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CN112088090B - 具有不对称表面粗糙度的夹层膜 - Google Patents

具有不对称表面粗糙度的夹层膜 Download PDF

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CN112088090B
CN112088090B CN201980032480.0A CN201980032480A CN112088090B CN 112088090 B CN112088090 B CN 112088090B CN 201980032480 A CN201980032480 A CN 201980032480A CN 112088090 B CN112088090 B CN 112088090B
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CN112088090A (zh
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J·D·施罗特
I·拉扎尔
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Kuraray Europe GmbH
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Abstract

本发明涉及基于增塑聚乙烯醇缩醛或离聚物的膜，其具有第一表面和第二表面以及彼此相对的第一边缘和第二边缘，其特征在于至少所述第一表面设置有从第一边缘到第二边缘Rv下降5%至75%的表面粗糙度梯度。制造包括具有夹层膜的两个透明片材的层合件的方法。

Description

具有不对称表面粗糙度的夹层膜
背景技术
本发明涉及用于层合装配玻璃的基于增塑聚乙烯醇缩醛或离聚物的夹层膜及其制造方法，所述夹层膜具有不对称的表面粗糙度。
层合安全玻璃通常由通过基于增塑聚乙烯醇缩醛，优选聚乙烯醇缩丁醛（PVB）的胶粘膜组合的两块玻璃板组成。层合安全玻璃特别用作机动车辆中的挡风玻璃。
为了制造这种层合装配玻璃，将增塑PVB膜夹在两块玻璃片材之间，并在除去夹带空气之后，再施加热和/或压力。为了除去空气和降低处理过程中膜的粘性，膜的表面设置有一定的粗糙度。可以通过膜的挤出工艺和/或通过随后的压花步骤来控制粗糙度。
PVB膜的挤出和压花步骤在本领域中是公知的，例如在EP 0185863B1中作为熔体破裂工艺和在WO 2014021459A1中作为压花工艺所公开的那样。
机动车辆中的挡风玻璃通常是弧形的。为了顺应玻璃的形状，将矩形夹层膜拉伸直到它们具有与玻璃片材相同的形状。如果挡风玻璃上设置有遮光带，即在挡风玻璃的上部设置有着色区，则该技术特别有用。
在该拉伸过程中，膜的粗糙度特性和厚度在表面上从均匀分布变为不对称分布。例如，在其整个表面上具有均匀表面粗糙度的膜在拉伸后将具有在膜的拉伸侧粗糙度较低的粗糙度梯度。表面上粗糙度的不对称分布导致在层合过程中膜的不同脱气和熔融行为。行为上的差异可能导致拉伸侧与未拉伸侧的脱气性能不同，并最终导致挡风玻璃生产中的损失率较高。
因此，本发明旨在提供一种膜，其在拉伸后具有在其表面上基本均匀的表面粗糙度分布。
发明内容
本发明的目的是基于增塑聚乙烯醇缩醛或离聚物的膜，其具有第一表面和第二表面以及彼此相对的第一边缘和第二边缘，其特征在于至少所述第一表面设置有从第一边缘到第二边缘Rv下降5%至75%的表面粗糙度梯度。
在第一实施方案中，至少所述第一表面设置有从第一边缘到第二边缘Rz下降5%至75%的表面粗糙度梯度。
在第二实施方案中，至少所述第一表面设置有从第一边缘到第二边缘的Rsm梯度为5%至75%的通道。
在第三实施方案中，所述膜设置有从第一边缘到第二边缘或从第二边缘到第一边缘的梯度为5%至50%的厚度。
通过测量在第一边缘和第二边缘的相同区域处，例如在距各个边缘5或10 mm距离处的相应表面粗糙度Rv、Rz、Rsm和/或厚度并计算比率来确定表面特性或厚度的梯度。
表面特性Rv、Rz、Rsm的梯度可以彼此独立地为从第一边缘到第二边缘在10%和65%之间或在15%和60%之间，或在20%和55%之间或在25%和50%之间，或在30%和45%之间或在35%和40%之间。
厚度梯度可以在10%和45%之间或在15%和40%之间，或在20%和35%之间或在25%和30%之间。
