CN1652926A - 耐冲击性优良的层合结构及其制造方法 - Google Patents

耐冲击性优良的层合结构及其制造方法 Download PDF

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CN1652926A
CN1652926A CNA038104814A CN03810481A CN1652926A CN 1652926 A CN1652926 A CN 1652926A CN A038104814 A CNA038104814 A CN A038104814A CN 03810481 A CN03810481 A CN 03810481A CN 1652926 A CN1652926 A CN 1652926A
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goods
pvb
sodium
plasticizer
stiffening
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B·C·王
C·A·史密斯
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EIDP Inc
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EI Du Pont de Nemours and Co
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Abstract

本发明是一种层合制品，包含至少三层增塑聚乙烯醇缩丁醛(PVB)片材，其中所述层合材料的至少一层是硬挺PVB片材，和至少两层是软质PVB片材。本发明的层合制品用来提供为免除发生于汽车、建筑物和窗户风挡之类的损坏而增加的防护，所述这些损坏乃是由于将它们暴露于诸如飓风级风中、狂风所推进的飞砂走石的冲击，或者故意的对包含本发明的层合材料的窗户风挡之类的冲击。

Description

耐冲击性优良的层合结构及其制造方法
本申请要求2002年5月16日提交的美国临时申请No.60/381,494的权益。
                      发明背景
增塑聚乙烯醇缩丁醛片材(PVB)被用于制造层合结构，例如，包括汽车、摩托车、船支和飞机等的交通工具的风档，家用和建筑用材，柜橱和陈列箱的档板材料以及玻璃片材形式的结构强度和层合稳定性均理想的其它制品。对于本申请而言，层合稳定性指的是保持玻璃与PVB处于粘合状态的能力和/或在严酷或甚至极端环境下保持层合材料层基本在一起的能力。在一些特殊用途中，需要或者高度优选耐冲击性和层合稳定性均优良。例如，能够优选，在住宅和其它建筑中应用的层合材料经受得住飓风、龙卷风和/或暴风雨雪情况下普遍存在的严酷条件。
已知各种采用PVB形成的玻璃层合材料，并叙述在美国专利4,297,262、美国专利4,230,771和英国专利828,381中。一般说，使PVB塑化，以便具有低的硬挺性并且在受冲击时容易变形，这对于汽车风档来说是一种优良的性能，在这种用途中涉及人的冲击，需要在猛烈碰撞时隔离乘客以及因此减少伤亡。但是，这些性能既不是承受高应力的建筑物窗户也不是会经受过度作用力的汽车和卡车侧风档所需要的性能。硬挺性低和弹性高这些方面的性能会限制在下列情况下的性能，即，当在层合材料的玻璃破损之后层合材料必须提供抗流动塑性时，例如，在玻璃层合材料经受高的风力，和/或，在发生飓风时经受飞砂走石冲击的时候，或者，在通过过度攻击重复冲击窗户而侵入交通工具或结构之处。诸如风档等传统PVB层合材料或标准建筑层合玻璃，在所设计的评价在飓风条件下层合材料性能的试验中均表现拙劣，例如Dade County，满载(FL)飓风风档系统试验方案，其中有严酷的冲击试验，继之以在破碎层合材料上进行的压力循环试验。
