CN103153615A - 多层组件 - Google Patents

多层组件 Download PDF

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Publication number
CN103153615A
CN103153615A CN2011800497150A CN201180049715A CN103153615A CN 103153615 A CN103153615 A CN 103153615A CN 2011800497150 A CN2011800497150 A CN 2011800497150A CN 201180049715 A CN201180049715 A CN 201180049715A CN 103153615 A CN103153615 A CN 103153615A
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China
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composition
polymer
multilayer module
layer
ctfe
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CN2011800497150A
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CN103153615B (zh
Inventor
S.卡雷拉
M.巴西
S.莫尔塔拉
P.托尼奥洛
J.A.阿布斯莱梅
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Solvay Specialty Polymers Italy SpA
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Solvay Solexis SpA
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    • H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
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Abstract

本发明涉及一种多层组件，该多层组件包含：(L1)一个第一内层[层(L1)]，该第一内层由一种第一组合物[组合物(C1)]制成，所述组合物(C1)包含：至少一种聚合物，该聚合物包含衍生自乙烯(E)以及三氟氯乙烯(CTFE)的重复单元；以及至少一种Ti化合物；以及(L2)一个第二外层[层(L2)]，该第二外层由一种第二组合物[组合物(C2)]制成，所述组合物(C2)基本上没有含TiO2的添加剂，所述第二组合物包含至少一种半结晶聚合物，该半结晶聚合物包含衍生自乙烯以及至少一种选自三氟氯乙烯(CTFE)、四氟乙烯(TFE)及其混合物的含氟单体的重复单元，所述半结晶聚合物具有至少35J/g的熔化热[聚合物(A)]。

Description

多层组件
本申请要求于2010年10月15日提交的欧洲申请号10187732.2以及于2011年4月12日提交的欧洲申请号11162130.6的优先权，出于所有的目的这些申请的全部内容通过引用结合在此。
技术领域
本发明涉及包含乙烯/三氟氯乙烯层的多层组件，更具体地涉及具有紫外阻隔特性的多层组件，该多层组件适于曝露于紫外辐射。
背景技术
乙烯/三氟氯乙烯聚合物因它们的杰出透明性、耐候性及机械特性而被广泛用于制造保护及包装薄膜以及涂层。
通常，颜料或添加剂，或者更广泛的含钛化合物被嵌入用于制备所述薄膜或涂层的乙烯/三氟氯乙烯聚合物中；例如，已发现TiO2化合物特别适用作紫外阻隔剂，从而成为要求紫外线不透过时的选择材料。
目前，钛化合物的光催化活性是一种公认现象，其可削弱聚合物基体的稳定性，并从而使薄膜或涂层丧失认可的长期性能，包括光学性能、机械性能。
