CN102145557B - 在高透射率下具有控制漫射性能的层压玻璃的夹层复合结构及其制造方法 - Google Patents

在高透射率下具有控制漫射性能的层压玻璃的夹层复合结构及其制造方法 Download PDF

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CN102145557B
CN102145557B CN2010105512883A CN201010551288A CN102145557B CN 102145557 B CN102145557 B CN 102145557B CN 2010105512883 A CN2010105512883 A CN 2010105512883A CN 201010551288 A CN201010551288 A CN 201010551288A CN 102145557 B CN102145557 B CN 102145557B
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R·A·福吉尔
T·R·菲利普斯
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Dow Global Technologies LLC
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Abstract

公开了在高透射率下具有控制漫射性能的层压玻璃的夹层复合结构及其制造方法。还公开了一种半透明的夹层或由其获得的层压制品，其具有低透明度、高雾度和至少60％的光透射率，其中基本上再现了蚀刻或喷砂玻璃的美学质量。此外，本发明的层压制品提供层压安全玻璃的安全特性。此外，制造本发明半透明层压制品的方法可以消除与喷砂或刻蚀方法有关的安全和环境问题。

Description

在高透射率下具有控制漫射性能的层压玻璃的夹层复合结构及其制造方法
本申请是国际申请日为2003年5月2日、国际申请号为PCT/US03/13800、发明名称为“在高透射率下具有控制漫射性能的层压玻璃的夹层复合结构及其制造方法”的国际发明专利申请进入中国的中国专利申请的分案申请，该中国专利申请的申请号为03810051.7、发明名称为“在高透射率下具有控制漫射性能的层压玻璃的夹层复合结构及其制造方法”。
本申请要求2002年5月3日申请的美国临时申请US 60/380,070的优先权。
技术领域
本发明涉及层压安全玻璃。更具体地说，本发明涉及半透明的层压安全玻璃。
背景技术
例如，在制造以下层压结构中使用增塑的聚乙烯缩丁醛板(PVB)，如：包括汽车、摩托车、船和飞机在内的交通工具用风挡；房屋和建筑物；壳体和展示箱中的架子；及其它需要具有理想的结构强度的玻璃板制品。在许多应用中，理想的层压制品是透明且无色的。在其它的应用中，层压制品为半透明是理想的。在层压安全玻璃领域中，半透明的层压制品已知多年。
典型地，半透明的层压制品具有70％或更低的透射水平。然而，典型地，使用喷砂或蚀刻的玻璃来制备具有更高透射水平，例如80-90％透射率，以及光漫射性能高的半透明(translucent)或半透明(semi-transparent)层压制品。
喷砂是这样一种方法，即在来自喷砂装置的压力的推动下，通过用高速的砂粒、玻璃珠或相似的聚集体轰击玻璃的表面而使玻璃较不透明。蚀刻是这样一种方法，通过使用在玻璃表面上反应的化学物质如酸来降低该化学物质与玻璃表面接触的区域的透明度而将表面化学蚀刻。这些方法中的任何一种都可以在玻璃上形成粗糙的表面，从而造成入射光在玻璃的表面处散射或漫射(diffusion)。