传统PVB层合材料，在经受压力负荷和循环试验时，最后均能在飓风中损坏。损坏的原因能够是，或者聚合物夹层发生了大的变形，能够使层合材料脱出风档框，和/或者，破损玻璃碎片的作用，最终切割到PVB层并使空气压或其它威胁因素渗透过用层合材料防护的结构。传统层合材料，采用借助过度攻击而增加通过层合材料的通路的手段，也能较容易地被穿透。应用比标准层合材料厚的PVB层得到较大的硬挺度和抗切断性，是不切实际的、因为所需要的夹层过厚还有费用方面的原因。类似地，难以应用传统厚度的较硬挺的PVB，因为硬挺PVB较难加工，并且制造产率损失相当大。
较硬挺玻璃层合材料的制造已采用除了PVB之外的，诸如聚氨酯和热塑性共聚物和包括PVB的所有这些与聚酯薄膜和聚碳酸酯薄膜相组合，的夹层。例如，Bolton等的美国专利No.4,663,228叙述了采用离聚物树脂形成韧性玻璃层合材料。
与日俱增的一种需求是用作抗暴风雨雪和飓风威胁的，特别是在沿海区域的建筑物窗户的玻璃层合材料。还有一种需求是抗流动塑性的机动交通工具的侧风档。需要这些玻璃层合材料具有改善的韧度和稳定性。它们还必须易于被制造，并且具有良好的光学性能，包括颜色或清晰度。
理想的是采用韧性的、稳定的、易于制造的和具有良好光学性能的PVB层合材料来满足这些需要。本发明的这些以及其它目的对于读者来说会是显而易见的。
                        发明概述
以一方面而论，本发明是一种层合制品，其包含至少两层Tg为约32℃～约35℃的软质增塑聚乙烯醇缩丁醛(PVB)片材，和还包含至少一层硬挺PVB夹层片材，其中硬挺夹层：(i)Tg为约35℃～约60℃，(ii)位于至少两层软质PVB之间，和(iii)包含漂白化合物。
                        发明详述
在一个实施方案中，本发明是一种包含至少三层增塑聚乙烯醇缩丁醛(PVB)片材的层合制品，其中层合材料的至少一层是硬挺PVB材料，和至少两层是软质PVB片材。本发明的层合制品用来提供为免除发生于汽车、建筑物和窗户风档之类的损坏而增加的防护，所述这些损坏乃是由于将其暴露于诸如飓风级风中，狂风所推进的飞砂走石的冲击、或者故意的对包含本发明的层合材料的窗户风档之类的冲击。
在实施本发明中，软质PVB和硬挺PVB两者均能按照PVB制造领域已知的惯用方法制造。例如，一种生产适用于本发明实施的软质PVB组合物的方法叙述在美国专利No.3,153,009中，在此引入作为参考。增塑PVB片材能够通过本领域熟知的方法制备。美国专利4,276,351叙述了一种制备增塑PVB片材的方法。美国专利No.4,696,971也叙述了一种制造增塑PVB片材的方法。美国专利5,886,075叙述了制造增塑PVB片材的还有的另一种方法。
本发明的层合材料包含至少两层或区软质PVB。作为用于本发明的术语，软质PVB指的是玻璃化转变温度(Tg)为约32℃～约42℃的PVB片材，Tg按照动态力学分析ASTM D4065(DMA)进行测定，采用tanδ(在1Hz下的相移)数值作为指示。
除了至少两层软质PVB片材之外，本发明的层合材料包含至少一层硬挺PVB树脂。作为在本文中使用的术语，PVB硬挺层是Tg为约42℃以上至约60℃的PVB片材，Tg按照DMA ASTM D4065进行测定，采用tanδ(在1Hz下的相移)数值作为指出。优选Tg为约45℃～约57℃，更优选47℃～约57℃，最优选约50℃～约55℃。
