CN110650995B - 抗水解聚酯膜 - Google Patents
抗水解聚酯膜 Download PDFInfo
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- CN110650995B CN110650995B CN201880030462.4A CN201880030462A CN110650995B CN 110650995 B CN110650995 B CN 110650995B CN 201880030462 A CN201880030462 A CN 201880030462A CN 110650995 B CN110650995 B CN 110650995B
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Abstract
通过有机涂层涂覆的二氧化钛颗粒用于提高取向聚酯膜的抗水解性的用途,特别地其中有机涂层不包含硅烷或不源自硅烷,并且特别地其中有机涂层选自有机磷化合物和聚合物有机涂层;取向聚酯膜,其包含通过有机涂层涂覆的这种二氧化钛颗粒;和包括这种膜的光伏电池。
Description
本发明涉及显示出改善的抗水解性的聚酯膜及其生产方法。
聚酯膜的有利的机械性能、尺寸稳定性和光学性能是众所周知的。然而,聚酯膜易于水解降解,这导致聚合物的特性粘度降低,并因此使膜的一种或多种上述期望的性能,特别是机械性能劣化。水解稳定性差自身还可以表现为膜的开裂。当膜暴露于潮湿条件和/或升高的温度,尤其是在延长的时间内长时间暴露时,例如在诸如光伏(PV)电池的外部应用中,抗水解性差特别有问题。
为了改善聚酯膜的抗水解性,已知将有机水解稳定剂掺入膜中。例如,尤其在US-5885709和EP-0838500中提出了在聚酯组合物中添加碳二亚胺作为封端剂,但这种添加剂具有散发出有害气体副产物的倾向。US-2003/0219614-A1报道了使用聚合碳二亚胺作为水解稳定剂减少了气体逸出的倾向。US-2002/0065346-A1教导了水解稳定剂选自酚类化合物、噁唑啉和/或单体或聚合碳二亚胺,任选地与有机亚磷酸酯组合。GB-1048068教导了使用有机羧酸的铜盐作为水解稳定剂。US-3657191和US-3869427教导了通过与碳酸亚乙酯或单官能缩水甘油醚反应来对聚酯的端基进行改性。在EP-0292251-A中还公开了通过使用含末端环氧基的化合物稳定的抗水解聚酯。在EP-1209200中,据报道缩水甘油酯和缩水甘油醚的组合在催化剂(其促进缩水甘油基和羧基之间的反应)的存在下改善了聚酯的抗水解性,尽管该公开内容涉及聚对苯二甲酸丁二醇酯(PBT),其结晶速度比PET快得多,以及其在制造注射成型材料中的用途。US-6498212公开了其中通过使用选自环氧乙烯-丙烯酸乙酯共聚物、环氧苯乙烯-丁二烯-苯乙烯嵌段共聚物和氨基聚乙烯共聚物的聚合物封端剂改善水解稳定性的聚酯。CA-2514589-A、US-4540729、US-5589126、US-7229697、US-7241507、US-2005/0137299-A1、US-2007/0238816-A1和US-2007/0237972-A1公开了在聚酯组合物中使用环氧化脂肪酸烷基酯(如环氧化硬脂酸2-乙基-己酯)和/或环氧化脂肪酸甘油酯(如环氧化大豆油或亚麻籽油)作为水解稳定剂。改善聚对苯二甲酸乙二醇酯(PET)膜的水解稳定性的其他方法包括同时控制参数如特性粘度、二乙二醇含量和结晶度,如EP-0738749-A中所公开。在EP-0620245-A中报道了结合抗氧化剂的存在来控制特性粘度和结晶度,以改善高温(180℃)老化特性,而不会损害用作电动机和电容器中的绝缘体材料的聚酯膜的面内分层性能。US-4115350和US-4130541教导了聚酯与单羧酸、酰胺和硫代酸的环氧化烷基酯的反应产物改善了由其制成的纤维和绳索中的聚酯的热稳定性。US-3372143教导了聚酯与环氧化烷氧基-或芳氧基-醚的反应产物改善了由其制备的纤维的染色性。WO-2011/030098-A和WO-2012/120260-A教导了在聚对苯二甲酸乙二醇酯(PET)膜中使用水解稳定剂,该水解稳定剂选自具有5至50个碳原子的支链单羧酸的缩水甘油酯,其中水解稳定剂以其与聚酯的至少一些端基的反应产物的形式存在于膜中。
与将有机水解稳定剂结合到聚酯膜中相关的问题之一是,虽然增加添加剂的浓度可以改善抗水解性,但是这样做的代价是降低熔点和/或特性粘度,并且聚酯膜的机械性能劣化,从而使膜可能变脆并且难以成膜。因此,机械性能降低的特别结果是成膜的聚酯的可加工性变差,并且在制造和随后的加工过程中发生膜网的破裂。
用有机水解稳定剂观察到的另一个问题是膜可能变色并显示出缺陷。对于基于环氧化脂肪酸甘油酯和多官能缩水甘油基化合物的水解稳定剂而言,这特别有问题。膜质量的这种降低本身是有问题的,并且还对加工性造成影响。这样的添加剂可能在聚酯膜中引起轮廓缺陷和不可接受的水平的模头线(die-line,模具划痕,压膜划痕),即整个膜网上的厚度均匀性差和/或光透射差,并且由于膜网的破裂,挤出物可能无法在膜线上加工。认为,这些问题至少部分归因于交联和凝胶形成,这干扰了膜在其制造过程中经历的拉伸过程。使用多官能缩水甘油基化合物作为聚酯的水解稳定剂的另一个问题是它们较高的聚酯链增长速率增加了熔体粘度,这进而降低了在给定温度下的挤出产量,这在经济上是不期望的。虽然理论上可以通过提高熔体温度降低粘度,但这将导致聚合物和水解稳定剂的降解速率增加,并导致凝胶形成。在其他聚酯产品(例如,注射成型PBT产品)的制造中,凝胶形成较小地成为问题,部分原因是与聚酯膜相比,那些产品的厚度要大得多。
基于环氧化脂肪酸,特别是环氧化脂肪酸甘油酯的有机水解稳定剂的另一个问题是,这样的添加剂在膜的制造和加工过程中具有分解的倾向,并且伴随着丙烯醛的形成,而丙烯醛是一种剧毒、易燃和恶臭的物质。
本发明的目的是提供替代的抗水解聚酯膜,特别地其中避免使用有机水解稳定剂,特别地其中可以在不形成有毒副产物的情况下制造和使用该膜,特别地在保持或改善膜制造的简易性、效率和经济性的同时而不增加膜破裂,特别地其中降低了模头线和轮廓缺陷的水平,并且特别地不损害膜的机械和/或光学性能。
本发明的其他目的是提供改善的抗水解聚酯膜,其不包含有机水解稳定剂或其在不存在有机水解稳定剂的情况下制造,即,其中相对于不含有机水解稳定剂或在不存在有机水解稳定剂的情况下制造的其他或常规的抗水解聚酯膜,其抗水解性提高,特别地在保持或改善膜制造的简易性、效率和经济性的同时而不增加膜破裂,特别地其中降低了模头线和轮廓缺陷的水平,并且特别地不损害膜的机械和/或光学性能。
