烷偶联剂为选自[3-(2-氨乙基氨基)丙基]三甲氧基硅烷、N-(2-氨乙基-3-氨丙基)三乙氧基硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、3-丙烯酰氧基丙基三甲氧基硅烷、3-丙烯酰氧基丙基三乙氧基硅烷、3-(甲基)丙烯酰氧基丙基三甲氧基硅烷、3-(甲基)丙烯酰氧基丙基三乙氧基硅烷、3-(甲基)丙烯酰氧基丙基三丙氧基硅烷、3-氨丙基三甲氧基硅烷和3-氨丙基三乙氧基硅烷中的任何一种或至少两种。
14.根据权利要求11所述的制造方法，其中，所述水性涂料组合物还包含醇类溶剂或水。
15.根据权利要求11所述的制造方法，其中，当所述粒子的pH为碱性时，所述水性涂料组合物含有用于将整个组合物的pH调节至8以上的pH调节剂，并且当所述粒子的pH为酸性时，所述水性涂料组合物含有用于将整个组合物的pH调节至5以下的pH调节剂，但是
所述水性涂料组合物与所述粒子之间的pH差小于3。
16.根据权利要求11所述的制造方法，其中，所述聚酯薄膜中粒径为300nm以上的聚集粒子的数量小于5。
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