CN113226740A - 玻璃接合用薄膜及其制备方法 - Google Patents

玻璃接合用薄膜及其制备方法 Download PDF

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Publication number
CN113226740A
CN113226740A CN201980078975.7A CN201980078975A CN113226740A CN 113226740 A CN113226740 A CN 113226740A CN 201980078975 A CN201980078975 A CN 201980078975A CN 113226740 A CN113226740 A CN 113226740A
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China
Prior art keywords
film
glass
bonding
metal salt
glass bonding
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Granted
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CN201980078975.7A
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CN113226740B (zh
Inventor
金惠珍
李学守
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Aisikai Mcwoo Co ltd
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SKC Co Ltd
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Abstract

本发明的玻璃接合用薄膜，包含聚乙烯醇缩醛树脂、增塑剂及金属盐，以上述薄膜整体为基准，每10ppm的上述金属盐的含量获得8.5kgf/cm2以上的接合力调节效果。本发明的玻璃接合用薄膜从玻璃接合用薄膜的表面向厚度方向具有金属盐的浓度梯度，因此可以提供于易调节接合力且水分敏感性得到改善的玻璃接合用薄膜。

Description

玻璃接合用薄膜及其制备方法
技术领域
本发明涉及一种玻璃接合用薄膜及其制备方法。
背景技术
通常，由一对玻璃面板和插入于这些面板之间的合成树脂薄膜构成的层合玻璃(钢化玻璃、安全玻璃)即使在破碎时其玻璃碎片也不会飞散，因此具有优异的安全性，从而广泛用于汽车等道路车辆的车窗玻璃和高层建筑的窗户玻璃。在适用于这种层合玻璃的薄膜中大多适用对无机类材料的亲和力高的聚乙烯醇缩醛树脂。
在一对玻璃面板之间夹有薄膜的层合玻璃具有层合玻璃所必需的基本特性，例如耐穿透性或玻璃碎片难以飞散等，但是其耐湿性可能较差，在这种情况下，在高湿度的气氛中，在层合玻璃的周缘中间膜直接接触空气，导致外边部出现白化现象。并且，出于防止这些白化现象等的目的，在薄膜和玻璃之间使用用于调整接合力的添加剂。
日本公开专利公报第1998-139496号(申请1996-290261号)公开了一种没有白化的薄膜,其作为含有聚乙烯醇缩丁醛、增塑剂、羧基金属盐和改性硅油的层合玻璃用中间膜。然而，由于上述薄膜使用极性低的改性硅油，因此与聚乙烯醇缩丁醛树脂的相容性降低，导致最终薄膜的雾度(Haze)增加，并且将与聚乙烯醇缩丁醛的羟基反应的玻璃的官能团受到改性硅油的干扰，因此接合力显著降低，耐穿透性和耐冲击性下降。
并且，当为了接合力调节效果而适用过量的添加剂时，反而导致耐湿性降低，从而在长期耐久性评价中黄度会增加。
发明内容
技术问题
本发明的目的在于提供具有改善的耐久性的玻璃接合用薄膜。
解决问题的方案
为了达到上述目的，本发明的一实施例的玻璃接合用薄膜，包含聚乙烯醇缩醛树脂、增塑剂及金属盐，上述玻璃接合用薄膜每10ppm的上述金属盐的含量获得8.5kgf/cm2以上的接合力调节效果。
上述金属盐的含量以上述薄膜整体为基准信息评价。