根据本发明的膜可以以实施方案的任何组合提供。在进一步的变体中，所述膜包括至少两个具有不同tg的增塑聚乙烯醇缩醛或离聚物的层。
此外，所述膜可以至少在一个边缘处设置有着色区。所述膜可以在第一边缘处和/或在第二边缘处设置有着色区，但是具有着色区的膜可以在3或4个边缘处设置有这样的着色区。着色区可用于保护汽车驾驶员免受阳光照射。由于在大多数现代汽车中，挡风玻璃胶合到车身上，因此这样的着色区进一步保护胶粘剂免受UV辐射。
可以在膜的一个或两个表面上设置表面特性Rv、Rz、Rsm的所有梯度。优选的是，对两个表面都设置相同的表面特性Rv、Rz、Rsm和相应的梯度。为了防止光学干扰，可能有益的是，对膜的表面设置不同的表面特性Rv、Rz、Rsm和/或相应的梯度。例如，表面可以设置有至少一个表面特性Rv、Rz、Rsm，这些表面特性在表面之间具有5-15%的差异，但是具有相同的梯度。在替代方案中，表面的表面特性Rv、Rz、Rs在一个边缘上可以是相同的，但是相应的梯度在表面之间可以具有5-15%的差异。
具体实施方式
优选地，本发明的膜在第一边缘上设置有9-35微米的表面粗糙度Rv。
此外，本发明的膜可以进一步在第一边缘上设置有15-55微米的表面粗糙度Rz。
进一步地，本发明的膜可以在第一边缘上设置有间距Rsm为100-800微米的通道。在其变体中，Rsm可以在200和350微米之间或在450和600微米之间。
本发明的膜可以进一步在第一边缘上设置有200-2500微米、优选500-900微米的厚度。
根据DIN EN ISO 4287和DIN ISO 4288测量膜的表面特性Rz、Rv和/或Rsm。用于测量表面粗糙度的测量装置必须满足EN ISO 3274。所用的轮廓滤波器必须符合DIN EN ISO11562。
表面特性Rz和Rv和Rsm可以是随机的或非随机的。随机表面粗糙度可以通过在熔体破裂条件下将增塑聚乙烯醇缩醛或离聚物挤出成膜和/或用具有随机表面的压花辊压花来实现。非随机表面粗糙度可以通过在一个或两个压花辊之间对已经制成的膜进行压花来实现。已经制成的膜可以通过挤出来制造，任选在熔体破裂条件下进行以引入基础/精细粗糙度。一种替代方法是流延成膜。
可以以使得膜的两侧具有不同的表面粗糙度Rv、Rz和Rsm的方式进行压花。这可以例如通过不同的压花工具或压花工具和/或压辊的温度来实现。
膜的两个表面上的通道可以彼此共享70-90°或5-45°的角度。在另一方面，在膜的至少一个表面上的通道与挤出方向或膜的最宽宽度方向成5-45°、优选35-45°的角度。
通道的间距Rsm在膜的表面上可以相同或不同，其中表面之间5%的偏差被认为是相同的。通道的间距可以为100-800微米、优选250-500微米。
膜的组成
根据本发明的膜可以基于离聚物或增塑聚乙烯醇缩醛。术语“基于”是指膜完全或大部分由离聚物或增塑聚乙烯醇缩醛组成，但可以包含以小于5重量%的少量添加的其它添加剂，如UV稳定剂、抗氧化剂和抗粘剂或增粘剂。这样的添加剂是层合装配玻璃领域的技术人员众所周知的。
用于本发明的聚乙烯醇缩醛可以以已知的方式通过将水解的聚乙烯基酯缩醛化来制备。例如，甲醛、乙醛、丙醛、丁醛等等，优选丁醛用作醛。
优选地，聚乙烯醇缩醛是聚乙烯醇缩丁醛（PVB）树脂。聚乙烯醇缩醛可以含有10至25重量%、优选17至23重量%和特别优选19至21重量%的乙烯醇基团和/或0至20重量%、优选0.5至2.5重量%的乙酸酯基团。
在另一个方法变体中，根据WO 2004/063231A1，用多元醛（特别是戊二醛）和氧代羧酸（特别是乙醛酸）部分交联的聚乙烯醇缩醛用作聚合物。这样的交联聚乙烯醇缩醛的粘度比类似的非交联聚乙烯醇缩醛的粘度高10%至50%。
优选将膜的水含量调节到0.15至0.8重量%、特别是0.3至0.5重量%。
在夹层膜领域中已知的所有增塑剂，特别是多元酸、多元醇或低聚醚二醇的酯，例如己二酸酯、癸二酸酯或邻苯二甲酸酯，特别是己二酸二正己酯、癸二酸二丁酯、邻苯二甲酸二辛酯、二乙二醇、三乙二醇或四乙二醇与直链或支链脂族羧酸的酯和这些酯的混合物，在一方面适合作为部分缩醛化的聚乙烯醇的增塑剂。脂族二醇与长链脂族羧酸的酯，特别是三乙二醇与含有6至10个碳原子的脂族羧酸如2-乙基丁酸或正庚酸的酯，优选用作聚乙烯醇缩醛的标准增塑剂。特别优选使用选自己二酸二正己酯（DHA）、癸二酸二丁酯（DBS）、邻苯二甲酸二辛酯（DOP）、二乙二醇、三乙二醇或四乙二醇与直链或支链脂族羧酸的酯，特别是三乙二醇-双-2-乙基丁酸酯（3GH）、三乙二醇-双-正庚酸酯（3G7）、三乙二醇-双-2-乙基己酸酯（3G8）、四乙二醇-双-正庚酸酯（4G7）的一种或多种增塑剂。