根据本发明,提供了包含二氧化钛颗粒的取向聚酯膜(oriented polyesterfilm,取向的聚酯膜,定向聚酯膜),其中所述颗粒被有机涂层涂覆。
本发明人出乎意料地发现,通过所述有机涂层涂覆的二氧化钛颗粒赋予聚酯膜出乎意料的良好的抗水解性,并且优于通常用于聚酯膜中的常规二氧化钛颗粒。此外,在不存在通常添加到聚酯膜中的常规有机水解稳定剂的情况下,由所述有机涂层涂覆的二氧化钛颗粒可以为聚酯膜提供足够的抗水解性。
本文所述的取向聚酯膜是自支撑膜或片,其是指在没有支撑基底的情况下能够独立存在的膜或片。该膜优选是单轴或双轴取向的,优选是双轴取向的。
构成膜的一种或多种聚酯通常是一种或多种合成线性聚酯。合适的聚酯通过将一种或多种二羧酸或它们的低级烷基(至多达6个碳原子)二酯与一种或多种二醇缩合可获得。二羧酸组分包含至少一种芳族二羧酸,其优选为对苯二酸、间苯二酸、邻苯二酸、1,4-、2,5-、2,6-或2,7-萘二羧酸,并且优选为对苯二酸(TA)或2,6-萘二羧酸,且优选为对苯二酸。聚酯还可包含衍生自诸如下述的其他二羧酸的一个或多个残基:4,4'-二苯基二羧酸、六氢对苯二酸、1,10-癸烷二羧酸、包括通式CnH2n(COOH)2的那些的脂族二羧酸,其中n为2至8(例如,琥珀酸、戊二酸、癸二酸、己二酸、壬二酸、辛二酸或庚二酸,优选为癸二酸、己二酸和壬二酸,更优选为壬二酸)。二醇优选选自脂族和脂环族二醇,例如乙二醇(EG)、1,3-丙二醇、1,4-丁二醇和1,4-环己烷二甲醇(CHDM),并且优选选自乙二醇(EG)。成膜聚酯树脂是膜的主要成分,占给定层总重量的按重量计至少50%,优选为至少65%,通常为至少80%,更通常为至少85%,并且在一个实施方式中,通常为给定层的总重量的按重量计至少95%。
聚酯优选是可结晶的聚酯。优选地,聚酯仅包含一种二羧酸,优选为芳族二羧酸,优选为对苯二酸或2,6-萘二羧酸,且优选为对苯二酸。优选地,聚酯仅包含一种二醇,优选为脂族二醇,优选为乙二醇。优选地,聚酯包含一种芳族二羧酸和一种脂族二醇。聚对苯二甲酸乙二醇酯(PET)或聚2,6-萘二甲酸乙二醇酯(PEN),特别是PET,是基础层的优选聚酯。聚酯可任选地包含相对少量的一种或多种衍生自上述其他二羧酸和/或二醇的残基,并且如果存在这样的少量,则所述一种或多种其他二羧酸的总量优选小于给定层的聚酯的总二羧酸部分的10mol%,优选小于5mol%,优选小于1mol%和/或所述一种或多种其他二醇的总量优选小于给定层的聚酯的总二醇部分的15mol%,优选小于10mol%,优选小于5mol%。聚酯是给定层的主要组分,并且占层总重量的按重量计至少50%,优选占给定层的总重量的按重量计至少65%,优选至少80%,更优选至少85%,并且在一个实施方式中,通常为给定层的总重量的按重量计的至少95%。
膜的给定层源自其的聚酯的特性粘度优选为至少约0.60,优选至少约0.65,优选至少约0.70。优选地,聚酯的特性粘度不大于约0.80,通常不大于0.75。优选地,聚酯的特性粘度为至少0.61,优选为至少约0.62,优选为至少约0.63。具有相对高的特性粘度的聚酯的使用提供了改善的水解稳定性,尽管粘度太高可能导致膜制造困难和/或需要专门的、更稳健的成膜设备。例如,太大地增加粘度可能意味着它适合于降低产量(即,减少每单位时间挤出的聚酯的量,其导致较不经济的过程)或增加挤出温度以降低熔体的粘度(其反过来可能导致聚合物的热降解和相关性能的损失),从而实现稳定的膜生产。
通常,在至高达约295℃的温度下通过缩合或酯交换以已知方式方便地进行聚酯的形成。在一个优选的实施方式中,可以使用本领域公知的常规技术,例如使用流化床如氮气流化床或真空流化床,使用旋转真空干燥机,使用固态聚合将可结晶聚酯的特性粘度增加至所需值。在聚合物和膜制造的以下描述中,将理解,术语“聚酯”包括“共聚酯”。
本发明的聚酯膜的形成可以通过常规技术进行。挤出通常在约250至约300℃范围内的温度下进行,然后淬火挤出物并取向淬火的挤出物。优选地,聚酯在约270至约300℃、优选为约280至约300℃的温度下挤出。
本发明的多层膜可使用本领域常规技术制备,包括本领域公知的共挤出、层压和涂覆技术,且最优选地通过共挤出。一般而言,术语共挤出工艺包括以下步骤:将各自的聚酯组合物通过多孔模头的独立孔共挤出,然后将仍然熔融的层合并在一起,或者优选通过单通道共挤出将熔融的层合并在一起,其中相应聚酯的熔融流首先在通向模头歧管的通道内合并,然后在流线流动的条件下在不相互混合的情况下从模头孔口一起挤出,从而制备层压膜。
淬火的挤出物的取向可以通过本领域已知的用于生产取向膜的任何方法来进行,例如管状或平面膜方法。通过在膜的平面中在两个相互垂直的方向上进行拉伸来实现双轴取向,从而获得令人满意的机械和物理性能的组合。在管状方法中,同时双轴取向可以通过挤出热塑性聚酯管来实现,随后将其淬火,再加热,然后通过内部气压膨胀以引起横向取向,并以将引起纵向取向的速率抽出。在优选的平面膜方法中,将成膜聚酯通过狭缝式模头挤出,并在冷却的流延鼓上快速淬火以确保将聚酯淬火至无定形状态。然后,通过在高于聚酯的玻璃化转变温度的温度下沿至少一个方向拉伸淬火的挤出物来进行取向。顺序取向可通过首先沿一个方向,通常是纵向方向,即通过膜拉伸机的向前方向,然后沿横向方向,将扁平的、淬火的挤出物拉伸来实现。挤出物的向前拉伸可方便地在一组旋转辊上或在两对轧辊之间进行,然后在拉幅机设备中进行横向拉伸。通常进行拉伸,使得取向膜的尺寸在拉伸方向或每个拉伸方向上是其原始尺寸的2至5倍,更优选2.5至4.5倍。通常,拉伸在高于聚酯的Tg的温度下进行,优选地比Tg高约15℃。如果仅需要在一个方向上取向,则可以使用更大的拉伸比(例如,至高达约8倍)。不需要在机器和横向上均等地拉伸,尽管如果需要平衡的特性,这是优选的。
可以并且优选通过在尺寸支撑下在高于聚酯的玻璃化转变温度但低于其熔化温度的温度下通过热定形在尺寸上稳定拉伸的膜,以引起聚酯的期望结晶。在热定形期间,可以通过称为“内倾(toe-in)”的过程在横向方向(TD)上进行少量的尺寸松弛。内倾可涉及约2至4%的尺寸收缩,但是由于要求低的线张力并且膜控制和卷绕成为问题,因此难以实现在工艺或机器方向(MD)上的类似尺寸松弛。实际的热定形温度和时间将根据膜的组成及其期望的最终热收缩率而变化,但不应选择以实质上降低膜的韧性性能如抗撕裂性。在这些限制内,通常期望约180至245℃的热定形温度。在一个实施方式中,热定形温度在约200至约225℃的范围内,这提供了水解稳定性的有利改进。在热定形之后,通常将膜快速淬火,以引起聚酯的期望结晶度。
