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CN1842414A - 利用硬质夹层的装饰层压安全玻璃及其制备方法 - Google Patents

利用硬质夹层的装饰层压安全玻璃及其制备方法 Download PDF

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CN1842414A
CN1842414A CN200480022546.1A CN200480022546A CN1842414A CN 1842414 A CN1842414 A CN 1842414A CN 200480022546 A CN200480022546 A CN 200480022546A CN 1842414 A CN1842414 A CN 1842414A
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sheet
image
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R·L·史密斯
H·A·埃尔沃基
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EIDP Inc
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EI Du Pont de Nemours and Co
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/10009—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets
    • B32B17/10018—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets comprising only one glass sheet
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
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    • B32B17/10807—Making laminated safety glass or glazing; Apparatus therefor
    • B32B17/10899—Making laminated safety glass or glazing; Apparatus therefor by introducing interlayers of synthetic resin
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Abstract

本发明是一种包括带有印刷图象的硬质夹层的装饰玻璃层压材料，所述图象被印刷在至少一个夹层表面上；以及一种制备该材料的方法。

Description

利用硬质夹层的装饰层压安全玻璃及其制备方法
本申请要求2003年8月7日提交的美国临时申请No 60/493,258的权益。
发明领域
本发明涉及利用硬质夹层的装饰层压安全玻璃及其制备方法。
发明背景
层压安全玻璃由通过吸收能量的塑料夹层典型地是聚乙烯缩丁醛(PVB)粘接的两层玻璃组成。层压安全玻璃用于汽车挡风玻璃以及建筑物装饰玻璃。建筑师频繁应用玻璃于许多需要的用途如扶手、隔墙、地板、门和高架螺栓固定玻璃。采用增塑PVB作夹层的层压安全玻璃，一般不符合这些应用的强度或支柱玻璃破损(post glass breakage)技术要求。专门设计的离聚物乙烯/甲基丙烯酸共聚物(得自杜邦公司)，形成硬质的、比惯用PVB夹层更硬挺且更韧性的夹层材料。利用更硬挺且更韧性夹层的层压安全玻璃，具有这些需要的建筑应用所要求的强度和支柱，玻璃破损技术规格。