尽管当通过惰性层在表面上涂覆/修饰时，将二氧化钛添加剂大量混合至所述聚合物基体中，然而，这些涂层对于乙烯/三氟氯乙烯聚合物完全抑制降解催化及酰氯产生并非全部有效，从而薄膜和涂层通常经历黄变现象，透明度和雾度以及机械性能很快受到影响。当乙烯/三氟氯乙烯聚合物长时间曝露在太阳光及环境条件下时，例如当这些薄膜用作PV电池模块中的保护前膜时，该问题尤其易于出现。
因此，目前在本领域中对于含钛化合物的乙烯/三氟氯乙烯聚合物结构存在不足之处，这些结构可承受UV和VIS光曝露并抵御潮湿和干燥条件，而不进行显著降解，并因此保持它们的原有特性(包括光学和机械特性)。
包括含钛化合物的ECTFE层的多层结构的实例是众所周知的。
因此，文件EP1281730A(AUSIMONT SPA)05/02/2003披露了一种金属基板的多层涂层，其中第一层包含一种ECTFE树脂，有可能包含一种填充剂(云母、金属氧化物、无机颜料)，该第一层进一步涂覆有通常包含一种改性共聚单体的其他ECTFE聚合物的另一层，从而降低它的结晶度。因此，该申请的实例3披露了一种多层结构，其中包含一种ECTFE聚合物的层粘附至一个金属基板上并涂覆有一种具有熔点221℃的乙烯(E)、三氟氯乙烯(CTFE)、全氟丙基乙烯醚(PFPVE)的三元共聚物，其中该ECTFE聚合物包含3％wt的涂有TiO2的云母颜料添加剂；由该申请人进行的测试证实，该材料具有低结晶度。
附图简要说明
图1示出了所记录的实例1的多层组件ECTFE-1//(ECTFE-2+紫外阻隔剂)//ECTFE-1，通过Perkin Elmer Lambda6分光光度计测量的紫外-可见透射率(％)与波长(nm)的函数关系，所述ECTFE-1具有至少35J/g的熔化热。
图2描述了在曝露QUV-B条件之前、以及在曝露所述条件的500小时之后和2000小时之后，记录的如上所述的实例1组件的TT(％)与波长(nm)的函数关系。
发明内容
因此，本发明涉及一种多层组件，该多层组件包含：
(L1)一个第一内层[层(L1)]，该第一内层由一种第一组合物[组合物(C1)]制成，所述组合物(C1)包含：
至少一种聚合物，该聚合物包含衍生自乙烯(E)以及三氟氯乙烯(CTFE)的重复单元，以及
至少一种Ti化合物；以及(L2)一个第二外层[层(L2)]，该第二外层由一种第二组合物[组合物(C2)]制成，所述组合物(C2)基本上没有含TiO2的添加剂，所述第二组合物包含至少一种半结晶聚合物，该半结晶聚合物包含衍生自乙烯以及至少一种选自三氟氯乙烯(CTFE)、四氟乙烯(TFE)及其混合物的含氟单体的重复单元，所述半结晶聚合物具有至少35J/g的熔化热[聚合物(A)]。
本申请人出人意料地发现，当将含钛化合物的ECTFE聚合物第一层与由高结晶氟化单体制成的第二层组合时，如上所述，基本上抑制了第一层的天气引起的降解。
不受这种理论的束缚，但本申请人认为，高结晶层的存在显著减小了环境湿气和/或氧通过所述层渗透及渗入至该含钛化合物的ECTFE层，当曝露于紫外线时，该渗入及渗透的水和/或氧主要负责产生自由基，并从而攻击该ECTFE聚合物基体，尤其是C-Cl键。
根据ASTM D3418，以10℃/min的加热速率，通过差示扫描热量法(DSC)确定聚合物(A)的熔化热。
聚合物(A)具有至少35J/g的熔化热，优选至少37J/g，更优选至少40J/g。
无熔化热上限是至关重要的，然而，应理解的是，聚合物(A)总体上具有最多55J/g的熔化热，优选最多53J/g的熔化热，更优选最多50J/g的熔化热。
本领域内众所周知的是，50/50mol/mol ECTFE或ETFE共聚物显示初最大结晶度，例如，最大熔点和熔化热。因此，对于至少35J/g熔化热的要求可以ECTFE和ETFE共聚物50/50摩尔比左右的组成范围实现，或者相对于该50/50摩尔比，通过非常轻微地增加或非常轻微地减小乙烯的量而实现。
本发明的组合物(C2)的聚合物(A)典型地包含：
(a)按摩尔计，从45％至55％，优选从47％至53％的乙烯(E)；
(b)按摩尔计，从55％至45％，优选从53％至47％的三氟氯乙烯(CTFE)、四氟乙烯(TFE)或其混合物；以及
(c)基于单体(a)和(b)的总量，按摩尔计，从0至5％，优选从0至2.5％的一种或多种氟化的和/或氢化的共聚单体。