上述玻璃接合用薄膜可以具有不均匀的浓度梯度，即上述玻璃接合用薄膜的表面与上述玻璃接合用薄膜的中心部相比以更高的浓度包含上述金属盐或金属离子。
上述金属离子可以衍生自上述金属盐。
上述玻璃接合用薄膜与不具有上述浓度梯度的基准薄膜相比可以具有1.3倍以上的接合力调节效果。上述基准薄膜为同样地适用除了具有上述浓度梯度之外的其他条件的玻璃接合用薄膜。
上述玻璃接合用薄膜的特征在于，上述玻璃接合用薄膜的两个表面可以与上述薄膜的中心相比含有分布更广的上述金属盐或上述金属离子。
上述玻璃接合用薄膜可以具有从上述玻璃接合用薄膜的一侧表面向另一侧表面的根据深度的上述金属盐或金属离子的浓度分布呈U形的浓度梯度。
上述金属盐的含量以上述玻璃接合用薄膜整体为基准可以为200ppm以下。
上述玻璃接合用薄膜在玻璃接合的状态下在65℃95％rh的恒温恒湿室中放置2周之前和之后的黄度变化量可以为2.5以下。
根据本发明的另一实施例的玻璃接合用薄膜的制备方法包括：熔融步骤，通过熔融包含聚乙烯醇缩醛树脂、增塑剂及金属盐的组合物来制备熔融树脂；及成型步骤，通过对将上述熔融树脂排出并成型为薄膜形状的成型部的至少一部分施加电压来形成玻璃接合用薄膜。
上述玻璃接合用薄膜可以以上述玻璃接合用薄膜整体为基准的每10ppm的上述金属盐的含量获得8.5kgf/cm2以上的接合力调节效果。
上述玻璃接合用薄膜可以具有不均匀的浓度梯度，即上述玻璃接合用薄膜的表面与上述玻璃接合用薄膜的中心部相比以更高的浓度包含上述金属盐或金属离子的。
在上述成型步骤中施加的电压可以为8kV以下。
上述成型部可以包括：排出口；模唇，位于上述排出口两侧；及电压施加部，位于上述模唇。
在上述成型步骤中，上述电压可以通过上述电压施加部施加。
在上述成型步骤中施加的电压可以将包含在上述熔融树脂中的金属离子移动到所排出的熔融树脂的表面，以在熔融树脂的表面上形成高浓度区域。
发明的效果
本发明的玻璃接合用薄膜从玻璃接合用薄膜的表面向厚度方向具有金属盐的浓度梯度，因此可以提供于易调节接合力且水分敏感性得到改善的玻璃接合用薄膜。
附图说明
图1为说明在本发明的实施例中适用的用于调节薄膜表面的离子浓度的模唇的装置结构的示意图。
图2为说明在本发明的实施例中测量的白化距离的测量方法的图。
图3为说明在本发明的实施例中用于评价CSS接合力的装置的概略图。
具体实施方式
*与关联申请的相互参照
本申请要求于2018年12月10日提交的韩国专利申请第10-2018-0157930号的优先权的权益，上述优先权的基础申请全文通过引用纳入本文。
下面，参照附图来对本发明的实施例进行详细说明，以使本发明所属技术领域的普通技术人员轻松实现本发明。本发明可通过多种不同的实施方式实现，并不限定于在本说明书中所说明的实施例。纵贯全文，对相似的部分适用了相同的附图标记。
在全体说明书中，作为马库什型描述中包含的术语的“其组合”是指，从由马库什型描述的多个构成要素组成的组中选择的一个以上的混合或组合，从而表示包括从由上述多个构成要素组成的组中选择的一个以上。
在全体说明书中，除非另有说明，如“第一”、“第二”或“A”、“B”等术语用于将相同的术语彼此区分。另外，除非上下文另有明确说明，单数形式旨在还包括复数形式。
在全体说明书中，“～”类可以是指在化合物内包含相当于“～”的化合物或“～”的衍生物。
在本说明书中，“B位于A上”是指B以与A直接接触的方式位于A上，或是指B在A与B之间夹着其他层的状态下位于A上，而不限于B以与A的表面直接接触的方式位于A上的意思。
在本说明书中，ppm以质量为基准计算。
在本说明书中，除非另有说明，单数的表示可解释为包括从文脉解读的单数或复数的含义。
本发明的发明人发现，在为了获得接合力调节效果而适用比较大量的金属盐化合物的情况下容易出现黄变现象，并在研究对此的解决方法的过程中，确认了即使适用类似量的接合力调节剂也能够调节接合力调节效果，或即使适用更少量也能够有效地调节接合力的方法，从而完成了本发明。本发明的发明人发现，在薄膜的制备过程中，通过施加电压使薄膜的表面侧具备更多的金属盐衍生金属离子的方式制备具有金属离子浓度梯度的薄膜，确认了将为了获得接合力调节效果而适用的金属盐化合物的适用量与以往相比实质上降低到等同量以下的同时，能够获得接合力调节效果，且耐湿性和/或耐久性也实质上改善，从而完成了本发明。