另外，已经发现，专门设计的离聚物乙烯/甲基丙烯酸共聚物夹层展示出，与惯用PVB夹层相比，改进得多的边缘稳定性。这种改进了的边缘稳定性，为层压玻璃(具有离聚物乙烯/甲基丙烯酸共聚物夹层)应用于传统层压玻璃(具有，例如，PVB夹层)不能应用的领域创造了条件，如淋浴间门和户外敞缘应用。在许多这些上述应用(扶手、隔墙、地板、门、高架螺栓固定玻璃和淋浴间门)中，理想的是在层压安全玻璃中具有装饰图象。
制造层压装饰玻璃的方法公开在WO 217154 A1、DE 29706880、US 4968553、US 5914178、EP 1129844 A1和DE 20100717中。这些装饰层压材料应用PVB，PVB/PET/PVB复合材料，或EVA(乙烯/醋酸乙烯共聚物)作为夹层。虽然所得装饰安全玻璃层压材料可以符合建筑安全规范，但是这些层压材料在诸如上文所列的需求应用中表现不佳。
另外，许多此类参考文献公开了经丝网印刷法制造装饰层压玻璃的方法(DE 29706880、US 4968553、US 5914178、EP 1129844 A1和DE 20100717)。丝网印刷图象于夹层上，是一种制造装饰层压安全玻璃的非常费时且昂贵的方法。喷墨技术有高的适应性，并且任何数字图象均能印刷在基材上。采用喷墨技术在用于层压安全玻璃的软质夹层(PVB和聚氨酯)上进行印刷已经公开在WO 0218154中。直接在PVB上喷墨印刷的几个缺点有：所有PVB夹层均有粗表面图案(Rz30-60μm)，这种粗表面图案的存在使空气能在层压过程中选出，如US5455103所述；这种粗表面图案能影响图象的斑点和分辨率方面的质量；另外，例如，聚乙烯缩丁醛是一种粘弹性聚合物，它能使带图象的夹层的尺寸稳定性差。
从专门设计的离聚物乙烯/甲基丙烯酸共聚物得到的夹层，相对于其它惯用夹层而言，是硬挺的，并且能够具有改善的尺寸稳定性，例如，相对于PVB而言。然而，申请人发现，在硬挺聚合物材料上印刷的一个问题是，硬挺聚合物完全不适合于具有准备好可供应用的印刷机和油墨的惯用印刷工艺。申请人发现，采用惯用喷墨印刷机在惯用离聚物夹层上进行的喷墨印刷工艺也有问题，因为离聚物乙烯/甲基丙烯酸共聚物没有软质得足以喂入经过许多惯用喷墨印刷机。
发明概述
一方面，本发明是一种将图象喷墨印刷到硬质热塑性夹层上的方法，所述方法包括的步骤有：将硬质夹层片材喂入经过喷墨印刷机，和喷墨印刷图象到所述片材上，其中夹层的储能杨氏模量，在0.3Hz和25℃下，为50～1,000MPa(兆帕)，按照ASTM D 5026-95a测定。
另一方面，本发明是一种在夹层片材的至少一个表面上带有图象的热塑性夹层片材，将图象印刷到所述片材上通过包括下述步骤的方法进行，硬质夹层片材喂入经过喷墨印刷机，和喷墨印刷图象到所述片材上，其中夹层的储能杨氏模量，在0.3Hz和25℃下，为50～1,000MPa(兆帕)，按照ASTM D 5026-95a测定。
又另一方面，本发明是一种包括在其间置有硬质带图象的夹层片材的至少两个玻璃片材的装饰玻璃层压材料，其中得到带图象夹层的方法包括的步骤有：(1)“喷墨”印刷着色油墨到夹层片材的至少一个表面上，所述夹层片材是硬质乙烯/甲基丙烯酸共聚物离聚物，其厚度小于或等于约0.38mm，其中所述夹层的储能杨氏模量，在0.3Hz和25℃下，为50～1,000MPa(兆帕)，按照ASTM D 5026-95a测定，从而得到带图象的夹层片材；和(2)将带图象的夹层片材层压在透明材料片材之间，得到装饰层压材料。