膜可通过使用在线松弛阶段进一步稳定。可替代地,松弛处理可以离线进行。在该附加步骤中,以低于热定形阶段的温度加热膜,并且具有大大降低的MD和TD张力。膜所经受的张力是低张力,并且通常小于5kg/m,优选小于3.5kg/m,更优选在膜宽度的1至约2.5kg/m的范围内,并且通常在膜宽度的1.5至2kg/m的范围内。对于控制膜速度的松弛过程,膜速度的降低(因此应变松弛)通常在0至2.5%、优选0.5至2.0%的范围内。在热稳定步骤中膜的横向尺寸没有增加。用于热稳定步骤的温度可以根据来自最终膜的期望性质的组合而变化,其中较高的温度给出更好的,即较低的残余收缩性质。通常期望温度为135至250℃,优选为150至230℃,更优选为170至200℃。加热的持续时间将取决于所使用的温度,但是通常在10至40秒的范围内,20至30秒的持续时间是优选的。可以通过多种方法来进行该热稳定过程,包括平面和垂直构造以及作为单独的处理步骤的“离线”或作为膜制造过程的连续的“在线”。与没有这种后热定形松弛的情况产生的膜相比,这样加工的膜将表现出较小的热收缩率。
本发明的聚酯膜优选包含以膜的总重量计为约1wt%至约40wt%、优选约1wt%至约20wt%、优选约5wt%至约20wt%、或约10wt%至约20wt%的所述通过有机涂层涂覆的二氧化钛颗粒。
在一个优选的实施方式中,聚酯膜是包括第一聚酯层(A)和第二聚酯层(B)的多层膜。第一层(A)和第二层(B)的每种聚酯均独立地选自上述聚酯。优选地,所述第二层(B)的聚酯是或包括与所述第一层(A)的聚酯相同的聚酯。在本文所述的PV电池(特别是其背板)的优选用途中,第一聚酯层(A)优选作为PV电池中最外层的层。
在该多层膜实施方式中,优选地至少第一聚酯层(A)包含所述通过有机涂层涂覆的二氧化钛颗粒,并且优选地,所述第二聚酯层(B)还包含所述通过有机涂层涂覆的二氧化钛颗粒。聚酯层(A)优选包含以层的总重量计为约1wt%至约40wt%、优选约1wt%至约20wt%、优选约10wt%至约20wt%的所述通过有机涂层涂覆的二氧化钛颗粒。优选地,所述第二层(B)包括以层的总重量计优选为约1wt%至约10wt%、优选为约1wt%至约5wt%的量的所述通过有机涂层涂覆的二氧化钛颗粒。优选地,在层(A)中所述通过有机涂层涂覆的二氧化钛颗粒的量大于在层(B)中通过有机涂层涂覆的二氧化钛颗粒的量。
在该多层膜实施方式中,优选地,所述第二层(B)包括源自所述多层膜的制造的再生废膜(reclaimed waste film,回收废膜)。
在该多层膜实施方式中,优选地,层(A)的厚度小于层(B)的厚度,优选地其中层(A)的厚度为层(B)的厚度的约10%至约40%,优选为约20%至约30%。
在本发明的聚酯膜包含单个聚酯层(特别是单个含二氧化钛的层)时,膜优选包含以膜的总重量计为约1wt%至约40wt%、优选约1wt%至约20wt%、优选约5wt%至约20wt%、并且优选约10wt%至约20wt%的所述通过有机涂层涂覆的二氧化钛颗粒。
本文所述的聚酯膜优选具有约12μm至约500μm、优选约12至约350μm、优选约12至约250μm、优选约20至约100μm的总膜厚度。
在本文所述的聚酯膜中,二氧化钛优选为金红石晶型。
有机涂层优选均匀地涂覆在所述二氧化钛颗粒上。有机涂层优选离散地涂覆在所述二氧化钛颗粒上。因此,涂覆二氧化钛颗粒的有机材料合适地是成膜有机材料。
优选地,有机涂层不包含硅烷或不源自硅烷。
有机涂层不是,并且优选地不包含聚硅氧烷。
在第一优选实施方式中(本文称为实施方式A),有机涂层是有机磷化合物。
优选地,二氧化钛颗粒涂覆有烷基膦酸或烷基膦酸的酯,其中烷基膦酸含有6至22个碳原子。
烷基膦酸或其酯优选由式P(R)(=O)(OR1)(OR2)表示,其中:
R为含有6至22个碳原子的烷基或环烷基;并且
R1和R2各自为氢、烷基、环烷基、芳基或芳烷基。
当R1和R2都是氢时,该化合物是烷基膦酸。当R1和R2中的至少一个是烃基时,该式代表烷基膦酸的酯。
优选地,R包含6至14个碳原子。
优选地,R是直链烷基。然而,支链烷基膦酸及其酯也是合适的。
在酯的情况下,R1和R2优选独立地选自烷基、环烷基、芳基或芳烷基,包含至多达10个碳原子,更优选至多达8个碳原子(即,酯是含至多达10个,且优选至多达8个碳原子的醇的酯)。R1和R2优选为烃基。在R1和R2为芳基或芳烷基的情况下,芳基优选为苯基。
R1和R2可以不同,但通常相同。优选地,R1和R2为氢。
特别合适的酯包括乙酯、丁酯、辛酯、环己酯和苯酯。
特别优选的磷化合物包括正辛基膦酸及其酯、正癸基膦酸及其酯、2-乙基己基膦酸及其酯、以及莰基膦酸(camphyl phosphonic acid,龙脑基膦酸)及其酯。
可以使用EP-0707051-A中教导的方法来制备根据实施方式A的涂覆的颗粒,其制造方法通过引用并入本文。
在其他优选的实施方式中(本文称为实施方式B),有机涂层是聚合物有机涂层。
聚合物有机涂层的聚合物主链优选不包含硅原子。
聚合物有机涂层优选源自包含碳、氢和氧原子,并且任选地进一步包含氮和/或磷和/或硫原子的单体。因此,应当理解,聚合物有机涂层优选源自不含硅原子的单体。
涂覆的二氧化钛颗粒(通过聚合物有机涂层涂覆)优选通过下述获得:在包含聚合多元酸或其盐的分散剂的存在下在高于所述二氧化钛颗粒的等电点的pH值下(并且优选地在高于7的pH下,并且优选在9至11的pH下),将二氧化钛颗粒分散在水中以产生具有改变的等电点的颗粒;将分散体的pH调节至低于9但高于颗粒的改变的等电点的值;和在如此产生的分散体的存在下聚合一种或多种烯键式(ethylenically,烯属)不饱和单体,使得所述二氧化钛颗粒被聚合的单体涂覆。优选地,根据EP-0572128-A的公开内容制造颗粒,其公开内容并入本文,并且特别地涂覆颗粒的制造方法的公开内容并入本文。
不受理论的束缚,认为涂覆的二氧化钛颗粒包含由分散剂形成的连贯(coherent)内涂层和由一种或多种烯键式不饱和单体的聚合形成的外涂层和/或在一种或多种烯键式不饱和单体的聚合过程中将分散剂结合在聚合物涂层中。
聚合多元酸优选选自聚磺酸、聚膦酸和聚羧酸或其盐,并且优选选自聚羧酸或其盐。当聚合多元酸为盐形式时,酸可以被部分或完全中和。合适的盐是碱金属盐或铵盐。
合适的聚磺酸优选选自木质素磺酸盐(lignosulphonate,木质素磺酸)、石油磺酸盐(petroleum sulphonate,石油磺酸)和聚(苯乙烯磺酸盐)(poly(styrene sulphonate),聚(苯乙烯磺酸)),包括聚(4-苯乙烯磺酸钠)。