基于聚乙烯醇缩醛的膜优选含有基于100重量份的聚乙烯醇缩醛计25至45重量份和最优选30至40重量份的增塑剂。
术语“离聚物”是指在层合装配玻璃领域中已知的非聚乙烯醇缩醛聚合物。基于离聚物的膜可以商品名Sentryglass从Kuraray Europe GmbH商购获得。
本发明的方法
本发明的另一个目的是根据本发明制造包括具有夹层膜的两个透明片材的层合件的方法。在该方法中，所述两个透明片材优选为具有弧形（即具有与较短的第二边缘相对的较长的第一边缘）的玻璃片材。这样的层合件用于机动车辆的挡风玻璃和后窗玻璃（backlights）。
本发明方法的特征在于包含增塑聚乙烯醇缩醛或离聚物的膜具有第一表面和第二表面以及彼此相对的第一边缘和第二边缘，对所述膜设置具有从第一边缘到第二边缘Rv下降5%至75%的表面粗糙度梯度的第一表面，在所述膜的第一边缘处对所述膜进行机械拉伸，直到该梯度减小至少5%，然后将所述膜置于两个透明片材之间，并通过施加热和压力进行层合。
在该方法的一个变体中，所述膜进一步具有从第一边缘到第二边缘Rz下降5%至75%的表面粗糙度梯度，并且在所述膜的第一边缘处对所述膜进行机械拉伸，直到该梯度减小至少5%，然后将所述膜置于两个透明片材之间，并通过施加热和压力进行层合。
在该方法的另一个变体中，所述膜在至少所述第一表面上进一步具有从第一边缘到第二边缘的Rsm梯度为5%至75%的通道，并且在所述膜的第一边缘处对所述膜进行机械拉伸，直到该梯度减小至少5%，然后将所述膜置于两个透明片材之间，并通过施加热和压力进行层合。
在该方法的另一个变体中，所述膜进一步具有从第一边缘到第二边缘为5%至75%的厚度梯度，并且在所述膜的第一边缘处对所述膜进行机械拉伸，直到该梯度减小至少5%，然后将所述膜置于两个透明片材之间，并通过施加热和压力进行层合。
在该方法的另一个变体中，所述膜进一步具有从第二边缘到第一边缘为5%至75%的厚度梯度，并且在所述膜的第二边缘处对所述膜进行机械拉伸，直到该梯度减小至少5%，然后将所述膜置于两个透明片材之间，并通过施加热和压力进行层合。
本发明的方法可以用已经公开的膜的所有变体和实施方案来进行。
例如，如果膜设置有从第一边缘到第二边缘Rv下降10%至35%的表面粗糙度梯度，则可以在所述膜的第一边缘处进行机械拉伸，直到该梯度为小于10%、优选小于5%。可以沿着表面粗糙度Rz和Rsm和/或厚度进行同样的拉伸过程。
图1示例性地示出了拉伸过程及其对膜的表面粗糙度的影响。最初，矩形PVB膜设置有表面结构的梯度，第一边缘在膜的右侧，且第二边缘在膜的左侧。通过适当的压花辊将该表面结构和梯度压花到膜的第一表面中。然后，在一个边缘处拉伸膜直到梯度基本上消失。采用该程序，可以得到具有均匀的表面粗糙度的弧形膜。
在将透明片材和膜组合之后，通过施加热和压力来完成层合件。术语“热和压力”是指使用高压釜、真空袋或真空环（例如根据WO 03/033583）的公知的层合工艺。
根据本发明制成的膜可特别用于生产汽车中的挡风玻璃。
实施例
在层合测试过程中，发现在层合件的边缘处形成气泡的速率强烈取决于压花膜的表面粗糙度Rz。例如，由于在边缘处形成气泡，Rz为56微米的膜导致最终层合件的不合格率（failure rate）为28%。在相同的工艺条件下，具有42微米的压花深度Rz的膜导致仅为3%的不合格率。由此得出结论，不合格率强烈取决于Rv。
如果拉伸在整个宽度上具有60微米的均匀Rz的膜，则所得的膜显示出在该膜的一个边缘上为56微米的Rz和在该膜的另一个边缘上为42微米的Rz。因此，该拉伸过程产生在层合过程中表现良好的膜的第一侧和由于气泡形成而具有较高不合格率的第二侧。
本发明中所描述的方法通过提出使用在膜上具有表面粗糙度梯度的膜，预期了通过拉伸产生的Rz差异。该梯度的坡形与通过拉伸产生的梯度坡形相反，使得膜的两个边缘在拉伸后更均匀，因此降低了在边缘处形成气泡的风险。
例如，在175℃下对PVB膜进行压花，其中压花辊以使得辊的一侧施加20巴且辊的另一侧施加10巴的方式压在膜上。这产生了其中膜的第一边缘显示出60微米的Rz且第二边缘显示出46微米的Rz的膜。在拉伸后，该膜在膜的整个宽度上，即也在第一边缘和第二边缘上具有42微米的均匀Rz。
这样的膜显示出与具有42微米的均匀Rz的未拉伸膜相同的低气泡形成和低不合格率。

