CN104816520A - 基于由非塑化聚乙烯醇缩醛形成的薄膜的具有热辐射隔离性能的复合玻璃层压件 - Google Patents

基于由非塑化聚乙烯醇缩醛形成的薄膜的具有热辐射隔离性能的复合玻璃层压件 Download PDF

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CN104816520A
CN104816520A CN201510059716.3A CN201510059716A CN104816520A CN 104816520 A CN104816520 A CN 104816520A CN 201510059716 A CN201510059716 A CN 201510059716A CN 104816520 A CN104816520 A CN 104816520A
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film
heat insulation
glass laminate
plasticizer
lamination glass
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CN104816520B (zh
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U.凯勒
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Kuraray Europe GmbH
Kuraray Co Ltd
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Kuraray Co Ltd
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Abstract

一种隔热层压玻璃层压件，由两块玻璃片之间的含有聚乙烯醇缩醛PA和任选的至少一种增塑剂WA的至少一个膜A和含有聚乙烯醇缩醛PB和至少一种增塑剂WB的至少一个膜B组成，特征在于在每种情况下在层压之前将少于16%重量的比例的增塑剂WA分散于膜A中，将至少16%重量的比例的增塑剂WB分散于膜B中，和将隔热颗粒分散于膜A中。

Description

基于由非塑化聚乙烯醇缩醛形成的薄膜的具有热辐射隔离性能的复合玻璃层压件
技术领域
本发明涉及一种使用基于非塑化聚乙烯醇缩醛的中间薄膜，生产具有隔热性能的层压玻璃片的方法。
为了生产具有隔热性能的层压玻璃片，其中以IR-吸收或IR-反射方式涂布的薄PET膜嵌入多个含有增塑剂的聚乙烯醇缩醛的层之间的方法是特别常用的。这里的一个缺点是这样的事实，即总是必须使用至少3个膜层(1 x 功能化PET， 2 x PVB膜)，因为PET不能通过功能化侧或背侧直接熔融在玻璃表面上。
除了玻璃表面的各种涂料的选择外，其替代在于使用含有大量IR吸收剂的中间层膜。举例来说，为此在膜生产期间将纳米级半导体颗粒，例如ITO或ATO，尽可能均匀地分布在膜的体积中。这里的一个缺点在于，在各种其它成分的存在下，在挤出法期间，难以保持颗粒在含有增塑剂的膜基质中的纳米级分布以使纳米颗粒的聚集不会导致不可接受的浊化。另一个缺点是增加了膜生产的复杂性，其由于特征“热-吸收”与另外的功能特征例如“声波阻尼”、“带通滤波”、“楔形厚度分布”和“遮蔽”的组合，导致生产商的产品以及处理机的范围增加。