虽然喷砂和蚀刻的方法可以形成不透明度从低到高的玻璃，同时光漫射和透射性能在建筑应用中提供美学的作用，但是因为操作蚀刻酸和/或来自形成的玻璃粉尘的矽肺病，所以这些方法本身是危险的。而且，任何在玻璃表面中形成缺陷的操作都造成当操作或冲击时可以导致玻璃破坏的应力，从而降低其安全性能。具有粗糙表面的玻璃遇到的另一个问题是，在玻璃上的褶皱中，沾染污垢的表面难以清洁。
典型地，市售白色夹层的透射水平非常低。实际上，市售白色夹层产品虽然使光通过，但不能使人通过夹层或通过由其制备的任何层压制品识别或辨别物体的形状。
理想的是提供通过层压制品识别物体的某种测量的半透明(translucent)或半透明(semi-transparent)玻璃层压制品，其中该层压制品具有喷砂或蚀刻玻璃的美学特性，同时具有标准透明安全玻璃层压制品的强度。
通过降低或消除与制造喷砂或蚀刻玻璃有关的安全性危险的方法获得这样一种具有美感的层压制品也是理想的。
发明内容
在一个方面中，本发明是一种含有粒径小于约10微米的着色剂颗粒的夹层组合物，其中该夹层：(1)具有约25％-90％的雾度，(2)使至少约60％的入射光透射过该夹层，和(3)具有至少20％的透明度。
在另一个方面中，本发明是一种包含至少2片玻璃和设置于其中的夹层的玻璃层压制品，其中该夹层：(1)含粒径小于约10微米的着色剂颗粒，其中该夹层：(1)具有约25％-90％的雾度，(2)使至少约60％的入射光透射过该夹层，和(3)具有至少20％的透明度。
在另一个方面中，本发明是一种用于制造适用于层压玻璃应用的PVB板的方法，该方法包括以下步骤：(a)以控制的速率向挤压机中供给着色剂；(b)共挤压聚乙烯缩丁醛树脂、着色剂、增塑剂及其它任选的添加剂；(c)使熔融的板组合物骤冷，从而获得适用于层压玻璃应用的尺寸稳定性的PVB板，其中该夹层：(1)具有约25％-约90％的雾度，(2)使至少约70％的入射光透射过该夹层，和(3)具有至少20％的透明度。
附图说明
图1是作为粒径函数的透射率-重质碳酸钙(CaCO3)浓度的曲线图。
图2是作为重质CaCO3浓度函数的透射率-粒径的曲线图。
图3是作为粒径函数的透明度-重质CaCO3浓度的曲线图。
图4是作为重质CaCO3浓度函数的透明度-粒径的曲线图。
图5是作为粒径函数的雾度-重质CaCO3浓度的曲线图。
图6是作为重质CaCO3浓度函数的雾度-粒径的曲线图。
发明详述
在一个实施方案中，本发明是一种含有着色剂颗粒的夹层组合物。本发明的夹层可以由适合于在玻璃层压制品中用作夹层材料的任何材料制造。例如，该夹层材料可以是酸共聚物或其盐，例如乙烯/甲基丙烯酸共聚物或其中和的型式(version)。夹层材料可以是聚氨酯聚合物、聚酯聚合物或聚乙烯缩丁醛(PVB)聚合物。优选地，该夹层材料含增塑的PVB聚合物。
可以根据任何已知方法在制造PVB板中通常使用的方法制备适合于在本发明的实践中使用的聚乙烯缩丁醛。例如，美国专利US3,153,009描述了一种适合于在本发明的实践中使用的工业制造PVB的方法。可以通过在5-100℃的温度下，在有酸或酸混合物的情况下，在水介质中通过将PVA与丁醛混合来制备在本发明的实践中使用的PVB树脂。