为了达到上述目的，根据本发明的一实施例的玻璃接合用薄膜保护聚乙烯醇缩醛树脂、增塑剂及金属盐。上述玻璃接合用薄膜具有不均匀的浓度梯度，即上述玻璃接合用薄膜的表面与上述玻璃接合用薄膜的中心部相比以更高的浓度的包含金属盐或金属离子的。
当从上述玻璃接合用薄膜的表面向内侧根据厚度适用不同的金属离子浓度时，可以提供玻璃接合用薄膜，其中，即使以相同量的金属盐化合物作为接合力调节剂，也由于以使金属盐化合物，尤其金属阳离子的分布集中于表面的方式具有浓度梯度而具有不同接合力。
这表明，具有接合力调节效果的添加剂(包含衍生自该添加剂的物质)充分作用于与接合的玻璃相互作用的玻璃接合用薄膜上，但玻璃接合用薄膜整体上使用相对少量的金属盐化合物，由此也可以获得改善玻璃接合用薄膜的水分敏感性的效果。
上述玻璃接合用薄膜的特征在于，上述玻璃接合用薄膜的两个表面可以与上述玻璃接合用薄膜的中心相比分布有更多的上述金属盐或上述金属离子。
上述玻璃接合用薄膜可以具有从上述玻璃接合用薄膜的一侧表面向另一侧表面的根据深度的上述金属盐或金属离子的浓度分布呈U形的浓度梯度。当具有这种浓度梯度时，可以将上述金属盐或金属离子以最有效的形式分布于上述玻璃接合用薄膜中。
上述U形并不意味着绝对的U形状，而是意味着整体上根据深度的金属离子浓度曲线图具有U形，不仅用于与“-”形区别开，还用于与如W形、L形、M形或N形区别开。
具体而言，上述TOF-SIMS通过将一次溅射时将要削掉的玻璃接合用薄膜的表面的厚度调节至1nm来适用，以对根据通过反复的溅射被削掉的厚度检测的量进行测量的结果为基准，上述玻璃接合用薄膜以每10nm的平均金属离子浓度为基准，在5至85nm处的浓度可以高于在105至155nm处的浓度，更具体而言，可以高2倍以上。
并且，上述玻璃接合用薄膜从6nm到15nm为止的金属离子浓度测量值可以为从96nm到105nm为止测量的金属离子浓度测量值的4倍以上。
这种浓度分布表明在表面侧的金属离子浓度与其他部分相比相当高。
以上述玻璃接合用薄膜整体为基准，每10ppm的上述金属盐含量可以获得8.5kgf/cm2以上的接合力调节效果，或可以获得8.5至50kgf/cm2的接合力调节效果，或可以获得9.5至40kgf/cm2的接合力调节效果。
上述接合力调节效果是指上述玻璃接合用薄膜的表面和玻璃表面的接合力调节，以CSS接合力为基准进行评价。
上述玻璃接合用薄膜与其他条件相同但不具有上述浓度梯度的基准薄膜相比可以具有1.3倍以上的接合力调节效果，具体而言，可以具有2倍以上的接合力调节效果，或可以具有3倍以上的接合力调节效果。
并且，上述玻璃接合用薄膜根据上述施加电压的强度可以具有4倍以上的接合力调节效果，或也可以具有2倍至6倍的接合力调节效果。
如上所述，上述玻璃接合用薄膜在适用相对少量的金属盐的同时具有相当优异水平的接合力调节效果，因此可以实质上防止发生当过量使用金属盐时会发生的耐湿性降低等缺点，且可以提高耐黄变特性等。
上述金属盐的含量以上述薄膜整体为基准可以为200ppm以下，或可以为150ppm以下，或可以为100ppm以下，或可以为1至80ppm。
上述金属离子可以包含二价金属离子或一价金属离子。
上述金属离子可以由二价金属离子或一价金属离子构成。
上述二价金属离子可以是镁二价离子。
上述一价金属离子可以是钠一价离子、钾一价离子及它们的组合。
上述金属离子可以是选自由镁二价离子、钾一价离子及它们的组合组成的组中的任一种。
由于关于上述金属盐的更具体说明与下面的关于组合物说明的内容重复，因此将省略其描述。
上述玻璃接合用薄膜通过将包括上述玻璃接合用薄膜的接合玻璃在65℃95％rh的恒温恒湿室中放置2周后取出来测量的白化距离为5mm以下，这意味着具有优异的耐湿特性。
上述玻璃接合用薄膜通过将包括上述玻璃接合用薄膜的接合玻璃在65℃95％rh的恒温恒湿室中放置2周之前和之后测量的黄度变化量可以为2.5以下。
包括上述玻璃接合用薄膜的接合玻璃的冲击接合力等级可以为3至4级。
上述玻璃接合用薄膜的厚度可以为0.4mm以上，具体而言，可以为0.4至1.6mm，或可以为0.5至1.2mm，或可以为0.6至0.9mm。当以这种厚度制备上述薄膜时，可以提供轻薄且具有优异的耐冲击性和耐穿透性等的特性的薄膜。