合适的聚羧酸优选选自聚马来酸、聚丙烯酸、取代的丙烯酸聚合物、丙烯酸共聚物,包括丙烯酸与磺酸衍生物的共聚物,磺酸衍生物包括2-丙烯酰胺基-2-甲基丙磺酸(2-acrylamido and 2-methyl propane sulphonic acid,2-丙烯酰胺基及2-甲基丙磺酸)。与丙烯酸或取代的丙烯酸可聚合的其他共聚单体可包含羧基。
优选地,分散剂表现出约1,000至约10,000的分子量(MW)。优选地,分散剂是基本上线性的分子。分子量测定可以在配备两个GPC Ultrastyragel柱,103和(5μm混合型,300mm x 19mm,Waters Millipore Corporation,Milford,MA,USA)和THF作为流动相的Hewlett-Packard 1050系列HPLC系统上进行。通过与聚苯乙烯标准的保留时间比较来计算分子量。
优选地,分散剂的量以二氧化钛颗粒(即,在用分散剂和一种或多种可聚合涂覆单体处理之前的核,未涂覆的二氧化钛颗粒)的重量计为约0.05至约5.0wt%,优选为约0.1至约1.0wt%。
优选地,聚合物有机涂层包含衍生自一种或多种烯键式不饱和单体的聚合物。换句话说,聚合物有机涂层包含衍生自一种或多种烯键式不饱和单体的聚合的聚合物。
一种或多种烯键式不饱和单体优选在水性溶剂中可聚合,优选地其中所产生的聚合物不溶于水并且任选地通过交联剂交联。
一种或多种烯键式不饱和单体优选选自含有可聚合不饱和基团的脂族和芳族化合物,优选地其中可聚合不饱和基团选自不饱和羧酸和不饱和羧酸酯。
一种或多种烯键式不饱和单体优选是酸性单体和所述酸性单体的酯,所述酸性单体选自丙烯酸、甲基丙烯酸、衣康酸、马来酸或其酸酐、富马酸和巴豆酸,所述酸性单体的酯包括丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸甲酯、丙烯酸丁酯和甲基丙烯酸乙酯。烯键式不饱和单体还可以选自苯乙烯、乙烯基甲苯、α甲基苯乙烯、乙烯、乙酸乙烯酯、氯乙烯、丙烯腈和氟化单体,包括氟化烯烃、氟化醚、氟化丙烯酸和甲基丙烯酸及其酯和氟化杂环化合物。优选地,一种或多种烯键式不饱和单体选自不饱和羧酸和不饱和羧酸酯,优选选自丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、甲基丙烯酸丁酯、乙酸乙烯酯和乙烯基异丁醚。
可以优选借助于一种或多种交联剂的存在来使聚合物有机涂层交联,优选地其中交联剂选自双官能和多官能的烯键式不饱和单体,优选地选自乙二醇二甲基丙烯酸酯、乙二醇二丙烯酸酯、甲基丙烯酸烯丙酯、丙烯酸烯丙酯、1,3-丁二醇二丙烯酸酯、二乙烯基苯和1,3-丁二醇二甲基丙烯酸酯,优选地其中基于一种或多种烯键式不饱和单体的总重量,所述交联剂的量为约1wt%至约20wt%,优选为约1wt%至约10wt%。
优选地,有机涂层选自上文针对实施方式A所述的有机涂层。
有机涂层优选以二氧化钛的重量计为约0.1至约200wt%、优选约0.1至约100wt%、约0.5至约100wt%、约2.0至约20wt%的量存在。优选地,二氧化钛颗粒与有机涂层的体积比为以体积计从1:1至1:25,并且优选为1:2至1:8。
二氧化钛优选具有使得它在290℃下表现出不大于1.0%、优选不大于0.5%的损失的水含量。
有机涂覆的二氧化钛优选不是疏水性的。优选地,有机涂覆的二氧化钛涂层是亲水性的。
二氧化钛颗粒优选还带有无机涂层,特别地为二氧化硅和/或氧化铝涂层,优选为氧化铝涂层,其中在将无机涂层施加到下面的二氧化钛核上之后,施加有机涂层。
涂覆的二氧化钛颗粒优选表现出这样的粒度,使得其体积分布中值粒径(相当于所有颗粒的体积的50%的等效球形直径,在累积分布曲线上读取,该体积%与颗粒的直径相关-通常称为“D(v,0.5)”值)的范围优选为0.01至5.0μm,更优选为0.05至1.0μm,更优选为0.05至0.40μm,优选为0.10至0.25μm,优选为0.15至0.25μm。优选地,按体积计为至少90%,更优选按体积计为至少95%的颗粒在体积分布中值粒径±0.8μm,特别是±0.5μm的范围内。可以通过电子显微镜、库尔特计数器、沉降分析和静态或动态光散射来测量颗粒的粒度。基于激光衍射(夫琅和费衍射)的技术是优选的。一种特别优选的方法利用从Malvern可获得的Mastersizer(例如3000)。中值粒度可以通过绘制代表低于所选粒度的颗粒体积百分比的累积分布曲线和测量第50百分位数来确定。
该膜可以进一步包含在聚酯膜的制造中常规使用的其他添加剂。因此,可以适当地掺入添加剂如交联剂、染料、颜料、空洞剂、润滑剂、抗氧化剂、自由基清除剂、热稳定剂、阻燃剂和抑制剂、防粘连剂、表面活性剂、滑动助剂、光泽改进剂、促降解剂(prodegradent)、粘度改进剂和分散稳定剂。可以常规方式将这样的组分引入聚合物中。例如,通过与成膜聚合物衍生自其的单体反应物混合,或者可以通过翻滚或干混或通过在挤出机中混合而将组分与聚合物混合,然后冷却,通常将其粉碎成颗粒或碎屑。也可以采用如上所述的母料技术。
然而,优选的是,膜不包含有机水解稳定剂。
还优选的是,膜不包含有机紫外线吸收剂,例如二苯甲酮、苯并三唑、苯并噁嗪酮或三嗪。
聚酯膜的特性粘度优选为至少约0.60、优选至少约0.61、优选至少约0.62、优选至少约0.63、优选至少约0.64、优选至少约0.65,并且典型地在约0.60至约0.70的范围内。使用具有相对高的特性粘度的聚酯膜提供改善的水解稳定性。
如下所述,通过测量膜的拉伸强度(脆性),特别是通过测量膜的断裂伸长率(ETB),来评价膜的抗水解性。未老化的膜通常显示出超过100%的ETB值。通常,直到将其ETB降低到小于10%的时间,膜在其最终用途中仍然有用。本发明的优选膜表现出抗水解性,使得在121℃和100%相对湿度下加速老化至少80小时,优选至少84小时,且优选至少90小时后,ETB为至少10%,优选至少20%,优选至少30%。
在一个实施方式中,聚酯膜的聚酯在(A)℃的温度下显示出吸热高温峰,并且在(B)℃的温度下显示出吸热低温峰,这两个峰均通过差示扫描量热法(DSC)测量,其中(A-B)的值在15℃至50℃的范围内,优选地在15℃至45℃的范围内,更优选地在15℃至40℃的范围内,并且在一个实施方式中在20℃至40℃的范围内,并且可以通过使用上述优选温度控制热定形温度来实现该特性。显示在本文公开的范围内的(A-B)值的优点是获得水解稳定性的有利改进。
