CN105504620A - 具有光致变色性质的含有增塑剂的聚乙烯醇缩醛的多层膜 - Google Patents

具有光致变色性质的含有增塑剂的聚乙烯醇缩醛的多层膜 Download PDF

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CN105504620A
CN105504620A CN201510643298.2A CN201510643298A CN105504620A CN 105504620 A CN105504620 A CN 105504620A CN 201510643298 A CN201510643298 A CN 201510643298A CN 105504620 A CN105504620 A CN 105504620A
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film
interlayer film
photochromic
polyvinyl acetal
polyvinyl
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六车慎一
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Kuraray Europe GmbH
Kuraray Co Ltd
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Abstract

本发明公开了“具有光致变色性质的含有增塑剂的聚乙烯醇缩醛的多层膜”。本发明涉及由至少两个基于含有增塑剂的聚乙烯醇缩醛的单个膜组成的用于层叠玻璃的光致变色夹层膜，其特征在于所述单个膜包含至少一种光致变色化合物并具有相差至少5？K的玻璃化转变温度。

Description

具有光致变色性质的含有增塑剂的聚乙烯醇缩醛的多层膜
技术领域
本发明涉及适于作为层叠安全玻璃中的夹层的含有增塑剂的膜，所述膜由至少两个基于含有增塑剂的聚乙烯醇缩醛的单个膜组成，其中所述单个膜包含光致变色化合物并具有不同的玻璃化转变温度。
背景技术
层叠安全玻璃通常由两块玻璃板和中间膜组成，所述中间膜将玻璃板粘合在一起。含有增塑剂的部分缩醛化的聚乙烯醇（聚乙烯醇缩醛），特别是聚乙烯醇缩丁醛（PVB）主要用作膜材料。层叠安全玻璃（LSG）例如在汽车行业中用作挡风玻璃或侧窗，以及在建筑行业中用作安全玻璃。
为了减少穿过层叠玻璃的阳光的量，长久以来已知的是向层叠玻璃的夹层膜中添加颜料或染料。此类着色对于挡风玻璃或建筑物用途是已知的，用于减少通过该层叠玻璃的传热。
将该膜着色或染色永久降低透明度。在没有阳光的情况下，尤其是在晚上，透明度可能变得过低。因此，向该夹层膜中引入光致变色化合物，所述化合物根据施加在该膜上的阳光辐射的强度而改变它们的颜色或暗度。光致变色化合物通过UV辐射由透明或略微着色状态变为深色状态。由深色向透明或略微着色（脱色）的逆反应通常是温度依赖性的。此类技术例如公开在US427742中。
该脱色反应以及由此在该夹层的透明与深色状态之间的切换时间取决于窗玻璃的温度，导致在高温下的快速脱色和在低温下的缓慢脱色。
这可能导致在较高温度下的透明膜和在较低温度下的深色膜，而与施加在该膜上的辐射无关。此类切换行为是不合意的，因为在夏天（高温和高辐射量），需要更深色的膜以阻挡阳光（且在冬天反之亦然）。
发明内容
因此，本发明的一个目的是提供具有降低的温度依赖性切换行为的用于层叠窗玻璃的夹层膜。
已经发现，脱色反应的速度以及由此在该夹层的透明与深色状态之间的切换时间可以受到该夹层的Tg影响。