图1为说明在本发明的实施例中适用的用于调节薄膜表面的离子浓度的模唇的装置结构的示意图。参照图1，下面将更详细地说明本发明。根据本发明的另一实施例的玻璃接合用薄膜的制备方法包括熔融步骤和成型步骤，从而制备在每10ppm的上述金属盐含量获得8.5kgf/cm2以上的接合力调节效果的玻璃接合用薄膜，上述金属盐含量以上述玻璃接合用薄膜的总含量为基准。
上述玻璃接合用薄膜可以具有不均匀的浓度梯度，即上述玻璃接合用薄膜的表面与上述玻璃接合用薄膜的中心部相比以更高的浓度包含金属盐或金属离子。
上述熔融步骤为通过熔融包含聚乙烯醇缩醛树脂、添加剂及金属盐的组合物来制备熔融树脂的步骤。
上述金属盐可以以金属盐状态或金属离子的形式存在于上述玻璃接合用薄膜中。
在上述熔融步骤中，可以适用应用于常规薄膜制备的树脂熔融方法，例如，可以适用双螺杆挤出机。
在后面将描述包含上述聚乙烯醇缩醛树脂和添加剂的组合物以及包含在上述添加剂中的金属盐。
上述成型步骤是通过对成型部的至少一部分施加电压来形成玻璃接合用薄膜的步骤，上述成型部用于将上述熔融树脂排出并成型为薄膜形状。
作为上述成型部，只要可在控制厚度的同时制成薄膜形状，就可以适用，在制备单层薄膜的情况下，可以将树脂放在挤出机(例如，双螺杆挤出机)中熔化并排出，以在通过T型模头控制厚度的同时制成薄膜形状，在多层薄膜的情况下，可以将树脂放在挤出机中分别熔融挤出后，通过如进料块和多歧管等的层压装置层压，然后在T型模头中成型为薄膜形状(共挤出方法)。
T型模头200位于上述成型部的一个末端，上述T型模头200包括供熔融树脂组合物1流入的流入口(图中未示出)和供熔融树脂组合物排出的流出口，且在上述流出口的用于排出熔融树脂组合物的部分两侧设有模唇210、230。在本发明的一实施例中，电压施加部220、240分别设在两侧的上述模唇210、230。例如，上述电压施加部220、240为如钨丝等的电压施加装置，其是能够向上述模唇210、230施加电压的装置。上述电压施加部220、240与外部电源装置(图中未示出)电连接。
上述电压施加部220、240通过调节上述模唇的电压来将上述熔融树脂1变成带电的熔融树脂2。上述带电的熔融树脂2包括高浓度区域3，其通过包含在熔融树脂1中的金属离子移动到表面而形成。上述高浓度区域3是指在下面将描述的表面离子浓度高于薄膜平均离子浓度的区域。在上述表面侧具有高浓度区域3的带电的熔融树脂2会在之后形成向厚度方向具有U状金属离子浓度梯度的玻璃接合薄膜。
适用于上述电压施加部220、240的电压可以为10kV以下的电压，或可以为1至10kV的电压，或可以为1.5至8kV的电压，或可以为2.5至6kV的电压。当上述电压过低时，向薄膜表面侧吸引作为阳离子的金属离子的力量较弱，因此难以诱导充分的浓度梯度，当适用过强的电压时，在高分子薄膜可能会发生劣化，且影响到玻璃接合用薄膜的光学特性、长期耐久性等的薄膜物理性能，反而会降低玻璃接合用薄膜的特性。
具体而言，当上述熔融树脂含有0.1至0.3wt％的金属盐时，可将从上述电压施加部施加的电压设为4至6kV，当上述熔融树脂含有大于0.3wt％且等于或小于0.8wt％的金属盐时，电压可以设为3至4kV。
上述电压可以被施加以吸引作为阳离子的上述金属离子，具体而言，可以被施加以带负电荷。
在上述成型步骤中施加的电压可以将包含在上述熔融树脂中的金属离子移动到所排出的熔融树脂的表面，以在熔融树脂的表面上形成高浓度区域。上述高浓度区域的范围和高浓度程度可以通过调节上述电压来在预定范围内变窄或变宽。
在上述成型步骤中成型的带电的熔融树脂2以每分钟5至15m的速度被排出以形成玻璃接合用薄膜，上述速度可以为每分钟5至15m，或可以为每分钟7至13m。
在上述成型步骤之后，可以以相同的方式适用通常用于制备玻璃接合用薄膜的工序，且将省略其详细描述。
将对用于形成上述熔融树脂的上述聚乙烯醇缩醛树脂和添加剂进行说明。
上述聚乙烯醇缩醛可以是通过用醛对聚合度为1,600至3,000的聚乙烯醇进行缩醛化而得到的聚乙烯醇缩醛，或可以是通过用醛对聚合度为1,700至2,500的聚乙烯醇进行缩醛化而得到的聚乙烯醇缩醛。当适用这种聚乙烯醇缩醛时，可以充分提高如耐穿透性等的机械物理性能。