Claims (5)

1.制造包括具有夹层膜的两个透明片材的层合件的方法，其特征在于，包含增塑聚乙烯醇缩醛或离聚物的膜具有第一表面和第二表面以及彼此相对的第一边缘和第二边缘，对所述膜设置具有从所述第一边缘到所述第二边缘Rv下降5％至75％的表面粗糙度梯度的第一表面，在所述膜的第一边缘处对所述膜进行机械拉伸，直到所述梯度减小至少5％，然后将所述膜置于两个透明片材之间，并通过施加热和压力进行层合，其中根据DINENISO4287和DINISO4288测量Rv，其中用于测量表面粗糙度的测量装置满足ENISO3274并且所用的轮廓滤波器符合DINENISO11562，其中“离聚物”是指在层合装配玻璃领域中已知的非聚乙烯醇缩醛聚合物。
2.根据权利要求1所述的方法，其特征在于，所述膜进一步具有从所述第一边缘到所述第二边缘Rz下降5％至75％的表面粗糙度梯度，并且在所述膜的第一边缘处对所述膜进行机械拉伸，直到所述梯度减小至少5％，然后将所述膜置于两个透明片材之间，并通过施加热和压力进行层合，其中根据DINENISO4287和DINISO4288测量Rz，其中用于测量表面粗糙度的测量装置满足ENISO3274并且所用的轮廓滤波器符合DINENISO11562。
3.根据权利要求1或2所述的方法，其特征在于，所述膜在至少所述第一表面上进一步具有从所述第一边缘到所述第二边缘的Rsm梯度为5％至75％的通道，并且在所述膜的第一边缘处对所述膜进行机械拉伸，直到所述梯度减小至少5％，然后将所述膜置于两个透明片材之间，并通过施加热和压力进行层合，其中根据DINENISO4287和DINISO4288测量Rsm，其中用于测量表面粗糙度的测量装置满足ENISO3274并且所用的轮廓滤波器符合DINENISO11562。
4.根据权利要求1至2中任一项所述的方法，其特征在于，所述膜进一步具有从所述第一边缘到所述第二边缘为5％至75％的厚度梯度，并且在所述膜的第一边缘处对所述膜进行机械拉伸，直到所述梯度减小至少5％，然后将所述膜置于两个透明片材之间，并通过施加热和压力进行层合。
5.根据权利要求1至2中任一项所述的方法，其特征在于，所述膜进一步具有从所述第二边缘到所述第一边缘为5％至75％的厚度梯度，并且在所述膜的第二边缘处对所述膜进行机械拉伸，直到所述梯度减小至少5％，然后将所述膜置于两个透明片材之间，并通过施加热和压力进行层合。
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