典型地，选择PVA与丁醛的比例以使PVB具有残留的羟基官能度，通常报道为聚乙烯醇的重量百分比。残留的羟基官能度可以根据在PVB中需要的性能而改变。在PVB树脂中获得所需残留重量百分比的聚乙烯醇所需的丁醛和PVA的相对数量对PVB制造领域的技术人员来说是显而易见的。在本发明的实践中，残留的羟基可以为约14-约30重量％。优选地，残留的聚乙烯醇为约15-约25重量％。更优选地，残留的聚乙烯醇为约15-约20重量％，最优选的，在本发明的实践中，PVB树脂具有约17-约19重量％的残留的聚乙烯醇。可以根据标准方法如ASTM D1396-92确定残留的聚乙烯醇的重量百分比。
本发明的PVB组合物含有着色剂。本发明的着色剂可以是与PVB组合物混合并且赋予PVB板颜色的任何材料。对于本发明而言，单数或复数形式的术语“着色剂”不但指黑色、绿色、红色、蓝色和黄色的着色剂或它们的各种组合，而且也指白色的着色剂和白色着色剂与其它着色剂的组合。术语“着色剂”还可以指“着色剂的混合物”。读者应该能够从使用该术语的上下文中辨别其适当的意义。只要颜色在本发明的PVB板中可以再现，则由适合于在本文中使用的着色剂赋予PVB板的颜色可以是在可见光谱中产生的任何颜色。在本发明的实践中使用的着色剂可以以固体形式、以溶液或以固/液分散体的方式加入到PVB组合物中。例如，为了容易加工，可以将液体形式的染料或颜料加入到PVB中。然而，应该指出，染料通常溶于树脂基体并将增加颜色，但无助于夹层的雾度。在本发明的实践中，要求至少一种着色剂是分散在夹层组合物中的固体颗粒。
在本发明特别优选的实施方案中，PVB组合物基本上由至少一种着色剂，即白色着色剂组成。正如上文所述的例外，白色着色剂优选以颗粒材料的形式加入。然而，可以通过本领域众所周知的方法，以浓缩物或以循环板材中组分的形式加入着色剂。已知或常规使用的任何白色着色剂都适合在本发明中使用。
优选地，白色着色剂选自硫酸钡(BaSO4)、硫酸镁(MgSO4)、氧化镁(MgO)、硅酸镁(MgSiO3)、二氧化钛(TiO2)、氧化锌(ZnO)、硫酸锌(ZnSO4)、氧化锑(SbxOy)(其中X为2或4，y为3-6)、磷酸钙(Ca3(PO4)2)、硫酸钙(CaSO4)或(CaCO3)或它们的混合物。
虽然对本发明的实践并非绝对关键，但就本发明PVB板或由此获得的层压制品的外观而言，着色剂的浓度是一个影响因素。图1、3和5说明了浓度与光透射率、透明度和雾度的关系。可以通过常规方法控制本发明夹层中着色剂的浓度以控制添加剂的浓度。例如，可以通过控制将着色剂计量到挤压机中的速率来控制与PVB树脂共同挤压的着色剂的浓度。
应该选择着色剂的浓度以使夹层或层压制品具有至少60％的入射光的光透射率。对于本发明而言，入射光是到达本发明夹层或层压制品表面的光。优选地，光透射率至少为约75％，更优选至少约80％，最优选至少约85％。可以通过任何用于这种确定的常规方法确定光透射率。例如，可以使用常规的分光光度计来确定本发明夹层透射过的光的百分比。
可以以小于约2.0wt％的浓度将着色剂加入到本发明的PVB组合物中。优选地，以约0.9-约1.8wt％的浓度加入着色剂。更优选地，着色剂的浓度为约0.6-约1.5wt％，最优选地为约0.3-约0.75wt％。如果其浓度低于约0.10wt％，则透明度过高而雾度过低。如果高于2.0wt％，则雾度过高而透明度过低。
然而，例如，取决于其它因素如粒径，在本发明的实践中加入的着色剂的浓度可以超出本文中公开的范围，而并不超出本文中设想的本发明的范围。关键因素是本发明层压制品中的PVB板具有高的光透射率，并具有赋予本发明层压制品基本上与蚀刻或喷砂玻璃板相同或相似的外观的透明度。
仔细的选择和/或操作着色剂的粒径可以控制板和得到的层压制品的透明度和漫射能力(diffusive power)。可以通过常规方法如使用适当尺寸的筛子来控制着色剂的粒径。或者，可以从着色剂的商业制造商处获得所需粒径的着色剂。图2、4和6说明了该粒径与光透射率、透明度和雾度的关系。