另一方面，本发明是一种在夹层片材的至少一个表面上带有图象的热塑性夹层片材，其中带图象的夹层的储能杨氏模量，在0.3Hz和25℃下，为50～1,000MPa(兆帕)，按照ASTM D 5026-95a测定。
又另一方面，本发明是一种包括在夹层片材的至少一个表面上带有图象的硬质夹层片材的装饰层压材料，其中所述夹层的储能杨氏模量，在0.3Hz和25℃下，为50～1,000MPa(兆帕)，按照ASTM D 5026-95a测定。
发明详述
在一个实施方案中，本发明是一种带图象的装饰硬质夹层。适用于实施本发明的硬质夹层优选具有的储能杨氏模量，在0.3Hz和25℃下，为50～1,000MPa(兆帕)，按照ASTM D 5026-95a测定。其它惯用夹层材料能够适于作为用于喷墨印刷的基材，但是应用硬质夹层材料具有多项优点。
硬质硬挺夹层，例如基于专门设计的离聚物乙烯/甲基丙烯酸共聚物或硬挺(低增塑的)PVB，利于使用光滑得多的表面图案以得到在层压过程中可接受的排气，原因在于，该表面图案与硬质夹层在一起不发生迅速破坏。例如，用于层压惯用增塑(软质)PVB的理想Rz范围为30～60μm，而用于硬质夹层的可接受Rz范围为5～15μm。用于离聚物夹层的光滑表面图案产生的印制图象，与直接印在PVB上的图象相比，具有较高的分辨率和较少的斑点。
相对于诸如软质PVB的其它惯用软质夹层材料而言，硬质夹层的较高模量，能够产生具有与较软质材料相比改进的尺寸稳定性的夹层。改进的尺寸稳定性能够改进带图象产品的图象稳定性，和使整个工艺就图象的伸长或收缩而言更可靠并且更有再现性。
得到带图象的硬质夹层的在硬质夹层上的印刷能够采用水基或溶剂基油墨，和采用惯用印刷工艺如丝网印刷或喷墨印刷来完成，然后将带图象的硬质夹层层压在两层玻璃或其它透明材料之间。在硬质聚合物印刷基材上的传统印刷方法之采用并不是惯用的，其原因乃是应用专门印刷油墨、印刷设备和印刷程序来得到良好质量的图象之技术条件。
在优选实施方案中，将图象印刷到硬质夹层上，采用装有按要求滴落(drop)的压电印刷头(print head)的喷墨印刷机如Spectra或Xaar，并且选择喷墨印刷机，使得夹层保持在床式支持体上。
夹层能够是任何清洁、透明、硬质的，能够以粘合方式结合到玻璃上的热塑性材料。所述夹层，例如，能够是含有30份以下增塑剂的PVB片材，或者离聚物夹层。优选所述夹层是离聚物乙烯/(甲基)丙烯酸共聚物，该片材的表面糙度(Rz)为5～15μm，夹层总厚度为0.38～2.29mm。所述夹层能够是单一夹层片材，或者，结合的几层夹层的组合，提供复合夹层。如果单一片材，夹层印刷基材片材优选为60mil(1.524mm)或更低，使惯用喷墨印刷设备能够适应高模量材料。更优选单一硬质夹层印刷基材片材为0.38mm或更低。能优选较薄的片材，原因在于，现在，与适应高模量(硬质)材料的较厚片材的可得惯用印刷设备相比，更多惯用印刷设备能适应具有高模量的印刷基材材料的较薄片材。
本文所用术语“乙烯/(甲基)丙烯酸”是一种简写形式的术语，它代表包含或者乙烯和丙烯酸单元或者乙烯和(甲基)丙烯酸单元的共聚物。离聚物通常称为部分中和的乙烯/(甲基)丙烯酸共聚物。按照实施本发明用于印刷的适宜夹层，能够通过采用专门设计的乙烯/丙烯酸共聚物离聚物来得到，所述离聚物，例如，市购自杜邦公司。