PVB片材的Tg能够取决于在组合物中增塑剂的含量。本发明的软质PVB片材每100份采用至少约30份(pph)增塑剂来增塑。优选本发明软质PVB采用约30～约50pph增塑，以所述树脂的总干重为基准计。本文所用的“干重”指的是干燥树脂的重量，即，在将水从未增塑的PVB树脂除去之后的树脂重量。更优选增塑剂存在量为约30～约45pph，和最优选存在量为约32～约45pph。优选，本发明硬挺PVB片材包含的增塑剂量为约5～约30pph，更优选增塑剂含量为约15～约30pph。甚至更优选增塑剂含量为约18～约28pph，和最优选约18～约22pph。
本发明增塑剂能够选自在制造增塑PVB片材组合物中已知的或惯用的任何物质。例如，本发明中适用的增塑剂能够是选自下述的增塑剂或增塑剂混合物：自脂族二醇与羧酸的化学反应制得的二酯，包括聚醚二醇或聚醚多元醇的二酯；和自多元羧酸和脂族醇制得的酯。为了方便起见，在叙述本发明的片材组合物时，在本文中能将增塑剂混合物称作“增塑剂”。即，在本文中所用的词“增塑剂”的单数形式，能够表示在给定片材组合物中或者使用一种增塑剂或者使用两种或两种以上增塑剂的混合物。对于熟悉本领域的读者显而易见所意欲的应用。在本发明中应用的优选增塑剂是通过三甘醇或四甘醇与含有6～10个碳原子的脂族羧酸的反应制得的二酯；和自癸二酸与含有1～18个碳原子的脂族醇的反应制得的二酯。更优选增塑剂是或者四甘醇二正庚酸酯(4GT)、三甘醇二-2-乙基己酸酯(3GO)或癸二酸二丁酯(DBS)。最优选增塑剂是3GO。
本发明硬挺PVB树脂组合物的挤出，相对于挤出软质PVB所需要的温度而言，需要高的挤出温度。例如，采用约30pph以下的增塑剂增塑的PVB树脂能够在约225℃～约245℃下挤出。优选所述树脂能够在约227℃～约245℃下挤出。更优选所述树脂能够在约228℃～约242℃下挤出，和最优选约230℃～约240℃。软质PVB能够在约175℃～约225℃下挤出。
在特别优选的实施方案中，在本发明层合材料中应用的PVB夹层的YID色泽为12以下。由于加工硬挺PVB必须使用较高的挤出温度，这能导致PVB片材颜色不理想，所以本发明组合物包含至少一种PVB漂白化合物。本发明的PVB漂白化合物(漂白化合物)是能够减少或消除PVB树脂颜色的任何化合物，相对于采用相同或相似工艺处理的另外的相同树脂而言，只是后者不含漂白化合物。通过漂白化合物所显示的漂白作用方式对于本发明来说没有严格要求。例如，用于实施本发明的漂白化合物能够是直接与存在于PVB树脂组合物中的成色化合物(色体)反应的化合物，或者能够生成直接与色体反应的化合物的化合物。漂白化合物能够是能够就地分解生成能够与存在于PVB树脂组合物中的色体反应的分解产物的化合物。在实施本发明中的漂白化合物能够是抑制色体形成的化合物。本发明的漂白化合物包括，例如，无机亚硫酸氢盐如亚硫酸氢钠或亚硫酸氢钾，有机亚硫酸氢盐如亚硫酸氢四甲铵，以及结构或功能类似的化合物。漂白化合物还包括磺基丁二酸酯如磺基丁二酸二烷基酯。例如，本发明能够包括磺基丁二酸二辛酯钠(DOSS)作为漂白化合物。
本发明的漂白化合物的含量能够为任何有效的有限量。用于本发明目的的有效量是，能够降低包含漂白化合物的PVB树脂的色泽的任何数量，相对于相同或基本相似的不包含漂白化合物的PVB树脂组合物而言。替代地，在缺少比较数据时，有效量是能够降低PVB树脂色泽至12 YID以下的任何数量。优选YID为约10以下，更优选为约8以下，和最优选为约6以下。树脂的色泽测定能够按照任何惯用或标准作法来进行。
漂白化合物的含量能够为约0.01～约0.85pph，以在制备PVB中所用的聚乙烯醇(PVA)的重量为基准计。优选漂白化合物的存在量为约0.05～约0.80pph，更优选为约0.10～约0.75pph，和最优选为约0.15～约0.70pph。在降低PVB片材色泽是所考虑的一个重要问题时，漂白化合物的含量经常也是生产成本和可以因包含添加剂而受影响的其它性能的函数。