优选地，该共聚单体(c)是选自如以上定义的丙烯酸单体群组的一种氢化的共聚单体。更优选地，该氢化的共聚单体选自丙烯酸羟烷基酯共聚单体(如羟乙基丙烯酸酯、羟丙基丙烯酸酯和(羟基)乙基己基丙烯酸酯)组成的群组。
然而，如上所述，优选聚合物(A)无共聚物(c)。
在聚合物(A)中，优选ECTFE共聚物，例如乙烯和CTFE的共聚物(以及任选地一种第三单体，如上所述)。
适用于本发明组合物的ECTFE聚合物通常具有超过220℃的熔融温度，优选超过225℃，甚至超过230℃，优选超过235℃。根据ASTM D3418，通过差示扫描热量法(DSC)以10℃/min的加热速率，确定该熔融温度。
本发明组件的组合物(C2)中发现给出特别良好结果的ECTFE聚合物基本上由衍生自以下的重复单元的那些组成：
(a)按摩尔计，从48％至52％的乙烯(E)；
(b)按摩尔计，从52％至48％的三氟氯乙烯(CTFE)。
导致重复单元不同于上述那些的端链、缺陷或少量单体杂质仍可包含在该优选ECTFE中，而这不影响该材料的特性。
按照ASTM3275-81程序，在230℃和2.16Kg条件下测量，ECTFE聚合物的熔体流动速率通常在0.01至75g/10min范围内，优选0.1至50g/10min，更优选0.5至30g/10min。
组合物(C2)基本上没有含TiO2的添加剂；该表述意在表示不存在有效剂量的含TiO2的添加剂以激发紫外催化的降解现象。相对于聚合物(A)的重量，这典型地对应于含TiO2的添加剂的量小于0.1％wt，优选小于0.05％wt，更优选小于0.01％wt。
除了聚合物(A)之外，组合物(C2)还可包含另一种热塑性聚合物。未特别限制该附加热塑性聚合物的选择；可使用氟化聚合物及氢化聚合物。通常，相对于聚合物(A)，小量使用这些附加成分。
根据某些实施例，组合物(C2)包括如上所述的聚合物(A)混合至少一种其他半结晶聚合物，该其他半结晶聚合物包含衍生自乙烯以及至少一种选自三氟氯乙烯(CTFE)、四氟乙烯(TFE)及其混合物的含氟单体的重复单元，所述半结晶聚合物具有小于35J/g的熔化热[聚合物(B)]。
根据该实施例，组合物(C2)总体上包含聚合物(A)作为主要成分，同时包含少量聚合物(B)，以便不会不利地影响层(L2)的阻隔特性；相对于聚合物(A)的重量，典型的量在5％wt至25％wt的范围内。
然而，优选实施例为聚合物(A)是组合物(C2)的唯一聚合物成分的实施例。
组合物(C2)任选地进一步包含填充材料，导电颗粒，润滑剂，热稳定剂，抗静电剂，增充剂，增强剂，有机和/或无机颜料，酸清除剂，如MgO，阻燃剂、抑烟剂等。
通过填充材料的非限制实例，可提及云母、氧化铝、滑石、炭黑、玻璃纤维、碳纤维、纤维或粉末形式的石墨、碳酸盐如碳酸钙制成。
当根据ASTM D1003标准于空气中测量时，当在具有约50μm厚度的层(L2)上确定时，层(L2)总体上优选为透明的，也就是说具有大于80％、优选大于85％、更优选大于92％的总透射率。
应理解的是，根据ASTM D1003，可确定在空气和水两者中层(L2)的总透射率。在这个后者的情况下，有待测量的样品典型地被置于填充有去离子水的石英瓶中。
因此，当在水中测量时，层(L2)的总透射率通常为至少85％，更优选至少90％，甚至更优选至少94％。
为此目的，组合物(C2)优选基本不含具有100nm或更大平均粒径的填充材料。典型地，组合物(C2)可完全不含任何尺寸的填充材料，如上所述。
未特别限制层(L2)的厚度；然而，应理解的是，层(L2)具有至少5μm、优选至少10μm、更优选至少12.5μm的厚度。具有小于5μm厚度的层(L2)尽管适用于本发明的多层组件，但是但当要求足够机械阻力时将不使用。
未特别限制层(L2)的厚度的上限，条件是所述层(L2)仍能提供指定使用的特定领域所要求的柔性及透明度。
对于用于保护PV电池模块的多层组件，有利地使用具有最多150μm、优选最多100μm、更优选50μm厚度的层(L2)。
本发明的多层组件的层(L1)由组合物(C1)制成，该组合物包含：
至少一种聚合物，该聚合物包含衍生自乙烯(E)以及三氟氯乙烯(CTFE)的重复单元，以及