作为对此的替代，WO 2005/059013 A1提出通过用特殊印刷油墨印刷PVB膜来应用热-吸收纳米颗粒。然而，膜粘附于玻璃表面的特性可受到印刷的不良影响。由于事实上PVB膜必须具有粗糙的表面以便不困难地去除层压过程中的空气，有可能对其施加的层(该层也部分地在可见光范围内吸收)在用玻璃表面压制后将是光学不均匀的。此外，厚塑化膜网的印刷是困难的，因为这样的膜在它们展开时会延展(alongated)，然后可能再收缩回来。
根据现有技术的热-绝缘膜具有分布于含增塑剂的层中的隔热颗粒。由于无机颗粒可能仅仅不佳地分散于所用的增塑剂中，存在着颗粒聚集的风险，因而存在膜浊化或玻璃层压件浊化的风险。
问题
因此，本发明要解决的问题是提供具有隔热特性的中间层膜，不必将纳米级半导体颗粒分散于含增塑剂的中间层膜的体积中。
已发现隔热颗粒可非常良好地分散于含有低水平的增塑剂或不含增塑剂的基于聚乙烯醇缩醛的薄膜中并且这些膜可在用于层压玻璃层压件的典型生产方法中直接熔融在一个玻璃表面上。
然后层压玻璃层压件通常需要的安全性特性可与含增塑剂的聚乙烯醇缩醛形成的至少一个层组合来获得。
因此，本发明涉及一种隔热层压玻璃层压件，由两块玻璃片之间的含有聚乙烯醇缩醛PA和任选的至少一种增塑剂WA的至少一个膜A和含有聚乙烯醇缩醛PB和至少一种增塑剂WB的至少一个膜B组成，其中，在每种情况下在层压之前
- 将少于16%重量的比例的增塑剂WA分散于膜A中，
- 将至少16%重量的比例的增塑剂WB分散于膜B中，和
- 将隔热颗粒分散于膜A中。
根据ISO 13837:2008 (v = 14 m/s; 以%计算的值)以试验层压件进行比较测量和评价，该试验层压件由2 x 2.1 mm透明玻璃(例如 PlaniluxTM)和中间布置的膜B(一种标准的汽车膜(例如 TROSIFOL VG R10 0.76))以及没有隔热颗粒的膜A组成，而相应构造的层压件中膜A具有隔热颗粒，认为隔热膜是具有如下的减少的总太阳能透射率(TTS)的膜：
TTS (无涂层的膜A) - TTS (有涂层的膜A) > 10%， > 12.5%， > 15%， > 17.5%或> 20%。
此外，根据本发明设置具有隔热颗粒的膜A，在与描述的试验层压件比较和对比后，可具有这样的优点：光透射(根据EN 410测量的TL; 2011，以%计算的值)通过引入隔热颗粒被减少至较小的程度，类似于总太阳能透射率TTS (根据ISO 13837:2008 ,v = 14 m/s; 以%计算的值)。
根据本发明所用的隔热膜A优选地具有大于1.2或大于1.25或大于1.30或大于1.35或大于1.40或大于1.45的TL/TTS的商。
隔热膜A可含有，例如 ITO、ATO、AZO、IZO、锑酸锌、锡掺杂氧化锌、硅掺杂氧化锌、镓掺杂氧化锌、钨酸盐例如LiWO3、NaWO3、CsWO3，六硼化镧或六硼化铈，作为隔热颗粒。
隔热颗粒优选地具有5-500 nm的平均直径。隔热颗粒在膜A中的比例可以是1-20%重量，优选2-10%重量。
膜A在所述层的层压之前的起始状态中的厚度是10-150 μm，优选20 – 120 μm。
在下文中，术语“起始状态”被理解为意指膜A和B在层压之前的状态，即是说仍处于分开的状态。
在所述层的层压之前的起始状态下以及在位于层压玻璃层压件的中间层堆叠之前，膜A和B可含有单一的增塑剂以及不同和相同组成的增塑剂二者的混合物。术语“不同的组成”指增塑剂的类型及其在混合物中的比例二者。膜A和膜B在层压后，即是说在成品层压玻璃后，优选地具有相同的增塑剂WA和WB。然而，在一个优选的变化中，膜A在其起始状态下不含有任何增塑剂，而在层压后含有增塑剂WB。