本发明包含表面活性剂。适用于本发明的表面活性剂能够是已知在聚乙烯醇缩丁醛制造领域中有用的任何表面活性剂。例如，适用于本发明的表面活性剂包括：月桂基硫酸钠、碱金属盐、月桂基硫酸铵、磺基丁二酸二辛酯钠、含有6～12个碳原子的全氟羧酸铵、芳基磺酸钠、氯代环戊二烯和马来酸酐的加合物、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、月桂基硫酸三乙醇胺、月桂基硫酸二乙基二环己基铵、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月桂基硫酸钠、磺基丁二酸二辛酯钠、椰油甲基氨基乙磺酸钠，和癸基(磺基苯氧基)苯磺酸二钠盐。
对于实施工艺条件的特定批次而言，能够包含任何有效量的表面活性剂。表面活性剂的含量能够为约0.01～约0.85pph，按重量计，以用于制备PVB的PVA的重量为基准计。优选表面活性剂的含量为约0.10～约0.80pph。更优选表面活性剂的含量为约0.15～约0.75pph。最优选表面活性剂的含量为约0.15～约0.70pph。
表面活性剂和PVB漂白化合物能够是相同的化合物。仅仅在表面活性剂也能起漂白化合物的作用时，漂白化合物是任选的。换句话说，在实施本发明中，认为漂白化合物是最重要的。例如，DOSS能够在本发明实施中用作表面活性剂。DOSS在本发明实施中也能是漂白化合物。在一个特别优选的实施方案中，DOSS能够作为表面活性剂和作为漂白化合物两者而包含在其中。在该实施方案中，任选应用除了DOSS之外的漂白化合物。
在制造片材时，在本发明的PVB树脂组合物中，能够任选包含抗氧剂，以便抑制PVB树脂和/或组分的氧化。按常规和市售已知优选的抗氧剂。最优选双酚抗氧剂，其令人惊异地更适用于制备低色泽PVB片材，特别是当使用3GO作为增塑剂时。双酚抗氧剂是可供应的并且能够大批地获得。适宜的双酚抗氧剂包括，例如2，2’-亚乙基双(4，6-二叔丁基酚)、4，4’-亚丁基-双(2-叔丁基-5-甲基苯酚)、2，2’-亚异丁基双(4，6-二甲基苯酚)，和2，2’-亚甲基双(6-叔丁基-4-甲基苯酚)。双酚抗氧剂能够例如以商品名ANOXTM29、LOWINOX22M46、LOWINOX44B25和LOWINOX22IB46市购。
抗氧剂能够以任何有效有限量包含在其中。优选抗氧剂含量为约0.01～约0.6％，以片材总重量为基准计。更优选抗氧剂存在量为约0.03～约0.3％，最优选其量为约0.05～约0.25％。
按常例已知用于PVB的、对从其制得的层合材料的冲击性能没有有害影响的普通辅助化合物，能够包含在本发明的树脂组合物中。这些添加剂包括：抗氧剂、着色剂、光稳定剂、特别是紫外光稳定剂/吸收剂，如TinuvinP、Tinuvin326和Tinuvin123。紫外光稳定剂能够通过吸收紫外光和防止紫外光对PVB有不良影响来稳定PVB组合物。能够加入粘性控制剂如羧酸的碱金属和碱土金属盐、无机酸的碱土金属盐，或这些盐的组合。在实施本发明中，应该注意，在汽车风档方面，粘性能够太高或太低，都应该进行控制，以便给机动车乘客最大保护免受抛击。在建筑和安全层合材料方面，理想的是使粘性最大，以便不发生自发脱层。
在还有的另一个实施方案中，层合制品能够得自本发明的PVB片材。在本领域中已熟知制造玻璃/PVB层合材料的方法，熟练的技术人员应当能够自现有要求专利保护的PVB片材制造层合材料。在本发明中提出专利保护的玻璃/PVB层合制品能够通过下述方法制得，例如，使PVB和玻璃的表面接触，然后在压热釜中从层合结构除去空气。能够将PVB表面打毛，以利于从层合材料除去空气。还已知其它方法并且按惯例应用。尽管在本发明中叙述了PVB/玻璃层合材料，但是PVB也能用作夹层材料，以便层合到诸如聚碳酸酯、聚酯和/或聚氨酯等其它材料上。