上述聚乙烯醇缩醛可以是通过合成聚乙烯醇和醛而得到的，对上述醛的种类没有限制。具体而言，上述醛可以选自由正丁醛、异丁醛、正戊醛、2-乙基丁醛、正己醛及其共混树脂组成的组。当使用正丁醛作为上述醛时，所制备的聚乙烯醇缩醛树脂具有与玻璃的折射率差小的折射率特性，还具有与玻璃等的接合力优异的特性。
上述添加剂包含增塑剂。
上述增塑剂可以选自由三乙二醇双2-乙基己酸酯(3G8)、四乙二醇二庚酸酯(4G7)、三乙二醇双2-乙基丁酸酯(3GH)、三乙二醇双2-庚酸酯(3G7)、己二酸二丁氧基乙氧基乙酯(DBEA)、己二酸二-(2-丁氧基乙氧基乙酯)(DBEEA)、癸二酸二丁酯(DBS)、己二酸二己酯(DHA)及其混合物组成的组中，更具体而言，作为上述增塑剂，可以适用三乙二醇双2-乙基己酸酯(3G8)。
上述添加剂包含金属盐化合物。
上述金属盐化合物为了获得接合力调节效果而被适用，具体而言，可以适用碳原子数2至16的羧酸的金属盐，更具体而言，可以适用碳原子数2至12的二价金属的金属盐，或碳原子数2至6的一价金属的金属盐。
包含在上述金属盐化合物中的金属离子可以为选自由钠一价阳离子、镁二价阳离子及钾一价阳离子组成的组中的任一种。
上述金属盐化合物可以以金属盐化合物原状态或溶解于溶剂中而离子化的状态适用于上述组合物，且用作接合力调节剂。具体而言，上述金属盐化合物可以调节薄膜和玻璃表面之间的接合力。当上述金属盐化合物以溶液状态适用于上述组合物时，与在所制备的薄膜或接合层中相比，可以使金属盐化合物或来源自上述金属盐化合物的离子的分散和移动变得更加容易。
上述金属盐化合物的含量相对于上述熔融树脂整体可以为200ppm以下，或可以为150ppm以下，或可以为100ppm以下，或可以为1至80ppm。在本发明中，ppm以质量为基准。
上述熔融树脂可以构成单层薄膜，或也可以构成多层薄膜的表面层。
上述金属盐化合物可以以上述组合物整体为基准以如上所述的含量包含，从而制备成单层的玻璃接合用薄膜。并且，上述金属盐化合物可以以上述组合物整体为基准以如上所述的含量包含，从而制备成多层的玻璃接合用薄膜。在这种情况下，可以通过含有上述金属盐化合物的组合物形成多层薄膜的表面层(接合层)。
用于制备接合玻璃的聚乙烯醇缩醛树脂组合物可以与紫外线稳定剂(紫外线吸收剂)一起适用，以便提高紫外线阻断效果，并且苯并三唑类化合物可以用作上述紫外线稳定剂。
由于紫外线的能量，通过分子中的羟基与位于靠近上述羟基的三唑环中所含的氮之间的相互作用，可能导致苯并三唑类化合物的键合结构发生变化，此时，若金属离子参与，则作为紫外线稳定剂的效果会降低。并且，苯并三唑类化合物与多价金属离子配位键合形成螯合环，但是以这种方式形成螯合环的苯并三唑类化合物不能充分起到紫外线稳定剂的作用，且可能削弱整个薄膜的耐久性。
作为上述紫外线稳定剂，只要作为紫外线稳定剂被适用，就可以不受限制地适用，也可以适用包含苯并三唑类化合物的紫外线稳定剂。具体而言，可以使用Chemipro Kasei公司的Chemisorb 12、Chemisorb 79、Chemisorb 74、Chemisorb 102及巴斯夫(BASF)公司的Tinuvin 328、Tinuvin 329、Tinuvin 326等。
在本发明中，为了使适用于玻璃接合用薄膜制备的苯并三唑类化合物作为紫外线稳定剂起到充分的功能并提高玻璃接合用薄膜本身的耐久性，制备成即使适用少量也具有优异的接合力调节效果。
上述金属盐化合物的含量相对于100重量份的上述苯并三唑类化合物可以为16重量份以下，或可以为12重量份以下，或可以为1至10重量份。当上述金属盐化合物的含量相对于100重量份的上述苯并三唑类化合物小于1重量份时，通过添加上述金属盐化合物获得的接合力调节效果可能不充分，当上述金属盐化合物的含量大于16重量份时，耐水性反而会降低。
上述组合物根据需要还可包含选自由抗氧化剂、热稳定剂、IR吸收剂及其组合组成的组中的添加剂。上述添加剂可以被包含在上述各层中至少一层中，或也可以被包含在整个薄膜中。
通过在上述组合物中包含上述添加剂来可以改善如薄膜的热稳定性、光稳定性等的长期耐久性和防散射性能。
上述抗氧化剂可以是受阻胺(hindered amine)类或受阻酚(hindered phenol)类抗氧化剂。具体而言，在要求150℃以上的工艺温度的聚乙烯醇缩丁醛(PVB)的制造工序中，受阻酚类抗氧化剂是更优选的。作为受阻酚类抗氧化剂可以使用巴斯夫(BASF)公司的IRGANOX 1076、1010等。