根据本发明所用的含增塑剂的膜B在所述层的层压之前在起始状态下含有至少16%重量，例如16.1-36.0%重量，优选22.0-32.0%重量和特别是26.0-30.0%重量的增塑剂。
根据本发明所用的膜A在所述层的层压之前在起始状态下可含有少于16%重量(例如15.9%重量)、少于12%重量、少于8%重量、少于6%重量、少于4%重量、少于3%重量、少于2%重量、少于1%重量的增塑剂或甚至没有增塑剂(0.0%重量)。具有低增塑剂含量的膜A优选地含有0.0-8%重量的增塑剂。
在根据本发明的方法中，膜A在所述层的层压之前的起始状态下具有不大于膜B的20%，优选15%的厚度，和优选不大于10%的厚度。
膜A在所述层的层压之前的起始状态下厚度为10-150 μm，优选20-120 μm，优选30-100 μm，优选40-80 μm和最优选50-70 μm。在层压玻璃中，膜的厚度通过从膜B转移增塑剂而增加。
膜A与膜B分开生产(例如挤压出)且或者完全无增塑剂或者具有小比例的增塑剂使得隔热颗粒的分散不受不利的影响。
膜B在起始状态的厚度为450-2500 μm，优选600-1000 μm，优选700-900 μm。至于使用多个膜B，对于其总厚度而言，情况也是如此。如果膜B在生产夹层之前被拉伸和/或另外地调整为弯曲形式的屏幕形状(例如档风玻璃)，则在层压时的指定厚度可再次减少至多20%。
至少一种薄的、隔热膜A是相对于根据本发明的层压玻璃层压件的玻璃表面定向。将膜A应用于两个玻璃表面也是可能的，以便提供具有层顺序玻璃/膜A/膜B/膜A/玻璃的层压玻璃层压件。在这里，膜A的修饰可以是相同或不同的。举例来说，膜A之一可具有隔热颗粒，而第二个膜A可具有导电结构，例如加热线、天线或具有光学功能的其它层。
在汽车玻璃窗的情况下，出于美观和稳定性原因，用密封剂密封层压玻璃层压件的边缘是不优选的。这增加这样的玻璃窗易受边缘缺陷形成的影响，例如各层彼此的分离(分层)或达到直至层压件的边缘的IR-吸收层的腐蚀或化学改性。
在根据本发明的方法中，具有低增塑剂含量的膜A可定制切割和布置，以使其在层压玻璃层压件中不达到远至层压件边缘的各处。特别是，与至少一块玻璃片比较，膜A可以在边缘区域小至少1 mm，以使膜B在该边缘区域与至少一块玻璃片直接接触。
此外，薄膜A，其在起始状态具有低增塑剂含量或甚至无增塑剂含量，可在插入玻璃/膜夹层之前进行穿孔，使得其可具有任何几何图案的开口，例如通道、孔或狭缝。
因此膜A可具有至少一个开口，使得膜B借助这个开口与承载膜A的玻璃片直接接触。在粘性结合形成成品层压玻璃后，在起始状态具有较高增塑剂含量的膜B在这些点上粘性结合到玻璃片而不间断。特别是，开口可因此在层压玻璃点获得，否则在所述开口后面的传感器元件、光学元件和/或天线元件的功能将会被隔热层阻碍。
根据本发明所用的膜A和B含有聚乙烯醇缩醛，其由聚乙烯醇或乙烯-乙烯醇共聚物的缩醛化生产。
所述膜可含有聚乙烯醇缩醛，各自具有不同的聚乙烯醇含量、缩醛化程度、残余乙酸酯含量、乙烯比例、分子量和/或缩醛基团的醛的不同链长度。
特别是，用于生产聚乙烯醇缩醛的醛或酮基化合物可以是线性或分支的(即是说“正”或“异”型)，含有2-10个碳原子，其导致对应的线性或分支的缩醛基团。因此聚乙烯醇缩醛被称为“聚乙烯醇(异)缩醛”或“聚乙烯醇(正)缩醛”。