本发明基于选择至少两种单独的基于含有增塑剂的聚乙烯醇缩醛的光致变色夹层膜（其具有不同的玻璃化转变温度），而不是选择具有作为高温与低温（例如在夏天和冬天）之间的折衷的平均Tg的夹层膜。根据温度，各膜表现出不同的切换行为。采用此类选择，所观察到的切换时间看上去几乎与温度无关。
本发明的目的因此是由至少两个基于含有增塑剂的聚乙烯醇缩醛的单个膜组成的用于层叠玻璃的光致变色夹层膜，其特征在于所述单个膜各自包含至少一种光致变色化合物并具有相差至少5 K的玻璃化转变温度。优选地，该单个膜的玻璃化转变温度相差至少10、15或20 K。
玻璃化转变温度方面的差异可以通过单个膜的不同增塑剂含量来实现。该单个膜的增塑剂含量优选相差至少5重量%，更优选相差至少10重量%和尤其相差至少15重量%。
在本发明的另一实施方案中，玻璃化转变温度方面的差异可以通过各个单个膜中聚乙烯醇缩醛的不同化学来实现。优选地，第一单个膜包含具有0.1至11摩尔%、优选0.1-4摩尔%、更优选0.1-2摩尔%的聚乙酸乙烯酯基团部分的聚乙烯醇缩醛。独立于该第一单个膜，第二单个膜可以包含具有5至8摩尔%、优选5至7.9摩尔%、更优选5至7.5摩尔%、最优选5至7.5摩尔%或5.3至7.2摩尔%的聚乙酸乙烯酯基团部分的聚乙烯醇缩醛。
除了光致变色特征之外，该夹层膜可以具有声音衰减性质。在本发明的这种实施方案中，一个或多个包含光致变色化合物的该单个膜可以具有声音衰减性质。此外，该夹层膜可以包含附加的单个膜，其不包含光致变色化合物并具有声音衰减性质。
按照ISO/PAS 16940（如07/16/2002）在由厚度为0.8毫米的夹层膜所组成的试样上测定该声音衰减性质特征，所述夹层膜层叠在两块厚度为2毫米的玻璃板之间。每次测定第一模式。
本发明的夹层膜的吸音效果应当在未来的玻璃层叠件的应用温度下最高。在汽车玻璃中，该应用温度为大约20℃，因为该窗户在冬天被加热，在夏天被空调装置冷却。在上述实验设置中，本发明的膜优选在17.5-22.5℃的温度范围内表现出最大衰减；在这里尤其是大于22%、优选大于23%和更优选大于24%的衰减值。
优选地，本发明的膜在2毫米玻璃/0.8毫米膜/2毫米玻璃层叠件中表现出根据ISO/PAS 16940（如07/16/2002）测得的大于10%的在10℃下的第一模式衰减值、大于10%的在15℃下的第一模式衰减值和大于21%的在20℃下的第一模式衰减值。
根据本发明使用的该单个膜可以各自以几乎任意厚度使用，只要不会不利地改变该隔音特征。所有单个膜例如可以具有相同的厚度；但是，不同厚度的单个膜的组合也是可能的。
该光致变色夹层膜可以由至少三个单个膜组成（A/B/A），其中在该夹层膜外侧上的两个单个膜（A）具有与夹层膜内侧上的单个膜（B）的玻璃化转变温度相差至少5 K的玻璃化转变温度。
在三层膜A/B/A形式的本发明的夹层膜的优选排列中，外层膜A具有大致相同的厚度，而内层膜B可以尽可能薄。多层膜总厚度为0.76毫米，该内层膜可以具有0.075至（bis）0.32毫米的厚度。
本发明的多层膜优选具有例如0.38、0.76、1.14毫米（即0.38毫米的倍数）的行业惯例总厚度。
本发明中使用的光致变色化合物可以是有机染料或无机颜料，例如选自三芳基甲烷类、芪类、氮杂芪类、硝酮类、俘精酸酐类、螺环吡喃类、萘并吡喃类、螺环-噁嗪类和醌类的化合物。
作为实例，下式显示了光致变色化合物的切换反应：
。
本发明的单个膜包含含有增塑剂的聚乙烯醇缩醛，所述聚乙烯醇缩醛通过用醛来缩醛化完全或部分皂化的聚乙烯醇获得。第一单个膜包含具有17-22重量%、优选18-21重量%和更优选19.5-20.5重量%的聚乙烯醇基团部分的聚乙烯醇缩醛。优选地，第二单个膜包含具有小于14重量%、优选11-13.5重量%和更优选小于11.5-13重量%的聚乙烯醇基团部分的聚乙烯醇缩醛。