考虑到与抗氧化剂的相容性，上述热稳定剂可以使用亚磷酸酯(phosphite)类的热稳定剂。例如，可以使用巴斯夫(BASF)公司的IRGAFOS168。作为上述IR吸收剂，可以使用ITO、ATO、AZO等，但本发明不限于此。
根据本发明的又一实施例的接合玻璃包括层叠体，上述层叠体在两张玻璃之间包括如上所述的玻璃接合用薄膜。
在本说明书中以上述两张玻璃为玻璃的情况为例说明，但是只要是透光面板就可以适用，并且可以适用塑料等的材料。
关于上述玻璃接合用薄膜的具体结构、组成、特征及制备方法等的内容与上述内容重复，因此将省略其描述。
上述接合玻璃通过将100mm*100mm面积的试片在65℃95％rh的恒温恒湿室中放置2周后取出来测量的平均白化距离为5mm以下，或可以为0至5mm，或可以为0.1至5mm。这种平均白化距离意味着即使在高温高湿条件下也具有相当优异的耐水性。
通过将上述接合玻璃在65℃95％rh的恒温恒湿室中放置2周之前和之后测量的黄度变化量可以为2.5以下。这表示具有优异的长期耐久性的结果，尤其，在同时包含苯并三唑类化合物和金属盐的薄膜的情况下，可以被评价为更优异的结果。
上述接合玻璃的CSS接合力可以为160至320kgf/cm2，或可以为160至280kgf/cm2，或可以为180至260kgf/cm2。这是玻璃和薄膜之间的适当的接合力范围，即意味着具有用作安全玻璃所需的充分的接合力。
在下文中，将参考具体实施例更详细地描述本发明。然而，应理解，这些实施例仅是用于帮助理解的示例，不应解释为限制本发明的范围。
1.材料的准备
1)制备添加剂组合物
通过混合相对于整个薄膜为0.15wt％的作为抗氧化剂的Irganox1010、0.3wt％的作为紫外线吸收剂的TINUVIN P、作为金属盐接合力调节剂的0.15wt％的乙酸镁(Mgacetate)及0.13wt％的乙酸钾(Mg acetate)来制备添加剂组合物1。
通过混合相对于整个薄膜为0.15wt％的作为抗氧化剂的Irganox1010、0.3wt％的作为紫外线吸收剂的TINUVIN P及0.56wt％的作为金属盐接合力调节剂的乙酸钾(Mgacetate)来制备添加剂组合物2。
通过混合相对于整个薄膜为0.15wt％的作为抗氧化剂的Irganox1010、0.3wt％的作为紫外线吸收剂的TINUVIN P、作为金属盐接合力调节剂的0.45wt％的乙酸镁(Mgacetate)及0.38wt％的乙酸钾(Mg acetate)来制备添加剂组合物3。
2)制备聚乙烯醇缩丁醛树脂(A)
将聚合度为1700、皂化度为99的聚乙烯醇缩醛树脂和正丁醛加入到反应器中，并进行常规聚乙烯醇缩丁醛树脂的合成过程，从而得到包含20.1wt％羟基、79.2wt％缩丁醛及0.7wt％乙酰基的聚乙烯醇缩丁醛树脂。
2.制备聚乙烯醇缩丁醛薄膜
1)用于实施例的薄膜制备的设定
为了调节薄膜表面的离子浓度，适用了在模唇210、230(DIE LIP)部分安装有钨丝220、240(由VWF Industries公司制造)的特殊类型的装置。
钨丝220、240的两端都连接到发电机，以便可以向上述钨丝施加电压，并且可以根据发电机的模式选择“正(POSITIVE)”或“负(NEGATIVE)”来向钨丝赋予(+)或(-)的特性。在本发明中，在实施例中为了控制金属离子的浓度分布，选择负(NEGATIVE)模式来使用(参照图1)。
2)实施例1至4的薄膜制备
在双螺杆挤出机中加入72.27wt％聚乙烯醇缩丁醛树脂(A)、27wt％的3G8作为增塑剂及0.73wt％的添加剂组合物1作为添加剂，熔融挤出，然后用在上面设定的装置通过T型模头以每分钟10M的速度制备成总厚度为760μm的薄膜形式。此时，通过在1至6kV的范围内改变施加电流并适用(参照表1)。
3)比较例1的薄膜制备
除了在没有施加电压的状态下制备之外，其余以与实施例1的薄膜相同的方式制备比较例1的薄膜。
4)比较例2的薄膜制备
在双螺杆挤出机中加入71.99wt％聚乙烯醇缩丁醛树脂(A)、27wt％的3G8作为增塑剂及1.01wt％的添加剂(2)，进行挤出，然后通过T型模头(T-DIE)以每分钟10M的速度制备成总厚度为760μm的薄膜形式。与比较例1相同地，没有施加电压。
