CN101903167A - 高阻燃面板 - Google Patents

高阻燃面板 Download PDF

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CN101903167A
CN101903167A CN2008801211977A CN200880121197A CN101903167A CN 101903167 A CN101903167 A CN 101903167A CN 2008801211977 A CN2008801211977 A CN 2008801211977A CN 200880121197 A CN200880121197 A CN 200880121197A CN 101903167 A CN101903167 A CN 101903167A
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copolymer
layer
acid
ethene
weight
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CN101903167B (zh
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L·P·罗兰
S·廷迪利耶
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Dow Chemical Co
Dow Global Technologies LLC
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EI Du Pont de Nemours and Co
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Abstract

本发明公开了阻燃面板结构，所述阻燃面板结构包括至少一个外部金属层、一个或多个包含一种或多种官能化聚合物的接合层、和由玻璃纤维织物制成的芯层。所述阻燃面板结构具有优异的阻燃性能，并且采用诸如挤出或压延的常规工艺以合理的成本制造。所述阻燃面板结构可用于对阻燃性和/或防火性有要求的应用中，例如用于建筑和工程应用、汽车或铁路应用、医疗设备和行李箱。

Description

高阻燃面板
本发明涉及在有阻燃和/或防火要求的环境中使用的阻燃面板。
发明背景
对于在建筑和工程应用中使用的面板而言，往往需要用阻燃材料来防止火势蔓延。阻燃面板常常用来覆盖建筑物的外表面和内表面并且通常具有“夹心”结构，即由金属制成的两个外层和由下文所述的阻燃组合物制成的中间层构成的结构。
对于建筑物面板来说，阻燃组合物的重要特性包括高阻燃性、良好的热性能和良好的机械特性。如今，适于制造建筑物面板的典型阻燃组合物取材于聚乙烯(PE)和/或乙烯乙酸乙烯酯(EVA)的共混物并含有最高约75重量％的阻燃添加剂，例如三水合铝(ATH)和/或氢氧化镁。为了满足严格的政府测试标准，例如DIN 4102 A2等级，已经通过加入大量阻燃添加剂(最高约90重量％)来达到显著改善组合物的阻燃性的目的。虽然通过加入如此大量的阻燃添加剂使组合物具有高阻燃性，但此类组合物也具有诸多缺点。加入如此大量的阻燃添加剂不但会降低热塑性聚合物的机械特性(例如塑性材料变得易碎，与最初的聚合物相比弹性降低，这对许多应用来说都很不利)，而且会加大制造复合材料面板的难度。随着阻燃添加剂含量的增加，热塑性组合物的加工性能降低，从而无法通过诸如挤出或压延的常规方法进行加工。对于这类阻燃添加剂含量较高的热塑性组合物，在适当的温度和压力条件下利用粘合剂聚合物和诸如平板层压的方法将铝薄板和热塑性组合物粘合在一起可制造阻燃复合材料面板。
另一方面，建筑和工程应用中也普遍要求节约成本。ATH之类的阻燃剂价格较高，使得含有大量这种化合物的典型阻燃组合物也价格不菲。诸如ATH或氢氧化镁之类阻燃添加剂高昂的造价以及必要制造工艺的复杂性和投入成本使得这类复合材料面板的生产缺乏吸引力。
因此，需要既具有较高阻燃性又可通过常规工艺以合理的成本制造的阻燃面板。
发明概述