本发明的聚酯膜优选在150℃下在30分钟内表现出低收缩率,优选小于3%,优选小于2%,优选小于1.5%,优选小于1.0%,特别是在膜的机器(纵向尺寸)中。优选地,在膜的两个尺寸(即,纵向和横向尺寸)中都显示出这样的低收缩率值。
在一个优选的实施方式中,该膜是不透明的,并且这种膜特别用作PV电池中的背板。不透明膜优选表现出以下透射光密度(TOD):至少0.4,优选至少0.5,优选至少0.6,优选至少0.7,优选至少1.0,且优选至少1.5,并且在一个实施方式中优选至少2.0,优选至少3.0,并且优选至少4.0。如本领域常规的,不透明度通常由一种或多种合适的遮光剂和/或增白剂提供。上文所述的涂覆的二氧化钛颗粒可以并且优选地确实用作遮光剂和/或增白剂。然而,任选地,膜可以进一步包含一种或多种另外的遮光剂和/或增白剂。不透明膜可根据需要着色。例如,本发明的膜可以是白色、灰色或黑色。
在一个优选的实施方式中,膜是白色的,这可以通过在其中掺入有效量的增白剂来实现。上文所述的涂覆的二氧化钛颗粒可以并且优选地确实用作增白剂。然而,任选地,膜可以进一步包含一种或多种另外的增白剂。另外合适的增白剂包括选自例如,金属或类金属氧化物如氧化铝、滑石和二氧化硅(特别是沉淀或硅藻土二氧化硅和硅胶)、煅烧的瓷土和碱金属盐如钙和钡的碳酸盐和硫酸盐的颗粒状无机填料。其他合适的另外增白剂包括不相容的树脂填料。可以使用这些填料的混合物。优选的另外的增白剂是颗粒状无机填料,优选为硫酸钡。掺入膜(或其层)中的增白剂的总量基于膜(或其层)中的聚酯的重量优选范围为按重量计约1%至约40%,通常为约5%至约30%,更通常为约8%至约25%。如本文所述,白色膜优选表现出如在本文所述测量的约80至约120单位范围内的白度指数。白色膜通常表现出的TOD范围为0.4至1.75,优选为至少0.5,优选为至少0.6,优选为至少0.7。
在一个替代实施方式中,膜是灰色或黑色的,通常表现出TOD为至少2.0,更通常为至少3.0,更通常为至少4.0,并且如本领域中常规的那样,这可以通过在其中掺入有效量的遮光剂如炭黑或金属填料如铝粉来实现。炭黑是优选的遮光剂。通常,这样的膜包含基于聚酯的重量为按重量计约0.3%至约10%、优选为0.5%至7%、特别地为1%至5%、且尤其为2%至4%的遮光剂。遮光剂可以存在于多层膜的多于一层或每一层中,或仅存在于其一层中。遮光剂合适地具有在0.01至1.5μm,特别地为0.02至0.05μm的范围内的粒径(如上所述定义和测量的)。
本发明的聚酯膜表现出高水平的膜均匀性和质量,以及优异的抗水解降解性。特别地,本发明的膜具有低水平的轮廓缺陷和/或模头线,均匀的厚度和透光性,以及优异的加工性,而膜网中没有缺陷或破裂。
本发明的膜特别适合用于光伏(PV)电池。如上所述,光伏电池是典型地包括前板(或前片)、前面密封材料、电极和光伏活性层(其中,光活性材料通常被支撑在电极支撑基板上)、背面密封剂、和背板(或背片)的多层组件。典型的PV电池还包括收集和管理电荷的各种组件。在PV电池的各种层的制造中已经提出了聚酯膜,例如前板、背板和一个或多个电极支撑层。通常由许多光伏电池组成的光伏模块通常根据所用的活性光伏材料进行分类。这些包括晶体硅、砷化镓(GaAs)、无定形硅(a-Si)、碲化镉(CdTe)、铜-铟-镓-(二)硒化物(CIGS)、染料敏化或有机电池。包含砷化镓、无定形硅、碲化镉、铜-铟-镓-(二)硒化物、染料敏化或导电有机材料的光伏电池通常称为薄膜光伏电池(TFPV电池),其可能是或可能不是柔性的。染料敏化的光伏电池特别受关注,其中活性光吸收层包含通过吸收入射光而激发的染料。其他薄膜硅PV电池包括原生结晶、纳米晶体(nc-Si或nc-Si:H)和黑硅PV电池。薄膜光伏电池是通过使用各种沉积方法和各种基板在基板上沉积一层或多层光伏材料薄层而制成的,该薄层的厚度范围从1纳米或2纳米变化到数十微米。密封材料是阻挡材料,其保护光活性层和电极层并提供对气体和溶剂渗透的高抗力。密封阻挡材料通常以自支撑膜或片的形式使用,如本领域中常规的那样,通常在真空下使用层压技术将其施加到包含光活性层和电极层的复合材料上。然后,将密封的复合材料夹在前板和背板之间。PV电池中使用的密封材料包括乙烯乙酸乙烯酯(EVA)共聚物树脂,通常其中乙酸乙烯酯组分在下述范围内:约10至约35wt%,优选为约15至约35wt%,优选为约20至约35wt%,优选为约25至约35wt%,并且优选为约28至约33wt%。合适的EVA密封材料包括可商购的树脂(DuPont,包括等级PV1410至PV1650Z)。其他密封材料包括基于离聚物的材料,即主要由非极性重复单元和少量(通常不超过约15wt%)含盐单元组成的聚合物。典型的离聚物包括热塑性羧酸盐离聚物,其中非极性共聚单体选自乙烯和苯乙烯(优选为乙烯),并且含有少量的含盐单元,例如甲基丙烯酸和/或丙烯酸的金属盐(例如,碱金属或锌盐)。示例性的离聚物密封材料是被碱金属或锌部分或完全中和的乙烯和甲基丙烯酸和/或丙烯酸的共聚物,例如(DuPont;例如等级1702)。其他密封材料包括聚乙烯醇缩丁醛树脂,也从DuPont可购买(例如PV5200系列)和硅酮树脂(例如Dow Corning的PV-6100系列光学透明硅酮密封剂)。其他密封材料包括聚烯烃,例如乙烯的均聚物和共聚物,例如与丙烯酸类和/或甲基丙烯酸类如甲基丙烯酸和/或丙烯酸的共聚物。
本发明的膜特别适合作为PV电池的背板或作为PV电池的背板中存在的层(特别是最外层)。PV电池的背板应显示出良好的抗水解性。背板应优选表现出良好的热尺寸稳定性。尺寸稳定性差可导致相邻的密封材料开裂,尤其是在设备制造过程中经历的升高的温度(通常还有低压)期间。背板优选还应表现出良好的紫外线稳定性。缺乏紫外线稳定性会在暴露于阳光下时自身表现为膜黄变、雾化和开裂,从而降低光伏电池的有效使用寿命。
本发明的膜还适用于其中水解稳定性至关重要的任何环境中,例如在潮湿条件下在升高的温度下延长的时间,以及在外部应用中。如本文所用,术语“在升高的温度下在潮湿条件下的长时间”是指膜在使用过程中经历的环境条件,例如作为PV电池,并且优选地通过使用本文所述的压力锅测试的加速老化测试来测量的(在至少80小时,优选至少84小时,且优选至少90小时的时间内在121℃和100%相对湿度下)。
本发明的膜还可用于电子或光电器件的制造,例如电致发光(EL)显示器件(特别是有机发光显示(OLED)器件)、电泳显示器(电子纸)和半导体器件(例如,通常是有机场效应晶体管、薄膜晶体管和集成电路)。