根据本发明所用的聚乙烯醇(正)缩醛特别是由至少一种聚乙烯醇与一种或多种含有2-10个碳原子的脂族非分支酮基化合物的反应产生。为此，优选地使用正丁醛。
用于在膜A或B中生产聚乙烯醇缩醛的聚乙烯醇或乙烯-乙烯醇共聚物可以是相同的或不同的，纯的或不同聚合度或水解度的聚乙烯醇或乙烯-乙烯醇共聚物的混合物。
在膜A或B中的聚乙烯醇缩醛的聚乙烯乙酸酯含量可通过使用皂化至适当程度的聚乙烯醇或乙烯-乙烯醇共聚物来设定。聚乙烯醇缩醛的极性受到聚乙烯乙酸酯含量的影响，从而增塑剂相容性和各层的机械强度也变化。进行聚乙烯醇或乙烯-乙烯醇共聚物与一些醛或酮基化合物的混合物的缩醛化也是可能的。
膜A或B优选地含有具有基于各层(相同或者不同)为0.1-20 mol%，优选0.5-3 mol%，或5-8 mol%比例的聚乙烯乙酸酯基团的聚乙烯醇缩醛。
膜A (在起始状态具有较低的增塑剂含量)所用的聚乙烯醇缩醛PA的聚乙烯醇含量可为6-26%重量，8-24%重量，10-22%重量，12-21%重量，14-20%重量，16-19%重量并优选16-21%重量或10-16%重量。
膜B (其在起始状态更富含增塑剂)所用的聚乙烯醇缩醛PB的聚乙烯醇含量可为14-26%重量，16-24%重量，17-23%重量并优选为18-21%重量。
膜A或B优选地含有非交联的聚乙烯醇缩醛。使用交联聚乙烯醇缩醛也是可能的。用于交联聚乙烯醇缩醛的方法描述于例如EP 1527107 B1和WO 2004/063231 A1 (含有羧基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。
根据本发明所用的膜A和/或B可含有作为增塑剂的一种或多种选自以下化合物：
- 多价脂族或芳族酸的酯，例如己二酸二烷基酯，例如己二酸二己基酯、己二酸二辛基酯、己基己二酸环己基酯、己二酸庚基酯和己二酸壬基酯的混合物、己二酸二异壬基酯、己二酸庚基壬基酯，和己二酸与含有脂环族酯醇或酯醇的醚化合物的酯，癸二酸二烷基酯，例如癸二酸二丁基酯，且还有癸二酸与含有脂环族酯醇或酯醇的醚化合物的酯，邻苯二甲酸的酯，例如邻苯二甲酸丁基苄基酯或双-2-丁氧基乙基邻苯二甲酸酯。
- 多价脂族或芳族醇或含有一个或多个非分支或分支的脂族或芳族取代基的低聚醚二醇的酯或醚，例如甘油、二甘醇、三甘醇或四甘醇与线性或分支脂族或脂环族羧酸的酯；后一类的实例包括二乙二醇-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/或一缩二丙二醇苯甲酸酯。
- 与脂族或芳族酯醇的磷酸酯，例如三(2-乙基己基)磷酸酯(TOF)、磷酸三乙基酯、二苯基-2-乙基己基磷酸酯，和/或磷酸三甲苯酯。
- 柠檬酸、琥珀酸和/或富马酸的酯。
按照定义，增塑剂是具有高沸点的有机液体。为此理由，也可使用具有沸点超过120℃的其它类型的有机溶剂作为增塑剂。
其中增塑剂WA存在于起始状态的膜A的变体膜A，并且还有膜B，特别优选地含有作为增塑剂的1,2-环己烷二甲酸二异壬基酯(DINCH)或二缩三乙二醇-双-2-乙基己酸酯(3GO或3G8)。
此外，膜A和B可含有另外的添加剂，例如余量的水、UV吸收剂、抗氧化剂、粘性调节剂，荧光增白剂或荧光添加剂、稳定剂、着色剂、加工助剂、有机纳米颗粒、热解硅酸和/或表面活性物质。特别是，膜B可包含作为粘性调节剂的0.001-0.1%重量的羧酸碱金属盐和/或碱土金属盐。
为避免隔热颗粒的腐蚀，膜A优选地包含少于150 ppm的氯离子和/或硝酸根离子和/或硫酸根离子。