本发明的层合材料包含总厚度至少0.75mm的多层PVB。硬挺PVB夹层的厚度优选占整个夹层总厚度的约20％～约80％。更优选硬挺PVB夹层的厚度占总夹层厚度的约22％～约70％，和最优选占约25％～约60％。
在特别优选自实施方案中，将薄的硬挺PVB层与软质PVB层象本文所叙述的那样排列组合使用，令人惊异地提高了层合材料的耐冲击性，并且避免了采用较厚硬挺PVB层产生的过高的制造收率下降。本发明的硬挺PVB层厚度为约0.25～约10mm，优选硬挺PVB层的厚度为约0.35～约8mm。更优选厚度为约0.45～约6mm，最优选约0.50～约4mm。
实施例
提供如下实施例和比较例用来进一步举例说明本发明。没有以所述实施例用任何方式限制本发明范围的意图，也不应当将它们以任何与本文要求专利保护的和/或叙述的发明不一致的方式用来限定权利要求书或说明书。
在下述实施例和比较例中，耐冲击性以平均穿透能来表示。平均穿透能的测定方法包括，在室温(21±2℃)下，采用31.5kg(70lb)摆锤冲击器撞击固定在竖直框上的0.304m×0.305m的层合材料，所述冲击器装有76mm直径圆形突起物(外圆角)。本测定中所使用的摆锤装置与英国标准学会(British Standards Institute)的AU209，Part4所叙述的装置相似，只是冲击器重得很多。采用冲击器，在按照布鲁斯顿梯级法调节的抛出高度下，顺序冲击具有相同结构的层合材料组。如果圆形突起物在给定冲击器抛出高度下没有穿透一个层合材料，那么在组中的下一个层合材料的冲击器抛出高度就增加76mm(3英寸)。相反，如果圆形突起物在给定高度下穿透层合材料，那么在同一组中下一个层合材料的冲击器抛出高度就减少76mm(3英寸)。每组层合材料的平均穿透能是，穿透当时的层合材料50％所需要的冲击器的平均势能。平均穿透能是冲击器质量、重力加速度和冲击器的平均穿透高度之积。冲击器的平均穿透高度能够采用布鲁斯顿梯级统计学来计算，正如在Mary Gibbons Natrella的“实验统计学”(Experimental statistics)，National Bureau of Standards Handbook 91，Washington，D.C.pages 10-22至10-23所概述的。
在下文的所有实施例和比较例中，PVB夹层均含有50～100ppm钾，作为粘性控制添加剂。这种添加剂，在片材成形期间，以甲酸钾的形式加入到聚合物熔体中。
比较例C1
将每100份干燥PVB树脂含有35份3GO增塑剂(35pph 3GO)、厚度总计2.54mm的PVB夹层层合到两片2.3mm×30.5cm×30.5cm的、在软化水中洗涤并漂洗过的透明退火浮法玻璃之间。所述玻璃/PVB/玻璃组合按下述方法脱气：将其置于橡胶袋中，密封该橡胶袋，然后将该橡胶袋抽真空。在环境温度(约23℃)下抽真空脱气5min之后，将装有所述组合及其内容物的整个橡胶袋置于120℃烘箱中，同时保持真空。使橡胶袋和其内容物在烘箱中停留总计20min，此后从烘箱中取出橡胶袋，并拆除真空软管。把以相同方法制造的十一个层合材料用于冲击试验。这组层合材料的平均穿透能为333焦耳。
比较例C2
所制十一个层合材料具有与比较例C1相类似的结构，只是PVB夹层含有22pph 3GO。夹层总厚度为2.54mm。平均穿透能为383焦耳。
比较例C3
所制十一个层合材料具有与比较例C1相类似的结构，只是PVB夹层含有29pph 3GO。夹层总厚度为2.54mm。平均穿透能为330焦耳。
比较例C4