本文公开的作为PV电池和其他电子设备中的一个或多个层的聚酯膜允许以卷到卷工艺制造这种设备,从而降低成本。
根据本发明的其他方面,提供了通过如本文所述的有机涂层涂覆的二氧化钛颗粒用于提高取向聚酯膜的抗水解性的用途,其中所述有机涂层不包含或不源自硅烷。
根据本发明的其他方面,提供了一种制造取向聚酯膜的方法,该方法包括以下步骤:
(i)挤出熔融聚酯的层;
(ii)将挤出物淬火;
(iii)在一个方向或两个相互垂直的方向上拉伸淬火的挤出物;和
(iv)将膜热定形,
其特征在于,在将聚酯形成为膜之前,以一定量将通过有机涂层涂覆的二氧化钛颗粒掺入到聚酯中,所述量相对于其中二氧化钛颗粒未被所述有机涂层涂覆的聚酯膜有效地提高所述聚酯膜的抗水解性,其中所述有机涂层不包含硅烷或不衍生自硅烷。
优选地,抗水解性的提高使得取向聚酯膜的ETB在121℃和100%相对湿度下加速老化至少80小时,优选至少84小时,且优选至少90小时后,为至少10%,优选至少20%,优选至少30%。
根据本发明的其他方面,提供了如本文所述的取向聚酯膜作为光伏电池中的层的用途,所述光伏电池优选地包括前板、一个或多个电极层、光伏活性层和背板,特别是其中所述背板包括所述取向聚酯膜。因此,根据本发明的其他方面,提供了如本文所定义的膜作为PV电池中的背板或PV电池中的背板中存在的层的用途。
根据本发明的其他方面,提供了一种光伏电池,其包括前板、一个或多个电极层、一个或多个光伏活性层和背板,其中前板和/或背板包括如本文定义的取向聚酯膜,特别地其中背板是或包括如本文定义的取向聚酯膜。在所述光伏电池中,将一个或多个电极层和一个或多个光伏活性层适当地包覆(coated,涂覆)在密封件(encapsulant,密封体,密封剂)中。
本文所述的取向聚酯膜优选是这种光伏电池中的最外层。优选地,在这种光伏电池中的取向聚酯膜是不透明的或白色膜。
性能测量
以下分析用于表征本文所述的膜:
(i)透射光密度(TOD)是使用Macbeth密度计TR 927(从Dent and Woods Ltd,Basingstoke,UK获得)以透射模式测量的。
(ii)白度指数是使用Colorgard系统2000,型号/45(由Pacific Scientific制造的)和ASTM D 313的原理测量的。
(iii)聚酯和聚酯膜的特性粘度(以dL/g为单位)是根据ASTM D5225-98(2003)在ViscotekTM Y-501C相对粘度计(参见例如,Hitchcock,Hammons&Yau在美国实验室(inAmerican Laboratory)(1994年8月)“现代粘度测定的双毛细管方法”)上通过在25℃下使用按重量计0.5%的聚酯在邻氯苯酚中的溶液并使用Billmeyer单点方法通过溶液粘度测定法测量的以计算特性粘度:
η=0.25ηred+0.75(lnηrel)/c
其中:
η=特性粘度(单位为dL/g),
ηrel=相对粘度,
c=浓度(单位为g/dL),且
ηred=降低的粘度(单位为dL/g),其等于(ηrel-1)/c(也表示为ηsp/c,其中ηsp是比粘度)。
(iv)抗水解性可以通过在121℃和100%相对湿度下对膜进行至多达100小时的处理(“压力锅测试”(PHT))来评估。将样品放在设置在上述温度和湿度的SMEG AVS 23L压力锅中固定的时间。在分析之前,使样品在室温和湿度下干燥24小时。然后,可以在不同的时间间隔测量与聚合物老化有关的性质。特别地,如下所述测量断裂伸长率(ETB)。
(v)断裂伸长率根据测试方法ASTM D882测量。使用直边和经过校准的样品切割器(10mm+\-0.5mm)沿机器方向切割膜的五个条带(长度为100mm)。每个样品均使用Instron3111型材料测试机进行测试,并使用带有橡胶颌面的气动夹具。控制温度(23℃)和相对湿度(50%)。十字头速度(分离速度)为25mm.min-1。应变率为50%。通过将分离率除以夹具之间的初始距离(样品长度)来计算。设备记录每个样品的断裂伸长率。断裂伸长率定义为:
其中L0是样品在夹具之间的初始长度。
(vi)聚酯膜的耐候性根据ISO 4892-2进行测试。
(Vii)评估尺寸为200mm x 10mm的膜样品的热收缩率,其在相对于膜的机器方向和横向的特定方向上切割,并标记了目测的测量值。样品的较长尺寸(即,200mm尺寸)对应于要测试收缩率的膜方向,即,为了评估机器方向的收缩率,测试样品的200mm尺寸沿膜的机器方向取向。将样品加热到150℃的预定温度(通过放置在该温度下的加热炉中)并保持30分钟的时间间隔后,将其冷却至室温,并手动重新测量其尺寸。计算热收缩率,并表示为初始长度的百分比。
(viii)使用Perkin Elmer DSC 7仪器获得差示扫描量热仪(DSC)扫描。将称重5mg的聚酯膜样品密封到标准的Perkin Elmer铝制DSC坩埚中。将膜和坩埚压平,以确保膜被部分约束,以使加热过程中取向松弛的影响最小。将样品放置在仪器的样品架中,以每分钟80℃的速度从30加热到300℃,以记录相关迹线。使用干燥的惰性吹扫气体(氮气)。DSC仪器的温度和热流轴已针对实验条件(即,加热速率和气体流速)进行了全面校准。峰值温度的值,即吸热高温峰(A)和吸热低温峰(B),被认为是从每次吸热熔化过程开始到每次吸热熔化过程结束所绘制的基线以上的最大位移。峰值温度测量值是使用Perkin Elmer软件中的标准分析程序得出的。测量的精度与准度为±2℃。
(ix)二氧化钛的水含量通过卡尔费歇尔滴定法,优选库仑卡尔费歇尔滴定法测量。通常,将样品在滴定池上游的烘箱中加热,释放的水通过干燥载气的流转移到滴定池,在此处通过卡尔费歇尔滴定法测定。适当地,将Metrohm 768KF库仑计与Metrohm 768KF烘箱联接用于进行库仑卡尔费歇尔滴定。
参考以下实施例进一步说明本发明。实施例不旨在限制如上所述的本发明的范围。
实施例
实施例1
通过将涂覆有氧化铝层和上文定义的有机涂层的二氧化钛(TR28;平均粒度为0.21μm)掺入到聚对苯二甲酸乙二醇酯(PET;IV为0.61)中来制备母料。基于组合物的总重量,母料的TiO2含量为40wt%。
制备两层共挤出膜,其中层(A)衍生自TiO2母料和聚对苯二甲酸乙二醇酯以提供以层(A)的总重量计为约14wt%的TiO2浓度。在传统的膜生产线上,在双螺杆挤出机的料斗中将母料与PET混合(通过真空除去水分)。层(B)为聚对苯二甲酸乙二醇酯和40%再生。