在另一个实施方案中，本发明是一种复合的带图象的夹层，该夹层能够通过一种包括下述步骤的方法得到，即，将贮能杨氏模量在0.3Hz和25℃下为50～1,000MPa，按照ASTM D 5026-95a测定，和有限厚度小于或等于约0.38mm的薄基材薄膜，喂入经过惯用喷墨印刷机，并且喷墨印刷图象到基材薄膜表面上，和然后使带图象的薄薄膜与第二热塑性夹层材料片材层压。复合印刷夹层优选厚度为约0.40～约2.29mm。其它片材厚度能够变化，但是应该至少0.025mm厚。其它片材能够是空白的、带印刷图象的或彩色的，能够是透明的、半透明的、不透明的，或者否则能是目视不同于印刷基材的。在优选实施方案中，能够将薄的印刷基材与较厚的(≥0.76mm)，例如，离聚物乙烯/甲基丙烯酸共聚物薄膜或片材层压，从而获得所要求的成品层压材料结构性能。带图象的夹层片材与较厚的聚合物片材的层压，产生在夹层上压印图象的且具有较厚夹层性能的产品。
其它片材能够是任何能以粘合方式与印刷离聚物薄膜结合的热塑性夹层材料。例如，较厚的薄膜能够是：乙烯共聚物和/或三元聚合物如乙烯/丙烯酸或乙烯/丙烯酸烷基酯共聚物和乙烯/丙烯酸/丙烯酸烷基酯三元共聚物；聚缩醛；聚乙烯缩丁醛；聚氨酯；聚氯乙烯或聚酯。
虽然一些印刷机能够适应高达约60mil(1.52mm)厚度的硬质压片片材，但是对于大多数其它印刷机而言，能够优选使用较薄的片材。优选薄基材薄膜的厚度为约0.025mm至约1.52mm。更优选，印刷基材的厚度为约0.1mm至约0.40mm。最优选，印刷基材的厚度为约0.25mm至约0.38mm。优选较厚薄膜片材具有补充薄薄膜厚度的厚度，以使夹层片材总厚度为约0.38mm至约2.29mm。更优选总厚度为约0.60mm至约1.75mm。最优选夹层总厚度为约1.14mm至约1.55mm。
本发明层压材料能够应用于任何应用惯用(即，非装饰)层压玻璃的领域。然而，除了作为安全玻璃的惯常应用以外，本发明层压材料还能用作装饰制品如眺望窗、装饰柜台顶面、图表艺术品、带图象的商店铺面窗、公司标识显示、广告媒体、和/或任何需要带图象透明层压材料的其它应用。对本发明而言的装饰图象是任何按照本文所述方法印刷到基材表面上的图象。图象可以是绘画的、逐字逐句的、摄制的、插图的、抽象设计的、单一色泽和/或色泽的任何组合(对本发明而言其除外黑色和白色)或各种类型图象的任何组合。
实施本发明所用的优选油墨是提供具有图象质量、光牢度和耐气候性的满意组合的印刷图象者。另外，并合本发明带图象的夹层的层压材料，应该具有在将应用它的各种领域中可接受的粘合性能。由于在本发明中用于印刷的聚合物夹层基材的特性，以及安全玻璃粘合性的技术要求，选择适宜油墨不是没有问题。适用于本发明实施的油墨也必须与基材相容，以便得到满意结果。
可用于压电工艺的印刷头可得自，例如，Epson，Seiko-Epson，Spectra，XAAR和XAAR-Hitachi。可用于热喷墨印刷的印刷头可得自，例如，Hewlett-Packard and Canon。适用于连续滴落印刷的印刷头可得自，例如Iris和Video。
在适用于本发明实施的油墨系统中任选包括连接料树脂。能够优选连接料树脂以改进油墨和层压材料基材的粘合性。适用于本发明实施的适宜连接料能够包括，例如，聚乙烯基吡咯烷酮/醋酸乙烯(PVP/VA)，聚乙烯基吡咯烷酮(PVP)和PUR。连接料树脂混合物也能应用于本发明实施中。通常已知的其它连接料能够用于本发明。
本发明层压材料能够在各种建筑用途中作为建筑构件应用，例如，窗玻璃、结构支架、墙、楼梯、扶手、隔墙、地板、天花板和门(包括淋浴间门)。本发明层压材料能够用于地面运输交通工具中，例如，汽车，对于本发明来说，包括，卡车，搬运车，赛车(SUV)，公共汽车和小轿车；摩托车；农用车；建筑用车；用于挖掘的车；火车，包括，例如，地铁车箱，市郊旅客列车，高架火车，客车和货车。本发明层压材料能够用于空中运输交通工具，例如，飞机，包括大型客机，非大型飞机，军用飞机，小型飞机，喷气式飞机，直升机，无人驾驶(自动操纵)飞机和遥控导航飞机。本发明导压材料能够用于水路运输交通工具，例如，机动船，帆船，远洋班轮，军舰和潜艇。本发明层压材料在交通工具中能够用作，例如，挡风玻璃，侧窗，内或外光罩，机(船、车)体板，地板，顶材料如遮日/月光篷顶，仪表盘罩。本发明层压材料也能够用于其它用途中，例如，家俱，包括桌面，橱柜，写字台面，餐具架或书架；画框；标志；广告牌；辅面窗；装饰品；房间或办公室装饰附件。本发明层压材料能够用于下述的不是全部也是大多数的用途中，即，玻璃和/或玻璃层压材料是有用的和理想的用途，其原因在于，在夹层上显示的图象的功能用途，以及，或者，替代地，原因是在夹层上显示的图象的非功能用途。