增塑剂与部分缩醛化的聚乙烯醇的相容性通常随着该增塑剂的降低的极性特征而降低。具有较高极性的增塑剂因此与具有较低极性的那些增塑剂相比与聚乙烯醇缩醛的相容性更高。或者，具有较低极性的增塑剂的相容性随着提高的缩醛化程度（即随着聚乙烯醇缩醛的羟基数量的降低以及由此造成的极性的降低）而提高。
由于聚乙烯醇基团的不同部分，该单个膜可以采用不同的增塑剂量，而不会发生增塑剂的渗出。优选地，基于该膜的配方，该单个膜因此包含相差至少5重量%、更优选相差至少7.5重量%和最优选相差至少10重量%的增塑剂含量。
该单个膜可以含有相同或不同的增塑剂。使用相同的增塑剂是优选的；单个膜中增塑剂共混物的组成有可能因迁移而略微改变。
该单个膜可以包含对于PVB膜已知的下列增塑剂的至少一种的增塑剂或增塑剂共混物：
- 多价脂族或芳族酸的酯，例如己二酸二烷基酯如己二酸二己酯、己二酸二辛酯、己二酸己基环己酯、己二酸庚酯和壬酯的混合物、己二酸二异壬酯、己二酸庚基壬酯和己二酸与含有脂环族键或醚键的酯醇的酯，癸二酸二烷基酯如癸二酸二丁酯和癸二酸与含有脂环族键或醚键的酯醇的酯，邻苯二甲酸的酯如邻苯二甲酸丁基苄酯或邻苯二甲酸双-2-丁氧基乙酯，环己烷二甲酸的酯如1,2-环己烷二甲酸二异壬酯，
- 具有一个或多个非支链或支链脂族或芳族取代基的多价脂族或芳族醇或低聚醚二醇的酯或醚，例如二-、三-或四-甘醇与直链或支链的脂族或脂环族羧酸的酯类；二乙二醇双(2-乙基己酸酯)、三乙二醇双(2-乙基己酸酯)、三乙二醇双(2-乙基丁酸酯)、四乙二醇双正庚酸酯、三乙二醇双正庚酸酯、三乙二醇双正己酸酯、四乙二醇二甲醚和/或二丙二醇苯甲酸酯可以作为后一类的实例，
- 与脂族或芳族酯醇的磷酸酯，如磷酸三(2-乙基己酯)（TOF）、磷酸三乙酯、磷酸二苯基-2-乙基己酯和/或磷酸三甲苯酯，柠檬酸、琥珀酸和/或富马酸的酯。
特别优选地使用以下增塑剂的一种或多种：
- 癸二酸二(2-乙基己酯)（DOS）、己二酸二(2-乙基己酯)（DOA）、己二酸二己酯（DHA）、癸二酸二丁酯（DBS）、双正庚酸三乙二醇酯（3G7）、双正庚酸四乙二醇酯（4G7）、三乙二醇双(2-乙基己酸酯)（3GO或3G8）、四乙二醇双(正-2-乙基己酸酯)（4GO或4G8）、己二酸二(2-丁氧基乙酯)（DBEA）、己二酸二(2-丁氧基乙氧基乙酯)（DBEEA）、癸二酸二(2-丁氧基乙酯)（DBES）、邻苯二甲酸二(2-乙基己酯)（DOP）、邻苯二甲酸二异壬酯（DINP）、双-异壬酸三乙二醇酯、三乙二醇双(2-丙基己酸酯)、1,2-环己烷二甲酸二异壬酯（DINCH）、磷酸三(2-乙基己酯)（TOF）和二丙二醇苯甲酸酯。
此外，本发明的单个膜可以包含本领域技术人员已知的其它添加剂如剩余量的水、UV吸收剂、抗氧化剂、粘附调节剂、光学增白剂、稳定剂、着色剂、加工助剂、有机或无机纳米粒子、热解法二氧化硅和/或表面活性物质。
在本发明的一个变体中，所有单个膜以大致相同的浓度包含提到的添加剂。在本发明的特殊变体中，该单个膜的至少一个不包含粘附调节剂（防粘剂）。在本发明的范围内，防粘剂指的是在其帮助下可以调节含有增塑剂的聚乙烯醇缩醛膜对玻璃表面的粘附力的化合物。这种类型的化合物对于本领域技术人员而言是已知的；在实践中，有机酸的碱金属盐或碱土金属盐，如乙酸钾/镁，常常用于此目的。
为了制造聚乙烯醇缩醛，将聚乙烯醇溶解在水中并在添加酸催化剂的情况下用醛如丁醛进行缩醛化。将沉淀的聚乙烯醇缩醛分离，洗涤至中性，任选地悬浮在呈碱性的水性介质中，此后再次洗涤至中性并干燥。
该聚乙烯醇缩醛的聚乙烯醇含量可以通过缩醛化反应中使用的醛的量来调节。还有可能使用具有2至10个碳原子的其它或几种醛（例如戊醛）来进行该缩醛化反应。
基于含有增塑剂的聚乙烯醇缩醛的膜优选含有通过用丁醛缩醛化聚乙烯醇获得的未交联的聚乙烯醇缩丁醛（PVB）。