使用标准的熔融共挤出系统将两层膜挤出并浇铸。使用两个独立运行的挤出机组装共挤出系统,其分别将聚合物熔体的进料供给到标准共挤出模块或连接这些料流的接点。从共挤出模块将熔体流输送到常规的平膜挤出模头,其允许在285℃下从普通共挤出模头浇铸熔体帘幕,然后在温度中淬火到旋转的冷却金属鼓上。以约17.8m/min的处理速度收集流延膜,并且其宽度为约2135mm。将流延挤出物在86.5℃的温度下沿挤出方向拉伸至其初始尺寸的约3倍。然后将冷却的拉伸膜送入温度为102℃的拉幅机中,在此将膜干燥并沿侧向拉伸至其初始尺寸的约3.97倍。横向拉伸温度为125℃。将双轴拉伸膜在215至220℃范围内的温度下热定形。
所得白色膜的最终厚度为50μm,层(A)为约10μm,且层(B)为约40μm。
实施例2(比较)
实施例2对应于实施例1,不同之处在于二氧化钛是不包含本文所述的有机涂层的氧化铝涂覆的金红石TiO2(来自Tayca Corporation的JR301;平均粒度为0.30μm)。
实施例3(比较)
使用不包含本文所述的有机涂层的另一等级的氧化铝涂覆的TiO2重复实施例1。
然后,如本文所定义,通过测量加速老化前后的断裂伸长率来评估每个膜的抗水解性,结果在图1中示出(其中x轴为时间(小时),且y轴为ETB(%))。与其中二氧化钛未涂覆本文所述的有机涂层的类似膜相比,实施例1的膜表现出令人惊讶的优异的抗水解性。
实施例4、5、6和7
制备一系列50μm的单层PET膜,它们具有各种等级的涂覆TiO2以及不含TiO2,如下:
实施例4:没有TiO2(对照)
实施例5:TR28(本发明)
实施例6:Ti-R104(DuPont;硅烷化氧化铝涂覆的金红石TiO2;比较)
实施例7:Ti-R960(DuPont;没有有机涂层的氧化铝和二氧化硅涂覆的金红石TiO2;比较)
用在PET中的60%的TiO2制备含有每种TiO2等级的母料。膜实施例5、6和7通过在常规膜生产线上在双螺杆挤出机的料斗(通过真空除去水分)中将母料与PET基础聚合物混合以在最终膜中提供约10.5wt%的TiO2制成。
经由10%的母料添加SiO2以在最终膜中提供2.3wt%的SiO2。将液体水解稳定剂(E10P;叔碳酸的缩水甘油酯;Hexion Speciality Chemicals)以每千克聚合物和其无机添加剂约8ml计量加入挤出机中。预期将TiO2添加到含水解稳定剂的膜中会降低该膜的水解稳定性。
然后,通过测量加速老化前后的断裂伸长率来测试膜,如本文所定义,结果在图2中示出(其中x轴为时间(小时),且y轴为ETB(%))。与实施例6和7(其中二氧化钛没有被本发明所定义的有机涂层涂覆)的膜相比,实施例5的膜表现出令人惊讶的优异的抗水解性。
Claims (52)
1.通过有机涂层涂覆的二氧化钛颗粒用于提高取向聚酯膜的抗水解性的用途,其中,所述有机涂层不包含硅烷或不源自硅烷,并且其中所述有机涂层是烷基膦酸或烷基膦酸的酯,其中,所述烷基膦酸含有6至22个碳原子。
2. 根据权利要求1所述的用途,其中,所述膜包含按所述膜的总重量计从1 wt%至40wt%的通过所述有机涂层涂覆的所述二氧化钛颗粒。
3. 根据权利要求1所述的用途,其中,所述膜包含按所述膜的总重量计从1 wt%至20wt%的通过所述有机涂层涂覆的所述二氧化钛颗粒。
4. 根据权利要求1所述的用途,其中,所述膜包含按所述膜的总重量计从10 wt%至20wt%的通过所述有机涂层涂覆的所述二氧化钛颗粒。
5.根据权利要求1所述的用途,其中,所述聚酯膜是还包括第二层(B)的多层膜中的层(A)。
6.根据权利要求5所述的用途,其中,所述第二层(B)是聚酯膜层。
7.根据权利要求5所述的用途,其中,所述聚酯膜的特性粘度为至少0.60。
8.根据权利要求5所述的用途,其中,所述聚酯膜的特性粘度为至少0.64。
9.根据权利要求6所述的用途,其中,所述第二层(B)的聚酯是或包含与所述层(A)的聚酯相同的聚酯。
10. 根据权利要求6所述的用途,其中,聚酯层(A)包含按所述层的总重量计从1 wt%至40 wt%的通过所述有机涂层涂覆的所述二氧化钛颗粒。
11. 根据权利要求6所述的用途,其中,所述聚酯层(A)包含按所述层的总重量计从1wt%至20 wt%的通过所述有机涂层涂覆的所述二氧化钛颗粒。
12. 根据权利要求6所述的用途,其中,所述聚酯层(A)包含按所述层的总重量计从10wt%至20 wt%的通过所述有机涂层涂覆的所述二氧化钛颗粒。
13. 根据权利要求6所述的用途,其中,所述第二层(B)包含按所述层的总重量计从1wt%至10 wt%的量的通过所述有机涂层涂覆的所述二氧化钛颗粒。
14. 根据权利要求6所述的用途,其中,所述第二层(B)包含按所述层的总重量计从1wt%至5 wt%的量的通过所述有机涂层涂覆的所述二氧化钛颗粒。
15.根据权利要求13所述的用途,其中,层(A)中通过所述有机涂层涂覆的所述二氧化钛颗粒的量大于层(B)中通过有机涂层涂覆的二氧化钛颗粒的量。
16.根据权利要求6所述的用途,其中,所述第二层(B)包含源自所述多层膜的制造的再生废膜。
17.根据权利要求6所述的用途,其中,所述层(A)的厚度小于所述层(B)的厚度,或者其中,所述层(A)的厚度为所述层(B)的厚度的10%至40%。
18.根据权利要求6所述的用途,其中,所述层(A)的厚度小于所述层(B)的厚度,或者其中,所述层(A)的厚度为所述层(B)的厚度的20%至30%。
19. 根据权利要求1至18中任一项所述的用途,其中,所述膜的总厚度为12 μm至500 μm。
20. 根据权利要求1至18中任一项所述的用途,其中,所述膜的总厚度为20 μm至100 μm。
21.根据权利要求1至18中任一项所述的用途,所述聚酯膜是双轴取向聚酯膜。
22.根据权利要求1至18中任一项所述的用途,其中,所述聚酯选自聚对苯二甲酸乙二醇酯和聚萘二甲酸乙二醇酯。
23.根据权利要求1至18中任一项所述的用途,其中,所述聚酯选自聚对苯二甲酸乙二醇酯。
24.根据权利要求1至18中任一项所述的用途,其中,二氧化钛为金红石晶型。
25.根据权利要求1至18中任一项所述的用途,其中,所述二氧化钛颗粒被所述有机涂层均匀并且离散地涂覆。
26. 根据权利要求1至18中任一项所述的用途,其中,所述烷基膦酸或它的酯具有式P(R)(=O)(OR1)(OR2),其中:
R为含有6至22个碳原子的烷基或环烷基;并且
R1和R2各自为氢、烷基、环烷基、芳基或芳烷基。
27.根据权利要求1至18中任一项所述的用途,其中,所述烷基膦酸的烷基或R含有6至14个碳原子,并且是直链烷基。
28.根据权利要求26所述的用途,其中,R1和R2独立地选自氢和含有至多达10个碳原子的烃基。