至少一种Ti化合物。
组合物(C1)的ECTFE聚合物通常包含：
(a)按摩尔计，从10％至90％，优选从30％至70％的乙烯(E)；
(b)按摩尔计，从90％至10％，优选从70％至30％的三氟氯乙烯(CTFE)；以及
(c)基于单体(a)和(b)的总量，按摩尔计，从0％至30％，优选从0.1％至15％的一种或多种氟化的和/或氢化的共聚单体。
例如，氟化的共聚单体的非限制性实例是例如全氟代烷基乙烯基醚、全氟代烷基乙烯(如全氟丁基乙烯)、全氟间二氧杂环戊烯、偏二氟乙烯。在它们中，优选的共聚单体是具有化学式CF2＝CFO-C3F7的全氟丙基乙烯基醚。
[0041]氢化的共聚单体的非限制性实例是具有以下通式的那些：CH2＝CH-(CH2)nR1，其中R1＝OR2，或-(O)tCO(O)pR2，其中t和p为等于0或1的整数，并且R2为H或氢化的直链或支链烷基或具有从1至20个碳原子的环烷基，任选地含有杂原子和/或氯原子，这些杂原子优选为O或N；R2任选地含有一个或多个官能团，优先选自OH、COOH、环氧化物、酯和醚，R2可以任选地含有双键；n为0-10范围内的一个整数。优选地，R2为含有羟基官能团的具有从1至10个碳原子的烷基，并且n为0-5范围内的一个整数。
[0042]优选的氢化的共聚单体选自以下类别：
具有以下通式的丙烯酸单体：CH2＝CH-CO-O-R2，其中R2选自丙烯酸乙酯、丙烯酸正丁酯、丙烯酸、羟烷基丙烯酸酯(如羟乙基丙烯酸酯、羟丙基丙烯酸酯、(羟)乙基己基丙烯酸酯)；
具有以下通式的乙烯基醚单体：CH2＝CH-O-R2，其中R2选自丙基乙烯基醚、环己基乙烯基醚、乙烯基-4-羟基丁基醚；
具有以下通式的羧酸的乙烯基单体：CH2-CH-O-CO-R2，其中R2选自乙酸乙烯酯、丙酸乙烯酯、乙烯基-2-乙基己酸酯；
具有以下通式的不饱和羧酸单体：CH2＝CH-(CH2)n-COOH，其中n具有以上提到的含义，例如乙烯基乙酸。
组合物(C1)的ECTFE聚合物具有的熔化热，如根据ASTM D3418，通过差示扫描热量法(DSC)以10℃/min的加热速率确定的为大于、等于或小于35J/g。换言之，组合物(C1)的ECTFE聚合物的结晶分数并非特别关键。
然而，当旨在最大化其中纳米级填料的分散能力时，优选具有低结晶度的ECTFE聚合物，即，具有小于35J/g、优选小于30J/g、更优选小于25J/g的熔化热。
因此，应理解的是，组合物(C1)优选的ECTFE聚合物实际上是那些包含大量衍生自小于50％摩尔、优选小于48％摩尔、更优选45％摩尔的乙烯的重复单元，因为它们使能由于含氟单体成分而实现改进的特性。
因此，组合物(C1)优选包含一种ECTFE聚合物，该ECTFE聚合物包含：
(a)按摩尔计，从30％至48％，优选从35％至45％的乙烯(E)；
(b)按摩尔计，从52％至70％，优选从55％至65％的三氟氯乙烯(CTFE)；以及
(c)基于单体(a)和(b)的总量，按摩尔计，从0至5％，优选从O至2.5％的如上所述的一种或多种氟化的和/或氢化的共聚单体。
组合物(C1)中发现给出特别良好结果的ECTFE聚合物为基本上由衍生自以下的重复单元的那些组成：
(a)按摩尔计，从35％至47％的乙烯(E)；
(b)按摩尔计，从53％至65％的三氟氯乙烯(CTFE)。
导致重复单元不同于上述那些的端链、缺陷或少量单体杂质仍可包含在该优选ECTFE中，而不影响该材料的特性。
关于钛化合物，它的选择将依赖于通过该添加剂获得所要求的特定功能。
当该Ti化合物旨在作为紫外阻隔剂时，典型地优选含有TiO2的无机化合物。
根据本发明的第一实施例，该Ti化合物为一种无机紫外阻隔化合物，该无机紫外阻隔化合物含有TiO2，且有可能含有至少一种其他无机氧化物。
在本实施例的含有TiO2的优选无机紫外阻隔化合物中，可以提及包含以下项的颗粒制成：
一个核芯，该核芯基本上由TiO2组成；以及
一个外壳，该外壳基本上由至少一种硅氧化物、铝氧化物或其混合物组成。
尽管未特别限制TiO2的晶型，应理解的是为了抑制光催化活性及由此产生的分解现象，总体上可理解的是金红石型TiO2优于锐钛矿型。