颗粒着色剂具有小于约10微米的中值粒径。优选地，着色剂的粒径为约2-约10微米，更优选地为约2.5-约8微米，最优选地为约3-约6微米。虽然不束缚于理论，但粒径与透明度之间的正比关系和粒径与雾度之间的反比关系是显然的。对于任何给定的重量％，着色剂颗粒越大，PVB板和得到的层压制品中的透明度越大且雾度越低。颗粒越小，板和得到的层压制品显示越低的透明度、越大的雾度和越大的漫射能力。
本发明夹层的透明度应该至少为20％。优选地，本发明夹层的透明度为约35％-约100％，更优选地为约45％-约95％，更加优选地为约50％-约90％，最优选地为约60％-约85％。
本发明夹层板的雾度与漫射能力有关。在本发明的夹层组合物中，当通过在仪器如雾度计上测量雾度％时，漫射能力优选为约25-约90％。更优选地，雾度％为约40-约85％，更加优选地为约50-约80％，最优选地为约55-75％。
本发明的一种PVB组合物含有增塑剂。本发明的增塑剂可以选自任何已知或在制造增塑PVB板组合物中通常使用的增塑剂。适合于在本文中使用的增塑剂可以是选自以下的增塑剂或增塑剂的混合物：通过脂肪族二醇与羧酸的化学反应获得的双酯，其包括聚醚二醇或聚醚多元醇的双酯；和通过多价羧酸和脂族醇获得的酯。本文中使用的优选增塑剂是通过三甘醇或四甘醇与具有6-10个碳原子的脂肪族羧酸的反应获得的双酯；和通过癸二酸与具有1-18个碳原子的脂族醇的反应获得的双酯。更优选地，增塑剂是三甘醇二(2-乙基己酸酯)(3GO)、四甘醇二-庚酸酯(4G7)或癸二酸二丁酯(DBS)。最优选的增塑剂是3GO。
为了获得增塑PVB板，增塑剂可以以任何所需的量加入。以树脂总的干重计，增塑剂可以以每100份(pph)树脂约5-约50的量加入。本文中使用的“干重”指的是干燥树脂，即已经从树脂中去掉水后树脂的重量。优选地，增塑剂存在的量为约20-约45pph，最优选的量为约32-约45pph。
可以使用“湿”法或“干”法进行增塑。当在本文中使用术语湿法时，其是这样一种方法，其中在将混合物送入挤压机之前或当将混合物送入挤压机时，将增塑剂与PVB树脂含水浆料和其它添加剂混合。在将增塑剂/PVB混合物送到挤压机中之前，该混合物的停留时间为2-24小时是优选的。例如，在美国专利US 3,153,009中描述了适合于在本文中使用的湿法。当在本文中使用时，干法是这样一种方法，其中在将混合物送入挤压机中之前或当将混合物送入挤压机中时，将增塑剂与干燥PVB树脂薄片混合。例如，在美国专利US 5,886,075中描述了适合于在本文中使用的干法。
在制备本发明的一种PVB组合物中含有表面活性剂。适合于在本文中使用的表面活性剂可以是任何已知在聚乙烯缩丁醛制造领域中有用的表面活性剂。例如，适合于在本文中使用的表面活性剂包括：十二烷基硫酸钠；十二烷基硫酸铵；二辛磺基琥珀酸钠；具有6-12个碳原子的全氟羧酸铵；芳基磺酸钠、氯化环戊二烯和马来酸酐的加成物；部分中和的聚甲基丙烯酸；烷基芳基磺酸盐；N-油基-N-甲基牛磺酸钠；烷基芳基聚醚磺酸钠；十二烷基硫酸三乙醇胺酯；十二烷基硫酸二乙基双环己基铵；仲烷基硫酸钠；硫酸化脂肪酸酯；硫酸化芳基醇等。优选的表面活性剂包括十二烷基硫酸钠、二辛磺基琥珀酸钠、椰油甲基氨基乙磺酸钠和癸基(硫代苯氧基)苯磺酸二钠盐。
在本发明的树脂组合物中可以含有任选的添加剂而不对PVB的立体异构产生影响。这种添加剂包括抗氧化剂、光稳定剂、粘合控制剂和/或表面张力控制剂以及其它的添加剂。