29.根据权利要求26所述的用途,其中,R1和R2为氢。
30.根据权利要求1至18中任一项所述的用途,其中,所述烷基膦酸或它的酯选自正辛基膦酸和它的酯、正癸基膦酸和它的酯、2-乙基己基膦酸和它的酯、以及莰基膦酸和它的酯。
31.根据权利要求1至18中任一项所述的用途,其中,涂覆的所述二氧化钛具有使得它在290°C下显示出不大于1.0%的损失的水含量,所述水含量通过库仑卡尔费歇尔滴定法测量。
32.根据权利要求1至18中任一项所述的用途,其中,涂覆的所述二氧化钛具有使得它在290°C下显示出不大于0.5%的损失的水含量,所述水含量通过库仑卡尔费歇尔滴定法测量。
33.根据权利要求1至18中任一项所述的用途,其中,有机涂覆的所述二氧化钛不是疏水的。
34.根据权利要求1至18中任一项所述的用途,其中,有机涂覆的所述二氧化钛是亲水的。
35. 根据权利要求1至18中任一项所述的用途,其中,所述有机涂层以按所述二氧化钛的重量计从0.1至200 wt%的量存在。
36. 根据权利要求1至18中任一项所述的用途,其中,所述有机涂层以按所述二氧化钛的重量计从0.1至100 wt%的量存在。
37. 根据权利要求1至18中任一项所述的用途,其中,所述有机涂层以按所述二氧化钛的重量计从0.5至100 wt%的量存在。
38. 根据权利要求1至18中任一项所述的用途,其中,所述有机涂层以按所述二氧化钛的重量计从2.0至20 wt%的量存在。
39.根据权利要求1至18中任一项所述的用途,其中,所述二氧化钛颗粒与所述有机涂层的体积比为按体积计1:1至1:25。
40.根据权利要求1至18中任一项所述的用途,其中,所述二氧化钛颗粒与所述有机涂层的体积比为按体积计1:2至1:8。
41.根据权利要求1至18中任一项所述的用途,其中,所述二氧化钛颗粒带有无机涂层,其中,所述有机涂层被涂覆到无机涂覆的所述二氧化钛颗粒上。
42.根据权利要求41所述的用途,其中,所述无机涂层是二氧化硅和/或氧化铝涂层。
43.根据权利要求42所述的用途,其中,所述无机涂层是氧化铝涂层。
44. 根据权利要求1至18中任一项所述的用途,其中,涂覆的所述二氧化钛颗粒通过有机涂层涂覆,具有0.01 μm至5.0 μm的粒度。
45. 根据权利要求1至18中任一项所述的用途,其中,涂覆的所述二氧化钛颗粒通过有机涂层涂覆,具有0.10 μm至0.40 μm的粒度。
46.根据权利要求1至18中任一项所述的用途,其中,所述膜不包含有机水解稳定剂。
47.根据权利要求1至18中任一项所述的用途,其中,所述膜不包含有机紫外线吸收剂。
48.根据权利要求1至18中任一项所述的用途,其中,所述膜是白色的。
49.根据权利要求1至18中任一项所述的用途,其中,所述聚酯膜的抗水解性使得在121°C和100%相对湿度下加速老化至少80小时之后,断裂伸长率为至少10%。
50.根据权利要求1至18中任一项所述的用途,其中,所述聚酯膜的抗水解性使得在121°C和100%相对湿度下加速老化至少80小时之后,断裂伸长率为至少20%。
51.根据权利要求1至18中任一项所述的用途,其中,所述聚酯膜的抗水解性使得在121°C和100%相对湿度下加速老化至少80小时之后,断裂伸长率为至少30%。
52.根据权利要求1至18中任一项所述的用途,其中,所述有机涂层不是并且不包含聚硅氧烷。
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2017
- 2017-05-08 GB GBGB1707356.0A patent/GB201707356D0/en not_active Ceased
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2018
- 2018-05-08 US US16/609,421 patent/US11629241B2/en active Active
- 2018-05-08 EP EP18725589.8A patent/EP3635037B1/en active Active
- 2018-05-08 KR KR1020197034176A patent/KR102616009B1/ko active IP Right Grant
- 2018-05-08 CN CN201880030462.4A patent/CN110650995B/zh active Active
- 2018-05-08 WO PCT/GB2018/051225 patent/WO2018206929A1/en active Search and Examination
- 2018-05-08 JP JP2020512926A patent/JP7202364B2/ja active Active
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WO2016146982A1 (en) * | 2015-03-13 | 2016-09-22 | Dupont Teijin Films U.S. Limited Partnership | Pv cells and backsheet polyester films |
Also Published As
Publication number | Publication date |
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CN110650995A (zh) | 2020-01-03 |
EP3635037B1 (en) | 2024-09-25 |
KR20200004326A (ko) | 2020-01-13 |
JP2020520406A (ja) | 2020-07-09 |
KR102616009B1 (ko) | 2023-12-22 |
JP7202364B2 (ja) | 2023-01-11 |
GB201707356D0 (en) | 2017-06-21 |
US11629241B2 (en) | 2023-04-18 |
US20200087488A1 (en) | 2020-03-19 |
WO2018206929A1 (en) | 2018-11-15 |
EP3635037A1 (en) | 2020-04-15 |
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