如上所述，该实施例的颗粒可进一步包含至少一个第三材料的其他层，该第三材料可为与该核芯和该外壳材料相同或不同的材料。这些颗粒可额外包含一种适当的涂层添加剂(如分散剂、稳定剂、抗静电剂等)的附加涂层，该附加涂层可完全包围(如封装)或部分覆盖该颗粒。已发现有机分散剂的涂层尤其有用，尤其是使用硬脂酸盐(酯和盐)的那些。
该实施例的颗粒总体上具有小于150nm、优选小于120nm、更优选小于100nm的平均粒径。具有小于150nm平均粒径的颗粒的选择普遍被建议用于实现层(L1)的透明度。实际上，如果使用大小明显小于可见光波长(通常从约380nm至约850nm)的颗粒，则大幅减小散射，从而可见光可穿透并传播，进而确保透明度。
由包括含TiO2的无机紫外阻隔化合物的组合物(C1)制成的层(L1)特别适用于制备旨在作为PV电池模块的保护前板的多层组件。
当根据ASTM D1003标准于空气中测量时，当在具有约50μm厚度的层(L2)上确定时，根据该实施例的层(L1)典型地具有大于85％、优选大于90％、甚至优选大于92％的总透射率。
根据本发明的第二实施例，该Ti化合物为一种含有TiO2、有可能结合其他无机氧化物的颜料。
对于不要求透明度的使用领域，将选择着色组合物(C1)；然而，在这些领域中，颜色稳定性及降解现象的避免，产生如机械特性不足或减少，仍极其有价值。
更普遍地，未特别限制层(L1)的厚度；然而，应理解的是，层(L1)具有至少15μm、优选至少20μm、更优选25μm的厚度。但是，具有小于15μm厚度的层(L1)尽管适用于本发明的多层组件，但当要求足够的机械阻力时将不被使用。
未特别限制层要求需的柔性及透明度。
对于用于保护PV电池模块的多层组件，有利地使用具有最多125μm、优选最多100μm、更优选75μm厚度的层(L1)。
总体上，层(L1)和层(L2)相互粘合，无需额外的粘附层。然而，在不超出本发明的范围内，层(L1)和层(L2)之间可存在一附加层。
然而，典型地优选其中层(L1)和(L2)直接连接的多层组件。
该多层组件可额外包含一个第三层(L3)，所述层粘附至层(L2)的相对侧的层(L1)上。
因此，该实施例的多层组件的设计可提供如上所述的层(L1)包含在如上所述的层(L2)与层(L3)之间，其中该层(L3)等于或不同于层(L2)，由一种组合物(C3)制成。
尽管未特别限定层(L3)的选择，特别适用于本发明目的的实施例为那些层(L3)由具有与上述组合物(C2)相同特征的组合物(C3)制成的实施例；优选地，层(L3)的组合物(C3)等同于层(L2)的组合物(C2)。
层(L2)的上述所有特征可提供给该实施例的层(L3)。
本发明还涉及一种用于制造上述多层组件的方法。
可使用任何用于组装聚合物层的常用技术以制备根据本发明的多层组件。
可能提及的这些技术的实例包括在至少等于它的聚合物成分的软化点的温度下，典型地超过它的聚合物成分的熔点的温度下，使用组合物(C1)、(C2)及可选(C3)的那些实例。优选地，通过共层压(colaminating)、共挤出(如共挤出层压、共挤出-吹塑以及共挤出模制)、挤出涂覆、涂覆、包覆注塑模制(overinjection-moulding)或共注塑模制来进行根据本发明的多层组件的制备。
通过共层压、共挤出或包覆注塑模制，以特别优选方式执行用于制备根据本发明的多层组件的方法。
基于多层组件使用以及每层的厚度，选择这些组合技术的一种或其他。
例如，旨在用作管、管道、膜、片材和板的多层组件通过共挤出优选地制备。
因此，通过上述层(L1)、层(L3)及可选层(L3)的共挤出，优选地进行本发明多层组件的制备方法。
根据本发明的多层组件的厚度并非关键，并且明显取决于对于所述组件所打算的使用。
本发明还涉及根据本发明的多层组件用于制造管、管道、包层、膜、片材、型材、板及空心体的用途。
如上所述，包含透明层的多层组件特别适于用作建筑膜、面料以及用于食品和药品包装。
而且，此外，根据本发明的另一实施例，发现本发明的多层组件特别关注的使用领域为PV模块保护领域。
因此，用于保护PV模块的方法为本发明的另一方面，其中该方法包括使用至少一个上述多层组件覆盖所述模块。
根据该方法，该多层组件可用于PV电池模块的前或后保护，前侧为曝露于入射光侧。如上所述，包含透明层的多层组件特别适用于PV模块中的前片。