5)比较例3的薄膜制备
在双螺杆挤出机中加入71.72wt％聚乙烯醇缩丁醛树脂(A)、27wt％的3G8作为增塑剂及1.28wt％的添加剂(3)，进行挤出，然后通过T型模头(T-DIE)以每分钟10M的速度制备总厚度为760μm的薄膜形式。与比较例1相同地，没有使用施加工序。
6)CSS比较样品制备
在双螺杆挤出机中加入73wt％的聚乙烯醇缩丁醛树脂(A)和27wt％的3G8作为增塑剂之后，进行挤出，通过T型模头(T-DIE)以每分钟10M的速度制备总厚度为760μm的薄膜形式。将该样品作为CSS接合力评价中的CSS值比较样品。
3.聚乙烯醇缩丁醛薄膜的物理性能评价
1)用于评价耐久性/耐水性的接合玻璃样品的制备
将实施例1至4和比较例1至3的薄膜在20℃和30％RH下放置1周，然后切成长*宽为100mm*100mm的尺寸，并在两面安装两张2.1T(mm，以下相同)的透明玻璃，以2.1T玻璃-薄膜-2.1T玻璃的层叠结构在真空层压机中在120℃和1大气压下预接合20秒。
之后，将预接合的玻璃-薄膜-玻璃的层叠体在高压釜中进行主接合，从而获得接合玻璃样品。作为主接合的条件，适用了从室温到140℃升温25分钟且在140℃下保持25分钟的条件。
2)耐久性评价：黄度变化量(d-YI)评价方法
使用Hunter Lab公司的Ultra Scan Pro，在D65和10℃条件下，根据ASTM E313标准，测量在上面制备的接合玻璃样品的正中心的黄度初始值(YIinitial)。将完成测量黄度初始值的试片在65℃95％rh的恒温恒湿室内放置2周，将其取出后，以与上述相同的方式再次测量黄度，以测量黄度完成值(Yifinal)，并通过以下式(2)计算黄度差。
式(2)d-YI＝YIfinal–YIinitial
由上述式(2)获得的值为2.5以下时，评价为合格(Pass)，大于2.5时，评价为不合格(Fail)。
3)耐湿性评价：白化距离测量
将以在上面制备的接合玻璃样品100在65℃95％rh的恒温恒湿室中放置2周后取出，用肉眼确认从四边的中心发生雾化(haze)的部分(出现白化现象的区域，10)用尺子测量其距离(参考图2)，并根据下述式(3)计算四边的值的平均值，并将其表示为白化距离(mm)。
式(3)平均白化距离＝(d1+d2+d3+d4)÷4
在上述式(3)中，将在第一边至第四边的正中心处测得的出现白化现象的距离分别称为d1至d4(单位为mm)。
当平均白化距离为5mm以下时，评价为合格(Pass)，超过5mm时，评价为不合格(Fail)。
4)CSS接合力评价
通过压缩剪切强度(Compressive Shear Strength，CSS)的接合力评价对聚乙烯醇缩醛薄膜与玻璃之间的接合力进行评价。
参照图3说明测量方法：通过将在上述实施例和比较例中制备的PVB膜120和CSS比较样品120在宽度方向的正中央切割成300mm*300mm的尺寸，在20℃和20％RH下放置1周进行调理。通过在上述薄膜的两面上安装两张2.1T透明玻璃110、130，以宽*长为50mm*150mm的2.1T玻璃-薄膜-2.1T玻璃的层叠结构在真空层压机中在150℃和1大气压下进行预接合50秒。之后，在高压釜中以从常温到140℃升温25min且在140℃下保持30min的条件进行主接合，从而获得接合玻璃样品100。
将以接合玻璃形式制备的试片在20℃和20RH下放置一小时以除热，然后使用穿孔器制备切成直径为1英寸(25.4mm)的圆形的用于CSS评价的样品。再次将评价用样品在20℃和20％RH下放置并进行调理2小时，然后取出，将样品安装在倾斜为45°的CSS用夹具310、320(支架)上，并使用通用测试装置(UTM)以每分钟2.54mm的速度进行压缩测试，测量在样品中力最大的地点上的力量的值(kgf)。作为测量，每个样品进行重复测试五次，计算除最高和最低值外的三个点的平均值，并将其表示为CSS接合力(参照表1)。
5)接合力调节效果计算
使用在上述4)中计算出的CSS接合力值，通过以下式(1)计算薄膜中每10ppm的金属盐含量的接合力调节效果。
式(1)：
Figure BDA0003090617410000161