在另一个实施方案中，本发明是含本发明夹层板的层压制品。可以通过夹层与玻璃或塑料材料的任何组合而获得该层压制品。例如，本发明的层压制品可以由玻璃和本发明的夹层组成，或该层压制品可以由聚合材料和本发明的夹层组成，或该层压制品可以由玻璃和聚合材料的组合与本发明的夹层组成。适合与本发明夹层一起使用的聚合材料可以是已知适合于在诸如窗户或门这样的应用中使用的作为玻璃或安全玻璃代用品的任何聚合材料。合适的聚合物例如是聚碳酸酯；丙烯酸和/或丙烯酸酯聚合物和共聚物、甲基丙烯酸和/或甲基丙烯酸酯聚合物和共聚物；或聚酯可以是适合于在本文中使用的热塑性材料。优选地，层压制品是含至少2片玻璃与设置在其中的本发明夹层的层压制品。可以根据已知和常规的作法装配本发明的层压制品。例如，可以通过包括以下步骤的方法装配本发明的层压制品：在热量和压力下将玻璃板、本发明的夹层和另一玻璃板铺设到一起，从而形成层压制品。各种提高层压制品质量的方法是已知而且常规的，例如在层叠之前使夹层的表面变粗糙以提供通道，从而使空气在层压的过程中从层压制品中逸出。
在另一个实施方案中，本发明是制备半透明PVB板的方法。可以通过共同挤压PVB与白色的着色剂和增塑剂而获得本发明的半透明PVB板。至少部分取决于包含多少增塑剂，挤压可以在约175-约245℃的温度下进行。可以将挤压的半透明板骤冷或冷却至等于或低于约40℃但高于约10℃的温度。优选地，将板冷却至低于约25℃的温度，更优选地，将板冷却至低于约20℃的温度，最优选地，将板冷却至低于约15℃的温度。为了储存，可以轧制并堆叠挤压的板。在任何情况下，都可以使用本发明的板来制造上述层压制品。
具体实施方式
实施例
提供以下实施例和对比例来进一步说明本发明。这些实施例既不打算以任何方式限制本发明的范围，它们也不应该用来以任何与如要求保护和/或如本文中所述的本发明不一致的方式来限定权利要求或说明书。
试验方法
根据ASTM D1003确定雾度，将雾度定义为偏离入射大于2.5度的透射光的百分比。将透明度定义为偏离入射光小于2.5度的透射光的百分比。使用Byk-Gardner Haze-gardPlus(HG Plus)或HunterLab Ultrascan球状分光光度计(Ultrascan)获得雾度/透明度测量数据。
对比例C1
使用中值粒径为3.5微米的CaCO3制备半透明的白色PVB板。以控制的方式将PVB干燥树脂、四甘醇二-庚酸酯(4G7)和碳酸钙送到标称210℃的双螺杆挤压机中。在冷却辊上骤冷所得的30密耳厚的板。最终的组合物名义上含70.3wt.％的PVB、27.8wt.％的4G7和1.9wt.％的碳酸钙。应该以以下步骤制备层压制品：将该板放在两片透明玻璃之间，使一组压料辊通过进行脱气，然后用135℃和200psi的同步循环(hold cycle)在空气高压釜中高压加热20分钟。在HG Plus上测量了透明度、雾度和光透射率％。表1中给出了结果。
实施例1-33
在转鼓(tumbler)上“干”混干燥PVB树脂、4G7增塑剂和碳酸钙4小时，然后将它们送入标称温度为210℃单螺杆挤压机中并挤压。将得到的熔体挤压成30密耳厚的板。与C1一样制备层压制品。在HGPlus上测量了透明度、雾度和光透射率％。表1中给出了结果。
表1
Figure BSA00000353170400091
表1(续)
Figure BSA00000353170400101

Claims (27)

1.一种夹层组合物，其含粒径小于10微米的着色剂颗粒，其中该夹层：(1)具有25％-90％的雾度，(2)使至少60％的入射光透射过该夹层，和(3)具有至少20％的透明度；其中透明度、雾度和光透射率使用HG PLUS测量。