又，本发明的多层组件已成功用作具有高水及氧气阻隔特性的复合膜的保护层。在该方法中，本发明的多层组件总体上进一步组装至聚对苯二甲酸乙二醇酯(PET)或聚萘二甲酸乙二醇酯(PEN)薄膜上，其中PET或PEN优选进一步涂有高阻隔材料薄层。通常，该高阻隔材料为一种无机材料，优选选自二氧化硅、氧化铝或其他混合氧化物，它们当经由如MOCVD技术涂覆时，有利地可提供10至50nm、优选10至20nm的涂层，仍确保可见光辐射的透明度。通过使用选自环氧或聚氨酯胶的胶黏剂，将本发明的多层组件粘附至该PET或PEN薄膜上涂覆的高阻隔材料层上而得到多层复合膜。因此，包含从外层至内层以下列顺序：层(L2)、层(L1)、任选地层(L3)、粘附层、高阻隔层以及PET或PEN层的组件为该实施例的优选实施例，从而使能实现良好氧气和水蒸气阻隔[当在38℃及90％RH下测定时，通常小于10-2g/(m2x天)]，结合杰出的耐候性及透明性。该实施例的组件特别适用作若干有机/无机电子装置(包括但不限于PV电池)的保护层。
该实施例的组件特别适用于保护PV电池的活性层，其中这些活性层对氧气和/或湿气特别敏感。在优选使用该实施例的组件保护的这类PV电池中，提及可为基于镓铟铜(二)硒化合物(CIGS)、碲化镉(CdTe)及有机光敏化合物的活性层。
若任何引用结合在此的专利、专利申请以及公开物中的披露内容与本申请的描述相冲突到达可能导致术语不清楚的程度，则本说明应该优先。
现在将参照以下实例更详细描述本发明，这些实例的目的仅是用作说明而非限制本发明的范围。
原料
聚合物
ECTFE-1为商标名称为
Figure BDA00003049120400141
的市售的50/50摩尔％的乙烯/三氟氯乙烯(E/CTFE)共聚物，具有242℃的熔点(Tm2)，42J/g的熔化热(ΔH2f)以及18g/10min(275℃/2.16kg)的MFI。
ECTFE2：为41/59摩尔％的E/CTFE共聚物，具有180℃的熔点(Tm2)，18J/g的熔化热(ΔH2f)以及1.4g/10min(230℃/2.16kg)的MFI。
含Ti化合物
TiO2-1为德国莎哈利本化学有限公司(Sachtleben Chemie GmbH)的商标名称为
Figure BDA00003049120400142
的市售紫外阻隔剂，其由核-壳型颗粒形成，这些核-壳型颗粒具有TiO2核，该TiO2核涂有混合Al2O3-SiO2氧化物的壳，这些颗粒使用硬脂酸表面处理，所述颗粒具有15nm的平均粒径，且可为粉末形式。
聚合组合物的制备及制粒
在配有三级桨式混合机的快速混合器中，对粉末形式的ECTFE-2聚合物及上述紫外阻隔颗粒进行预混，从而得到一种均匀粉末混合物，该均匀粉末混合物具有所述成分之间所要求的重量比。
ECTFE-1中不包括添加剂，也可为一粉末。
然后，在配有6个温区及4mm2孔模口的双螺杆30-34挤出机(LEISTRITZ)中，通过挤出来处理ECTFE-2和紫外阻隔剂和/或ECTFE-1粉末的粉末混合物。基于ECTFE-1和ECTFE-2的组合物的处理设定点分别总结于表1和表2中。
ECTFE-1
表1
进料区 T1 T2 T3 T4 T5
210 225 240 250 260 270
螺杆速度设定为300rpm，转矩为49％，从而产生约6kg/h的通过量，并且熔融挤出温度为265℃。
基于ECTFE-2的组合物
表2
进料区 T1 T2 T3 T4 T5
180 200 200 210 220 220
螺杆速度设定为300rpm，转矩为59％，从而产生约6.6kg/h的通过量，并且熔融挤出温度为265℃。
将挤出的线股在水浴中冷却、进行干燥、校准并且在一台造粒机中进行切割。
实例1-通过共挤出制备多层组件
为了制备多层组件，在配有2.5”单级挤出机(A)和2”卫星共挤出机(B)的共挤出流延膜生产线中处理这些颗粒。挤出机经由配有选择器塞头的分流器连接至模口以提供以下层顺序：B/A/B(L2/L1/L3)。该模口为915mm宽自动测量模口。离开该模口时，熔化带被流延在三个随后冷却辊上，调节它的速度以得到约100μm厚度的薄膜。通过具有更新模口的β射线测量控制系统，控制总厚度及随着宽度的厚度变化。以下处理条件用于100μm厚的薄膜(25/50/25μm为部分厚度顺序)。