还有可能使用交联的聚乙烯醇缩醛，特别是交联的聚乙烯醇缩丁醛（PVB）。合适的交联的聚乙烯醇缩醛例如描述在EP 1527107 B1和WO 2004/063231 A1（含羧基基团的聚乙烯醇缩醛的热自交联）、EP 1606325 A1（与聚醛交联的聚乙烯醇缩醛）和WO 03/020776 A1（与乙醛酸交联的聚乙烯醇缩醛）中。这些专利申请的公开内容经此引用完全并入本文。
水解的乙酸乙烯酯/乙烯共聚物的三聚物也可以在本发明的范围内用作聚乙烯醇。这些化合物通常水解至超过92摩尔%并含有1至10重量%的基于乙烯的单元（例如Kuraray Europe GmbH的“Exceval”类型）。
此外，由乙酸乙烯酯和至少一种附加的烯属不饱和单体能够的水解的共聚物也可以在本发明的范围内用作聚乙烯醇。
在本发明的范围内，该聚乙烯醇可以使用纯的形式或以具有不同聚合度或水解度的聚乙烯醇混合物的形式使用。本发明的夹层膜有可能由2、3、4或5个单个膜组成，相邻的单个膜具有提及的不同性质。
本发明的膜优选具有三个单个膜，第一和第三单个膜是相同的。
为了制造本发明的膜，可以首先通过挤出法分别地制造该单个膜并随后例如通过在薄膜卷绕机上将它们卷绕在一起来机械接合成本发明的夹层膜。
还有可能通过同时共挤出该单个膜来制造该夹层膜。该共挤出例如可以使用适当地装有共挤出模头或供料头（feed block）的设备来进行。
在汽车行业中，经常使用在上部区域中具有所谓着色带的膜。为此，该膜的上部可以与适当着色的聚合物熔体一起共挤出，或者该多层体系中的单个膜之一可以具有不同的颜色。在本发明中，这可以通过将至少一个单个膜完全或部分着色来实现。
本发明的膜或单个膜的制造通常通过挤出或共挤出来进行，其在特定条件下（熔体压力、熔体温度和模头温度）产生熔体断裂面，即随机的表面粗糙度。
或者，可以通过在至少一对辊之间的压印过程将规律的、非随机的粗糙度压印到本发明的已经制得的夹层膜上。压花膜在层叠玻璃生产过程中通常具有改善的脱气特征并优选用于汽车行业。
与生产方法无关，本发明的膜具有施加到一侧或更优选施加到两侧上的具有15至150微米的粗糙度Rz、优选15至100微米的Rz、更优选20至80微米的Rz和最优选40至75微米的Rz的表面结构。
本发明的膜也非常适于制造玻璃/膜/塑料层叠件，例如用于用PET层永久粘合玻璃板。两个塑料板（例如由聚碳酸酯或PMMA制成）的粘合采用本发明的膜也是可行的。
本发明的膜尤其可用于以本领域技术人员已知的方式通过与一个或多个玻璃板层叠来制造层叠安全玻璃。该层叠安全玻璃可用于汽车行业，例如用作挡风玻璃，或用于建筑行业，例如用于窗户或透明外立面元件，或用于家具制造。
本发明的膜的进一步用途是在制造光伏模块中。
基于聚乙烯醇缩醛的膜的生产与组成基本上例如描述在EP 185 863 B1、EP 1 118 258 B1、WO 02/102591 A1、EP 1 118 258 B1或EP 387 148 B1中。
测量程序
根据ASTM D 1396-92测定PVB的聚乙烯醇和聚乙酸乙烯酯含量。缩醛化程度（=丁醛含量）可以作为使根据ASTM D 1396-92测定的聚乙烯醇与聚乙酸乙烯酯含量之和达到一百所需要添加的部分来计算。重量%向摩尔%的转化根据本领域技术人员已知的公式来进行。
采用10 K/分钟的加热速率在-50℃-150℃的温度间隔内按照DIN 53765通过差示扫描量热法（DSC）来测定该部分缩醛化聚乙烯醇的玻璃化转变温度。采用第一加热速率（ramp）后接冷却速率并后接第二加热速率。按照DIN 51007由与第二加热速率相关的实测曲线来测定该玻璃化转变温度的位置。该DIN中心（TgDIN）定义为半阶高度处的水平线与实测曲线的交点。阶梯高度定义为中间切线与玻璃化转变之前和之后实测曲线的基线的两个交点之间的垂直距离。