在上述式(1)中，上述CP10是每10ppm金属盐的CSS接合力调节效果，上述SS是CSS比较样品的CSS值，上述TS是实施例或比较例样品的CSS测量值，Cm是金属盐添加量(ppm)。
[表1]
Figure BDA0003090617410000162
Figure BDA0003090617410000171
*接合力调节效果上升率是以百分比表示基于比较例1的每10ppm的CSS接合力调节效果值的实施例1至4的每10ppm的CSS接合力调节效果值的比率的值。
参照上述表1的比较例1和实施例1至4，可以确认，随着施加电压的增加，适用相同类型和含量的金属盐的薄膜的CSS接合力减少。施加5或6kV的电压的实施例4、5与适用约3倍的金属盐的比较例2或比较例3相比具有类似或更调节的接合力值。
就每10ppm的CSS接合力调节效果而言，根据施加的电压逐渐显示出优异的效果，但是还可以确认，与5V相比，在6V的情况下增加程度降低。
参考上述表1中的结果，即使与现有的薄膜相比适用少量的金属盐接合力调节剂，上述薄膜也能够获得与现有薄膜相同或更高的接合力调节效果，在获得足够的接合力调节效果的同时，能够防止发生当多量适用金属盐时可能发生的问题，即耐久性下降和/或耐湿性降低。
如上所述，虽然对本发明的优选实施例进行了详细说明，但本发明的权利范围不限于此，且使用在权利要求书中定义的本发明的基本概念的本领域技术人员的各种变更或变形均属于本发明的范围。
*附图标记说明
1：熔融树脂 2：带电的熔融树脂
3：高浓度区域
200：T型模头 210：第一模唇
220：第一电压施加部 230：第二模唇
240：第二电压施加部
300：CSS评价装置 310：第一夹具
320：第二夹具
100：接合玻璃 110：第一玻璃
120：接合薄膜 130：第二玻璃
10：出现白化现象的区域 20：没有出现白化现象的区域
d1：在第一边的白化距离 d2：在第二边的白化距离
d3：在第三边的白化距离 d4：在第四边的白化距离

Claims (10)

1.一种玻璃接合用薄膜，其特征在于，
包含聚乙烯醇缩醛树脂、增塑剂及金属盐，
且每10ppm的上述金属盐的含量具有8.5kgf/cm2以上的接合力调节效果。
2.根据权利要求1所述的玻璃接合用薄膜，其特征在于，
具有不均匀的浓度梯度，即上述玻璃接合用薄膜的表面与上述玻璃接合用薄膜的中心部相比以更高的浓度包含上述金属盐或金属离子。
3.根据权利要求1所述的玻璃接合用薄膜，其特征在于，
与不具有上述浓度梯度的基准薄膜相比，具有1.3倍以上的接合力调节效果。
4.根据权利要求1所述的玻璃接合用薄膜，其特征在于，
上述玻璃接合用薄膜的两个表面与上述玻璃接合用薄膜的中心相比含有分布更多的上述金属盐或上述金属离子。
5.根据权利要求1所述的玻璃接合用薄膜，其特征在于，
具有从上述玻璃接合用薄膜的一侧表面向另一侧表面的根据深度的上述金属盐或金属离子的浓度分布呈U形的浓度梯度。
6.根据权利要求1所述的玻璃接合用薄膜，其特征在于，
在65℃95％rh的恒温恒湿室中放置2周之前和之后的黄度变化量为2.5以下。
7.一种玻璃接合用薄膜的制备方法，其特征在于，
包括：
熔融步骤，通过熔融包含聚乙烯醇缩醛树脂、增塑剂及金属盐的组合物来制备熔融树脂，及
成型步骤，通过对将上述熔融树脂排出并成型为薄膜形状的成型部的至少一部分施加电压来形成玻璃接合用薄膜；
制备以上述薄膜整体为基准的每10ppm的上述金属盐的含量获得8.5kgf/cm2以上的接合力调节效果的上述玻璃接合用薄膜。
8.根据权利要求7所述的玻璃接合用薄膜的制备方法，其特征在于，
在上述成型步骤中施加的电压为8kV以下。
9.根据权利要求7所述的玻璃接合用薄膜的制备方法，其特征在于，
上述成型部包括：
排出口，
模唇，位于上述排出口两侧，及
电压施加部，位于上述模唇；
在上述成型步骤中，上述电压通过上述电压施加部施加。
10.根据权利要求7所述的玻璃接合用薄膜的制备方法，其特征在于，
在上述成型步骤中施加的电压将包含在上述熔融树脂中的金属离子移动到所排出的熔融树脂的表面，以在熔融树脂的表面上形成高浓度区域。
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