挤出机A供有ECTFE-2和紫外阻隔剂的组合物的颗粒，如上详述制备(用作层L1)的，同时共挤出机B供有ECTFE-1的颗粒(用作层L2和L3)。两个挤出机均配有网包过滤器(screen packfilter)。
为了得到所希望的厚度及比率，挤出机及生产线速度设定如下：
挤出机A＝＞65rpm
挤出机B＝＞70rpm
生产线速度＝＞12m/min。
这些实例中使用的挤出机A温度特征曲线总结于表3中：
表3
区 温度(℃)
主机筒区1 255
主机筒区2 260
主机筒区3 260
主机筒区4 260
主机筒区5 260
夹具 260
适配器1 260
适配器2 260
这些实例中使用的挤出机B温度特征曲线总结于表4中：
表4
区 温度(℃)
主机筒区1 275
主机筒区2 280
主机筒区3 280
主机筒区4 280
夹具 280
适配器1 280
适配器2 280
分流器、模口和压延辊温度进一步详见表5：
表5
区 温度(℃)
分流器 280
模口区1 285
模口区2 285
模口区3 285
模口区4 285
模口区5 285
上辊 90
中辊 170
下辊 170
在边缘切割之后，薄膜的总宽度为约710mm。
多层组件的表征
利用Gardner Haze-Gard Plus仪器，根据ASTM D1003，对实例1的多层组件表征它的光学特性。为了评估有可能与表面粗糙度或缺陷相关的虚假影响，将薄膜样品在水中，即，通过浸没在一个充满水的石英试池中来分析样本。确定了总透射率为94.7％并且雾度值为4.8，很好地证明本发明的多层组件的透明度及清晰度。图1示出了所记录的实例1的多层组件ECTFE-1//(ECTFE-2+紫外阻隔剂)//ECTFE-1，通过Perkin Elmer Lambda6分光光度计测量的紫外-可见透射率(％)与波长(nm)的函数关系。
QUV-B测试-一般步骤
QUV-B测试法为一种循环紫外风化步骤，在该方法中，分层的颗粒固定在面对发出UV辐射(即UV-B313nm)的荧光灯的堤层(bank)的支架中。该波长对于分解/降解聚合物尤其有用；即使自然光不足，也可实现耐候性及抗紫外线的加速评估。
在测试过程中，通过冷凝而不是通过喷射将水施加至测试样品上。为了控制循环测试，该QUV配有一可变间隔定时器，其中该可变间隔定时器使UV和冷凝在50℃交替，后跟随8小时70℃UV辐射以及高温度。
上述QUV测试用于监控本发明的多层组件抵御紫外曝光及天气条件；在曝露QUV-B条件各种时间之后，水中测定总透射率及雾度并与初始值对比。
为了进行比较的目的，对由上述组合物ECTFE-2+紫外阻隔剂制成的单层薄膜以及多层组件ECTFE-2//(ECTFE-2+紫外阻隔剂)//ECTFE-2进行相同测试。所有结果总结于以下表中。
表6
Figure BDA00003049120400181
表6中提供的数据证实：在不存在外层(L2)时，曝露QUV-B条件500小时之后，含有Ti化合物的ECTFE聚合物的薄膜快速降解，从而产生不可接受的雾度(大于10)及TT(小于90％)的值。
另一方面，具有至少35J/g熔化热的聚合物(A)的保护层的内含物可对所述内膜提供适当的保护，从而即使延长曝露QUV-B条件，雾度和TT也可保持在可接受的水平。换句话说，该组件保持透明及清晰，并且在吸收光谱中未检测到显著变化；因此，图2描述了曝露于QUV-B条件之前、500小时之后以及2000小时之后，所记录的实例1组件的TT(％)与波长(nm)的函数关系：可以看出光学行为无显著差异。对比的最后实例示出了作为具有至少35J/g熔化热的聚合物(A)的保护层的选择的关键性：在这种情况下，其中该保护层由不符合这种要求的聚合物制成，组件的光学特性尤其是雾度在曝露QUV-B2000小时之后经历实质性降解。

Claims (17)

1.一种多层组件，该多层组件包含：
(L1)第一内层[层(L1)]，该第一内层(L1)由第一组合物[组合物(C1)]制成，所述组合物(C1)包含：
至少一种聚合物，该聚合物包含衍生自乙烯(E)以及三氟氯乙烯(CTFE)的重复单元，以及
至少一种Ti化合物；以及