褪色动力学的测量
使用具有50 KLux氙灯的紫外-可见光谱仪记录吸收光谱，该氙灯滤光至用于辐射的Air Mass 2条件。
该褪色时间（T½）计算为完全活化的光致变色染料至褪色至其整体光致变色活化的50%的时间（以秒为单位）。
实施例
制备具有不同的残余乙酸酯含量的聚乙烯醇缩醛
PVB 1：
将100重量份的聚乙烯醇Mowiol 29-99（Kuraray Europe GmbH的市售产品）溶解在1075重量份的加热至90℃的水中。在40℃的温度下，加入56.8重量份的正丁醛，并在12℃的温度下在搅拌的同时加入75重量份的20%的盐酸。将该混合物加热至69℃，在该聚乙烯醇缩丁醛（PVB）已沉淀后，在该温度下搅拌2小时。在冷却至室温后，将该PVB分离，用水洗涤至中性并干燥。获得具有20.0重量%（28.8摩尔%）的聚乙烯醇含量和1.3重量%（1摩尔%）的聚乙酸乙烯酯含量的PVB。
PVB 2：
按照实施例1制备PVB；使用具有93.1摩尔%的水解度的100重量份的聚乙烯醇Mowiol 30-92（Kuraray Europe GmbH的市售产品）和73重量份的正丁醛。获得具有11.6重量%（17.7摩尔%）的聚乙烯醇含量和9.1重量%（7.1摩尔%）的聚乙酸乙烯酯含量的PVB。
对本发明的目的而言，用表1中所示的组成制造不同的PVB膜。Reversacol Humber Blue和Reversacol Pennine Green（Vivimed Labs Ltd的市售产品）用作光致变色染料。染料的混合比为按重量计1:1。
表2显示了单个膜A和B以及在实施例1中通过膜1和2的共层叠（co-lamination）来获得的三层膜的褪色时间。表3显示了通过本发明的层叠件实现的褪色时间比的改善。实施例1的层叠件显示了与低温下的实施例3同样快速的褪色，并显示了与高温下的实施例2同样快速的褪色。此类层叠件可用于全年条件。

Claims (10)

1.由至少两个基于含有增塑剂的聚乙烯醇缩醛的单个膜组成的用于层叠玻璃的光致变色夹层膜，其特征在于所述单个膜包含至少一种光致变色化合物并具有相差至少5 K的玻璃化转变温度。
2.如权利要求1所述的光致变色夹层膜，其特征在于所述单个膜具有相差至少5重量%的增塑剂含量。
3.如权利要求1或权利要求2所述的光致变色夹层膜，其特征在于所述第二单个膜包含具有小于14重量%的聚乙烯醇基团部分的聚乙烯醇缩醛。
4.如权利要求1至3任一项所述的光致变色夹层膜，其特征在于所述第一单个膜包含具有17至22重量%的聚乙烯醇基团部分的聚乙烯醇缩醛。
5.如权利要求1至4任一项所述的光致变色夹层膜，其特征在于所述第二单个膜包含具有0.1至11摩尔%的聚乙酸乙烯酯基团部分的聚乙烯醇缩醛。
6.如权利要求1至5任一项所述的光致变色夹层膜，其特征在于所述第一单个膜包含具有5至8摩尔%的聚乙酸乙烯酯基团部分的聚乙烯醇缩醛。
7.如权利要求1至6任一项所述的光致变色夹层膜，其特征在于所述单个膜包含至少一种光致变色化合物，其选自三芳基甲烷类、芪类、氮杂芪类、硝酮类、俘精酸酐类、螺环吡喃类、萘并吡喃类、螺环-噁嗪类和醌类。
8.如权利要求1至7任一项所述的光致变色夹层膜，其特征在于所述夹层膜由至少三个单个膜组成，其中在所述夹层膜外侧上的两个单个膜具有与夹层膜内侧上的单个膜的玻璃化转变温度相差至少5 K的玻璃化转变温度。
9.如权利要求1至8任一项所述的光致变色夹层膜，其特征在于所述夹层膜通过单个膜的共挤出制得。
10.如权利要求1至9任一项所述的光致变色夹层膜在汽车行业中，在挡风玻璃中，在建筑行业中或在外立面元件模块中的用途。
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