因此膜A的氯化物含量可少于150 ppm，优选少于100 ppm，和特别是少于50 ppm。在理想的情况下，膜A的氯化物含量为少于10 ppm或甚至是0 ppm。
膜A的硝酸根含量可任选地少于150 ppm，优选地少于100 ppm，和特别是少于50 ppm。在理想的情况下，膜A的硝酸根含量为少于10 ppm或甚至是0 ppm。
另外任选地，膜A的硫酸根含量可以是少于150 ppm，优选地少于100 ppm，和特别是少于50 ppm。在理想的情况下，膜A的硫酸根含量为少于10 ppm或甚至是0 ppm。
膜A另外可包含大于0 ppm的镁离子。镁含量优选地大于5 ppm，特别优选地为10 ppm， 特别是5-20 ppm。
本发明也涉及用于生产所述隔热层压玻璃层压件的方法，其中膜A布置于玻璃片上，然后由至少一个膜B覆盖，然后施加第二块玻璃片。
或者，可能将膜B布置在玻璃片上，然后用至少一个膜A覆盖，并施加第二块玻璃片。当然，也可能先使膜A和膜B在一起，然后将这些共同地布置在玻璃片上。
可能根据本发明，先通过升高温度将膜A熔融在玻璃片的整个区域上或局部，然后用膜B将其覆盖。或者，膜A和B可共同地布置在两块玻璃片之间并在升高的温度下熔融。
生产层压玻璃的层压步骤优选地以使得膜A和B布置在两块玻璃片之间并将如此生产的分层体在升高的温度以及增压或减压下压制以形成层压件的方式进行。
为了层压分层体，可在之前采用和不采用预层压件生产的情况下，采用本领域技术人员熟悉的方法。
在从约10至15巴的升高的压力和从100至145℃的温度下，将称为高压釡工艺的方法进行约2小时。真空袋或真空环的方法，例如根据EP 1 235 683 B1，在约200毫巴和130-145℃进行。
也可使用称为真空层压机的机器。这可由加热和抽空的室组成，其中层压玻璃窗可以在30-60分钟内层压。从0.01至300毫巴的减小的压力和从100至200℃，特别是130-160℃的温度，已在实践中证明其价值。
在最简单的情况中，为生产层压玻璃层压件，使膜A或B布置于玻璃片上，而另外的膜B或A同步或随后布置。然后应用第二块玻璃片并生产玻璃膜层压件。然后，借助于本领域技术人员已知的任何预层压方法可除去过多的空气。在此，各层也已先彼此轻微地粘性结合并粘性结合于玻璃上。
然后可使玻璃膜层压件经受高压釡处理。膜A优选地布置于第一块玻璃片上并用较厚的膜B覆盖，然后应用第二块玻璃片。该方法可以许多可预想的和在原则上可实行的变通方法进行。例如，膜A容易地从具有适当宽度的辊取出，而膜B已预先剪裁成要生产的层压玻璃的尺寸。这特别在挡风玻璃和其它汽车玻璃窗零件的情况下是有利的。在这种情况下，特别有利的是，在定制切割之前另外还拉伸较厚的膜B。这能够更经济地使用膜，或者对于其中膜B具有彩色色调的情况，允许其曲率适应上部片边缘。
在汽车领域中，特别是生产挡风玻璃的领域中，通常在上部区域使用称为墨带的膜。为此，膜A和B任一的上部可以与适当着色的聚合物熔体共同挤出，或者可能在膜A和B之一的多层系统中的某些区域有不同的着色。在本发明中，这可通过对膜A和B中的至少一个完全或部分着色来实现。
根据本发明，膜B因此可具有彩色色调，其特别是已经在现有工艺步骤中适应挡风玻璃的几何形状。
膜B具有楔形的厚度分布也是可能的。即使采用膜A的平面平行的厚度分布，根据本发明的层压玻璃层压件也获得楔形厚度分布并可用于机动车辆的挡风玻璃用于HUD显示器。