层合材料采用叠层PVB夹层来制造，这样两个含有20pph 3GO的0.51mm的层夹在两个含有35pph 3GO的0.76mm的层当中。PVB片材叠层层合在两块如比较例C1所述的2.3mm玻璃之间。所有组合夹层的厚度为2.54mm。夹层的平均增塑剂含量为约29pph 3GO，大致相当于比较例C3的平均增塑剂含量。将这样的十一个层合材料用于冲击试验。平均穿透能为325焦耳。这也相似于比较例C3中的层合材料的平均穿透能。
实施例1
层合材料如比较例C4那样制备，只是将PVB夹层叠层，使得两层0.76mm 30pph 3GO片材夹在两层0.51mm 20pph 3GO片材之间。所有组合夹层厚度为2.54mm。夹层的平均增塑剂含量为约29pph3GO，大致相当于比较例C3和C4的平均增塑剂含量。十一个层合材料受到冲击。平均穿透能为455焦耳，与比较例C3和C4中的层合材料相比，有显著增加，但是平均增塑剂含量却是相等的。

Claims (22)

1.一种层合制品，包含至少两层Tg为约32℃～约35℃的软质增塑聚乙烯醇缩丁醛(PVB)片材，且还包含至少一层硬挺PVB夹层片材，其中硬挺夹层：(i)Tg为约35℃～约60℃，(ii)位于至少两层软质PVB之间，和(iii)包含漂白化合物。
2.权利要求1的制品，其中所述硬挺PVB包含约5pph～约30pph以下的增塑剂。
3.权利要求2的制品，其中所述增塑剂的存在量为约15pph～约30pph以下。
4.权利要求3的制品，其中所述增塑剂的存在量为约18pph～约25pph。
5.权利要求4的制品，其中所述增塑剂的存在量为约18pph～约22pph。
6.权利要求2的制品，其中所述增塑剂是选自下述的增塑剂或增塑剂混合物：由脂族二醇与羧酸的化学反应得到的二酯，包括聚醚二醇或聚醚多元醇的二酯，和由得自多元羧酸和脂族醇得到的酯。
7.权利要求6的制品，其中所述增塑剂选自通过三甘醇和含有6～10个碳原子的脂族羧酸的反应制得的二酯；和由癸二酸与含有1～18个碳原子的脂族醇的反应制得的酯。
8.权利要求7的制品，其中所述增塑剂是三甘醇2-乙基己酸酯。
9.权利要求7的制品，其中所述增塑剂是癸二酸二丁酯。
10.权利要求6的制品，其中所述硬挺PVB包含选自阴离子表面活性剂的表面活性剂，包括：月桂基硫酸钠、月桂基硫酸铵、磺基丁二酸钠、含有6～12个碳原子的全氟羧酸铵、芳基磺酸钠、氯代环戊二烯和马来酸酐的加合物、部分中和的聚甲基丙烯酸、烷基芳基磺酸盐、二烷芳基聚醚磺酸钠、月桂基硫酸三乙醇胺、月桂基硫酸二乙基环己基铵、二烷基磺酸钠、硫酸化脂肪酸酯、硫酸化芳基醇、二烷基磺基丁二酸钠等。
11.权利要求10的制品，其中所述表面活性剂选自磺基丁二酸钠、和磺基丁二酸二烷基酯钠。
12.权利要求11的制品，其中所述表面活性剂是磺基丁二酸二烷基酯钠。
13.权利要求12的制品，其中所述表面活性剂是磺基丁二酸二辛酯钠(DOSS)。
14.权利要求13的制品，其中所述漂白化合物选自磺基丁二酸二烷基酯钠、磺基丁二酸钠、有机亚硫酸氢盐、无机亚硫酸氢盐等。
15.权利要求14的制品，其中所述漂白化合物是磺基丁二酸二烷基酯钠。
16.权利要求15的制品，其中所述漂白化合物是磺基丁二酸二辛酯钠。
17.权利要求16的制品，其中所述PVB包含抗氧剂。
18.权利要求17的制品，其中所述抗氧剂是取代双酚化合物。
19.权利要求18的制品，其中所述硬挺PVB片材的厚度为约0.1mm～约0.75mm。
20.权利要求19的制品，其中所述硬挺PVB片材的厚度为约0.15mm～约0.72mm。
21.权利要求20的制品，其中所述硬挺PVB片材的厚度为约0.20mm～约0.70mm。
22.权利要求21的制品，其中所述硬挺PVB片材的厚度为约0.25mm～约0.68mm。
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