实施例
现给出以下实施例举例说明本发明。无意用这些实施例以任何方式限制本发明范围。
试验方法
表面糙度，Rz，按照ISO-R468所述从10处的平均糙度来确定，以微米为单位表示。表面糙度采用Mahr Federal(Providence，RI)表面分析仪测定。
层压：采用喷墨印刷机将图象印刷到15mil(0.38mm)厚的夹层表面上。在层压之前，将片材层以75℃烘箱干燥最少16hr至0.2％以下水含量。为层压，将15mil透明夹层层置于带图象的表面上。多层结构经脱气(借助于真空胎或者夹辊法)然后采用标准层压条件在热压罐内成型。
实施例1
采用Epson 3000印刷机将黄色单色图案印刷到0.38mm厚离聚物乙烯/甲基丙烯酸共聚物夹层上。所用油墨如下表所示。如上文所述层压印刷夹层。
  分散体   丙烯酸系聚合物颜料黄120二丙二醇单甲醚
  连接料   Khrumbhaar 1717
  溶剂   二丙二醇甲基醚醋酸酯
  DPnP
实施例2
印刷黄色单色图案和层压均如实施例1所述。所用油墨如下表所示。
  分散体   丙烯酸系聚合物颜料黄120二丙二醇单甲醚
  连接料   Khrumbhaar 3107
  溶剂   二丙二醇甲基醚醋酸酯
  DPnP
实施例3
印刷黄色单色图案和层压均如实施例1所述。所用油墨如下表所示。
  分散体   丙烯酸系聚合物颜料黄120二丙二醇单甲醚
  连接料   Khrumbhaar 1728
  溶剂   二丙二醇甲基醚醋酸酯
  DPnP
实施例4
印刷黄色单色图案和层压均如实施例1所述。所用油墨如下表所示。
  分散体   丙烯酸系聚合物颜料黄120二丙二醇单甲醚
  连接料   Laropal 80
  溶剂   二丙二醇甲基醚醋酸酯
  DPnP
实施例5
印刷黄色单色图案和层压均如实施例1所述。所用油墨如下表所示。
  分散体   丙烯酸系聚合物颜料黄120二丙二醇单甲醚
  连接料   Laropal 81
  溶剂   二丙二醇甲基醚醋酸酯
  DPnP
实施例6
印刷黄色单色图案和层压均如实施例1所述。所用油墨如下表所示。
  分散体   丙烯酸系聚合物颜料黄120二丙二醇单甲醚
  连接料   Laropal A101
  溶剂   二丙二醇甲基醚醋酸酯
  DPnP
实施例7
采用#6棒在JV3印刷机上将SunJet油墨，紫外线固化油墨，市购自Sun Chemical，涂布在60mil厚乙烯酸共聚物离聚物基材表面上。然后，涂敷过的基材以16英尺/分钟的速度通过UV固化站(得自Fusion UV Systems公司)，采用每线性英寸300瓦的UV灯。发现，油墨瞬间干燥，层压粘合良好。

Claims (21)

1.一种制备具有层压材料粘合强度至少约1000psi的装饰层压材料的方法，所述方法包括下述步骤：(1)将着色油墨喷墨印刷到夹层片材的至少一个表面上，其中夹层厚度为60mil(1.524mm)或更低，储能杨氏模量，在0.3Hz和25℃下，为约100MPa(兆帕)至约1,000MPa，按照ASTM D 5026-95a测定，得到带图象的夹层片材；和(2)将带图象的夹层片材层压在透明材料片材之间，得到装饰层压材料；其中颜料包括至少一种选自下述的颜料，即，PY139，PY120，PY155，PY14，PY110，PY128，PY180，PY95，PY93，PY19/PR202，PR122，PB15：4，PB15：3，和PB17。