在最简单的情况中，膜B为有或无墨带和有或无楔形厚度分布的可市售获得的PVB膜。具有纳米颗粒分散于其中用于IR保护的膜B也可作为有色膜使用。当然，膜B也可以是具有声学功能的膜，使得通过与膜A的组合获得进一步改进的隔音性能。当然，膜B也可已经结合了一些提及的功能。
薄膜A一般通过采用流延膜生产线挤出或以吹塑膜的形式生产。在此，表面粗糙度也可通过受控流隙或用流延膜法另外通过使用结构化的冷却辊生产。
此外，已经生产的膜可通过至少一对圆柱体之间的压纹过程凸印出规则的、非随机粗糙度。根据本发明所用的膜优选地在一侧表面结构具有Rz从0至25 μm，优选Rz从1至20 μm，特别优选Rz从3至15 μm和特别是Rz从4至12 μm的粗糙度。如果与玻璃片接触的膜A的侧面具有不大于其厚度的20%的表面粗糙度Rz，则是特别优选的。提供隔热涂层的表面在施用涂层之前优选地具有特别低的表面粗糙度。特别地，此处的粗糙度参数Ra为少于3 μm和Rz为少于5 μm。

Claims (15)

1. 一种隔热层压玻璃层压件，由两块玻璃片之间的含有聚乙烯醇缩醛PA和任选的至少一种增塑剂WA的至少一个膜A和含有聚乙烯醇缩醛PB和至少一种增塑剂WB的至少一个膜B组成，特征在于在每种情况下在层压之前
- 将少于16%重量的比例的增塑剂WA分散于膜A中，
- 将至少16%重量的比例的增塑剂WB分散于膜B中，和
- 将隔热颗粒分散于膜A中。
2. 依据权利要求1的隔热层压玻璃层压件，特征在于膜A的隔热颗粒含有至少一种选自以下的化合物：ITO、ATO、AZO、IZO、锑酸锌、锡掺杂氧化锌、硅掺杂氧化锌、镓掺杂氧化锌、LiWO3、NaWO3、CsWO3或六硼化镧。
3. 依据权利要求1或2的隔热层压玻璃层压件，特征在于所述隔热颗粒具有5-500 nm的平均直径。
4. 依据权利要求1-3的任一项的隔热层压玻璃层压件，特征在于所述膜A包含含有6-26%重量的比例的乙烯醇基团的聚乙烯醇缩醛PA和所述膜B包含含有14-26%重量的比例的乙烯醇基团的聚乙烯醇缩醛B。
5. 依据权利要求1-4的任一项的隔热层压玻璃层压件，特征在于所述膜B包含0.001-0.1%重量的羧酸的碱金属和/或碱土金属盐。
6. 依据权利要求1-5的任一项的隔热层压玻璃层压件，特征在于所述膜A具有比膜B更小的表面积。
7. 依据权利要求1-6的任一项的隔热层压玻璃层压件，特征在于所述膜A具有至少一个开口，使得所述膜B借助这个开口与承载膜A的玻璃片直接接触。
8. 依据权利要求1-7的任一项的隔热层压玻璃层压件，特征在于所述膜B由至少两个子膜B’和B’’组成，其具有不同的增塑剂含量。
9. 依据权利要求1-8的任一项的隔热层压玻璃层压件，特征在于所述膜B具有楔形的厚度分布。
10. 依据权利要求1-9的任一项的隔热层压玻璃层压件，特征在于所述膜B具有彩色区域。
11. 依据权利要求1-10的任一项的隔热层压玻璃层压件，特征在于膜A具有彩色区域。
12. 依据权利要求1-11的任一项的隔热层压玻璃层压件，特征在于所述膜A具有1-150 μm的厚度。
13. 依据权利要求1-12的任一项的隔热层压玻璃层压件，特征在于膜A具有少于150 ppm氯离子和/或硝酸根离子和/或硫酸根离子。
14. 依据权利要求1-13的任一项的隔热层压玻璃层压件，特征在于膜A具有大于0 ppm的镁离子。
15. 一种生产依据权利要求1-12的任一项的层压玻璃层压件的方法，特征在于所述膜A布置于玻璃片上，然后由至少一个膜B覆盖，然后施加第二块玻璃片。
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