2.一种夹层组合物，其含粒径小于10微米的着色剂颗粒，其中该夹层：(1)具有25％-90％的雾度，(2)使至少60％的入射光透射过该夹层，和(3)具有至少20％的透明度；其中透明度、雾度和光透射率使用HG PLUS测量，其中以夹层的总重量计，着色剂的浓度小于2.0重量％。
3.权利要求1或2的组合物，其中该着色剂的粒径为2-10微米。
4.权利要求3的组合物，其中该着色剂的粒径为2.5-8微米。
5.权利要求4的组合物，其中该着色剂的粒径为3-6微米。
6.权利要求1的组合物，其中以夹层的总重量计，着色剂的浓度小于2.0重量％。
7.权利要求2或6的组合物，其中该着色剂的浓度为0.9-1.8重量％。
8.权利要求7的组合物，其中该着色剂的浓度为0.6-1.5重量％。
9.权利要求8的组合物，其中该着色剂的浓度为0.3-0.75重量％。
10.权利要求9的组合物，其中该着色剂选自BaSO4、MgSiO3、MgSO4、MgO、ZnO、ZnSO4、SbxOy，其中X为2或4，y为3-6、TiO2、Ca3(PO4)2、CaSO4、CaCO3或者它们的任何混合物。
11.权利要求10的组合物，其中该着色剂选自TiO2、CaCO3或它们的混合物。
12.权利要求11的组合物，其中该着色剂是CaCO3。
13.一种玻璃层压制品，其包含至少两片玻璃和位于其中的夹层组合物，其中该夹层：(1)含粒径小于10微米的着色剂颗粒，(2)具有25％-90％的雾度，(3)使至少60％的入射光透射过该夹层，和(4)具有至少20％的透明度；其中透明度、雾度和光透射率使用HG PLUS测量。
14.权利要求13的层压制品，其中该夹层组合物含有粒径为2-10微米的着色剂。
15.权利要求14的层压制品，其中该夹层组合物含有粒径为2.5-8微米的着色剂。
16.权利要求15的层压制品，其中该夹层组合物含有粒径为3-6微米的着色剂。
17.权利要求13的层压制品，其中雾度％为40-85％。
18.权利要求17的层压制品，其中雾度％为50-80％。
19.权利要求18的层压制品，其中雾度％为55-75％。
20.权利要求13的层压制品，其中该层压制品透射过至少75％的入射光。
21.权利要求20的层压制品，其中该层压制品透射过至少80％的入射光。
22.权利要求21的层压制品，其中该层压制品透射过至少85％的入射光。
23.权利要求13的层压制品，其中该透明度为35％-100％。
24.权利要求23的层压制品，其中该透明度为45％-95％。
25.权利要求24的层压制品，其中该透明度为50％-90％。
26.权利要求25的层压制品，其中该透明度为60％-85％。
27.一种制造适合用于层压玻璃应用的PVB板的方法，该方法包括以下步骤：(a)以控制的速率向挤压机中供给着色剂；(b)共同挤压聚乙烯缩丁醛树脂、着色剂、增塑剂及其它任选的添加剂；(c)使熔融的板组合物骤冷，从而获得具有适合用于层压玻璃应用的尺寸稳定性的PVB板，其中该PVB板：(1)具有25％-90％的雾度，(2)使至少60％的入射光透射过该PVB板，和(3)具有至少20％的透明度；其中透明度、雾度和光透射率使用HG PLUS测量。
CN2010105512883A 2002-05-03 2003-05-02 在高透射率下具有控制漫射性能的层压玻璃的夹层复合结构及其制造方法 Expired - Lifetime CN102145557B (zh)

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