2.权利要求1的方法，其中所述硬质夹层包括或者乙烯和甲基丙烯酸或者乙烯和丙烯酸的共聚物离聚物。
3.权利要求2的方法，其中所述带图象的夹层厚度小于或等于约0.38mm，其中使带图象的夹层与一个或多个另外的夹层片材层压，得到总厚度约0.40mm至约2.29mm的复合夹层。
4.权利要求3的方法，其中所述其它夹层包括选自下述聚合物的热塑性聚合物：PVB、PET、PUR、PC、PVC、乙烯/(甲基)丙烯酸共聚物离聚物和乙烯/(甲基)丙烯酸/丙烯酸烷基酯三元共聚物。
5.权利要求4的方法，其中采用按要求滴落(DOD)的喷墨印刷工艺印刷所述图象。
6.权利要求5的方法，其中所述DOD工艺是压电工艺。
7.权利要求6的方法，其中所述DOD工艺是热喷墨印刷工艺。
8.权利要求7的方法，其中采用连续滴落喷墨印刷工艺印刷所述图象。
9.按照权利要求1的方法得到的装饰层压材料，其具有至少1000psi的压缩剪切强度。
10.权利要求9的层压材料，其中所述带图象的夹层与至少一种其它夹层的至少一个另外的片材层压，以生产带图象的复合夹层，其中至少一个另外的夹层片材的厚度足以使复合夹层的总厚度为约0.40mm至约2.29mm，且其中带图象的复合夹层进一步与至少一个玻璃片材层压。
11.一种将图象印刷到硬质热塑性夹层基材上的方法，该方法包括将至少一种油墨印刷到该热塑性基材表面上的步骤，其中印刷到热塑性基材上的至少一种油墨包括紫外线固化油墨，且其中所述夹层具有的贮能杨氏模量，在0.3Hz和25℃下，为约100MPa(兆帕)至约1,000MPa，按照ASTM D 5026-95a测定，从而得到带图象的夹层片材。
12.权利要求11的方法，其中所述印刷方法或者是喷墨印刷或者是丝网印刷。
13.一种在夹层片材的至少一个表面上带有图象的热塑性夹层片材，其中带图象的夹层的贮能杨氏模量，在0.3Hz和25℃下，为50～1,000MPa(兆帕)，按照ASTM D 5026-95a测定。
14.一种装饰层压材料，包含在夹层片材的至少一个表面上带有图象的硬质夹层片材，其中夹层的贮能杨氏模量，在0.3Hz和25℃下，为50～1,000MPa(兆帕)，按照ASTM D 5026-95a测定。
15.权利要求14的层压材料，其中所述层压材料包括至少一个玻璃片材。
16.权利要求15的层压材料，其中所述层压材料包括至少两个玻璃片材。
17.权利要求16的层压材料，其中所述带图象的夹层的厚度为60mil(1.524mm)或更少。
18.权利要求17的层压材料，其中所述带图象的夹层的厚度为0.38mm或更少。
19.权利要求18的层压材料，其中所述夹层是复合夹层，后者包括带图象的夹层和至少一个另外的夹层片材，其中复合夹层的总厚度为约0.40mm至约2.29mm。
20.一种包含装饰层压材料的制品，所述装饰层压材料包括在夹层片材的至少一个表面上带有图象的硬质夹层片材，其中夹层的贮能杨氏模量，在0.3Hz和25℃下，为50～1,000MPa(兆帕)，按照ASTMD 5026-95a测定。
21.权利要求20的制品，其中所述制品是选自下述的制品：用于陆路、空中或水路运输的交通工具；建筑构件；家俱；画框；标志；广告牌；铺面窗；装饰品；以及装饰附件。
CN200480022546.1A 2003-08-07 2004-08-06 利用硬质夹层的装饰层压安全玻璃及其制备方法 Pending CN1842414A (zh)

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