(L2)第二外层[层(L2)]，该第二外层(L2)由第二组合物[组合物(C2)]制成，所述组合物(C2)没有含TiO2的添加剂，所述第二组合物包含至少一种半结晶聚合物，该半结晶聚合物包含衍生自至少一种选自三氟氯乙烯(CTFE)、四氟乙烯(TFE)及其混合物的含氟单体以及乙烯的重复单元，
所述半结晶聚合物具有至少35J/g的熔化热[聚合物(A)]。
2.如权利要求1所述的多层组件，其中该组合物(C2)的聚合物(A)包含：
(a)按摩尔计，从45％至55％，优选从47％至53％的乙烯(E)；
(b)按摩尔计，从55％至45％，优选从53％至47％的三氟氯乙烯(CTFE)、四氟乙烯(TFE)或其混合物；以及
(c)基于单体(a)和(b)的总量，按摩尔计，从0至5％，优选从0至2.5％的一种或多种氟化的和/或氢化的共聚单体。
3.如权利要求1或2所述的多层组件，其中该组合物(C2)的聚合物(A)为具有超过220℃的熔融温度的ECTFE聚合物。
4.如权利要求3所述的多层组件，其中该组合物(C2)的聚合物(A)基本由以下组成：
(a)按摩尔计，从48％至52％的乙烯(E)；
(b)按摩尔计，从52％至48％的三氟氯乙烯(CTFE)。
5.如上述权利要求中任一项所述的多层组件，其中组合物(C2)包含聚合物(A)作为唯一聚合物成分。
6.如上述权利要求中任一项所述的多层组件，其中层(L2)具有至少5μm、优选至少10μm、更优选至少12.5μm的厚度。
7.如上述权利要求中任一项所述的多层组件，其中组合物(C1)的ECTFE聚合物包含：
(a)按摩尔计，从10％至90％，优选从30％至70％的E；
(b)按摩尔计，从90％至10％，优选从70％至30％的CTFE；以及
(c)基于单体(a)和(b)的总量，按摩尔计，从0至30％，优选从0.1％至15％的一种或多种氟化的和/或氢化的共聚单体。
8.如权利要求7所述的多层组件，其中组合物(C1)的ECTFE聚合物基本由以下组成：
(a)按摩尔计，从35％至47％的E；
(b)按摩尔计，从53％至65％的CTFE。
9.如上述权利要求中任一项所述的多层组件，其中该钛化合物为含有TiO2的无机化合物。
10.如权利要求9所述的多层组件，其中该钛化合物为由包含以下的颗粒制成的无机紫外阻隔化合物，所述颗粒包含：
核芯，该核芯基本上由TiO2组成；以及
外壳，该外壳基本上由至少一种硅氧化物、铝氧化物或其混合物组成。
11.如上述权利要求中任一项所述的多层组件，进一步包含第三层(L3)，该第三层(L3)在层(L2)的相对侧粘附至层(L1)上。
12.如权利要求11所述的多层组件，其中层(L3)由与组合物(C2)相同的组合物(C3)制成。
13.一种用于制备如上述权利要求中任一项所述的多层组件的方法。
14.如权利要求13所述的方法，包含共层压、共挤出、挤出涂覆、涂覆、包覆注塑模制及共注塑模制中的任一项。
15.根据权利要求1至13中任一项所述的多层组件用于制造管、管道、包层、膜、片材、型材、板及空心体的用途。
16.一种用于保护PV模块的方法，该方法包括使用至少一个根据权利要求1至13中任一项所述的多层组件覆盖所述模块。
17.根据权利要求1至13中任一项所述的多层组件用以制备高阻隔复合膜的用途，包含通过使用选自环氧或聚氨酯胶的胶黏剂，将所述多层组件组合至高阻隔材料的薄层上，该高阻隔材料的薄层涂覆在聚对苯二甲酸乙二醇酯(PET)或聚萘二甲酸乙二醇酯(PEN)膜上。
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US20190351658A1 (en) 2019-11-21
JP6328423B2 (ja) 2018-05-23
JP2013544672A (ja) 2013-12-19
US11338558B2 (en) 2022-05-24
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KR20140004079A (ko) 2014-01-10
WO2012049193A1 (en) 2012-04-19

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