令人吃惊的是，利用由下列部分组成的阻燃面板结构可以解决上述问题：
(i)至少一个外部金属层；
(ii)一个或多个包含一种或多种官能化聚合物的接合层；和
(iii)由玻璃纤维织物制成的芯层。
与满足较高政府测试标准(例如DIN 4102 A2等级)要求的现有技术阻燃面板相比，本发明的阻燃面板结构具有相当好的阻燃特性，并且还能通过常规工艺例如挤出或压延以合理的成本进行制造。
发明详述
根据本发明的阻燃面板结构的至少一个外部金属层可由任何合适的金属制成，这些金属适用于有阻燃要求的应用中的结构，并且可选自例如铝、不锈钢、铜、钢、黄铜、以及它们的合金。该金属层使阻燃面板结构本身具有强度和刚度，使其适合在多种气候条件下使用，提高其阻燃性并改善外观效果，而且还不会显著增加结构总重。由于铝具有重量轻、耐腐蚀和耐久性的优点，因此优先使用。当根据本发明的面板结构中使用一个外部金属层时，该金属层邻近包含一种或多种官能化聚合物的一个或多个接合层中的一者。当根据本发明的面板结构中使用两个外部金属层时，每一层都邻近一个或多个接合层中的其中一层，从而夹在芯层两侧。至少一个外部金属层的厚度范围优选介于100和500μm之间。
所谓“一个或多个接合层”是指：i)一个或多个接合层位于外部金属层和芯层之间，其中接合层彼此邻近，或者ii)一个或多个接合层位于芯层两侧，其中接合层彼此邻近。根据本发明的面板结构的一个或多个接合层包含一种或多种官能化聚合物。所谓“官能化聚合物”是指聚合物与有机官能团进行接枝和/或共聚，该聚合物可以为均聚物、共聚物或三元共聚物。根据本发明的阻燃面板结构的接合层中使用的一种或多种官能化聚合物优选地选自：酸酐官能化的聚合物(a)、乙烯酸共聚物(b)、具有乙烯和选自下列共聚单体的共聚单元的共聚物(c)：C4-C8不饱和酸酐、具有至少两个羧酸基团的C4-C8不饱和酸的单酯、具有至少两个羧酸基团的C4-C8不饱和酸的二酯、以及它们的混合物。为了与一个或多个外部金属层之间具有较强粘附力，需要有羧酸或酸酐官能团。
适合用作一个或多个接合层的组分的酸酐接枝聚合物(a)为酸酐接枝聚合物。优选地，酸酐接枝聚合物包括已经与约0.01至约3重量％(优选地从约0.05至约1重量％)的不饱和二元羧酸酸酐接枝的聚合物，其中所述重量百分比是按酸酐接枝聚合物的总重量计的。接枝剂包括不饱和二元羧酸酸酐，例如马来酸酐、柠康酸酐、衣康酸酐和四氢邻苯二甲酸酐，优选马来酸酐。被接枝的聚合物可以为均聚物、共聚物或三元共聚物。优选地，一种或多种酸酐接枝聚合物为酸酐接枝聚烯烃。实例包括接枝的聚乙烯、聚丙烯、乙烯α烯烃、乙烯(甲基)丙烯酸烷基酯共聚物、乙烯乙酸乙烯酯共聚物、乙烯-丙烯-二烯亚甲基共聚物(EPDM)、苯乙烯-乙烯-丁二烯-苯乙烯(SEBS)共聚物和苯乙烯-丁二烯-苯乙烯(SBS)共聚物。“(甲基)丙烯酸烷基酯”是指丙烯酸烷基酯和/或甲基丙烯酸烷基酯。优选的酸酐接枝聚合物选自：接枝聚乙烯、接枝聚丙烯、接枝乙烯乙酸乙烯酯共聚物、接枝乙烯(甲基)丙烯酸烷基酯共聚物、以及它们的混合物。
用于制备马来酸酐接枝聚乙烯(MAH-g-PE)的聚乙烯为选自下列材料的通常可得的聚乙烯树脂：HDPE(密度大于0.94g/cm3)、LLDPE(密度为0.915至0.925g/cm3)、LDPE(密度为0.91至0.94g/cm3)和茂金属聚乙烯。用于制备马来酸酐接枝聚丙烯(MAH-g-PP)的聚丙烯包括聚丙烯的均聚物、无规共聚物、嵌段共聚物和三元共聚物。聚丙烯的共聚物包括聚丙烯与其他烯烃(例如1-丁烯、2-丁烯和多种戊烯异构体)的共聚物。乙烯α烯烃共聚物包含乙烯和一种或多种α烯烃。α烯烃的实例包括但不限于：丙烯、1-丁烯、1-戊烯、1-己烯、4-甲基-1-戊烯、1-庚烯、1-辛烯、1-壬烯、1-癸烯、1-十一碳烯和1-十二碳烯。
乙烯(甲基)丙烯酸烷基酯共聚物为乙烯共聚单体和至少一种(甲基)丙烯酸烷基酯共聚单体的共聚作用所产生的热塑性乙烯共聚物，其中烷基包含1至10个碳原子，优选包含1至4个碳原子。当根据本发明的面板结构的一个或多个接合层中使用乙烯(甲基)丙烯酸烷基酯共聚物时，该共聚物优选地选自：乙烯(甲基)丙烯酸甲酯共聚物、乙烯(甲基)丙烯酸乙酯共聚物、乙烯(甲基)丙烯酸丁酯共聚物、或它们中两种或更多种的组合。
如本文所用，术语“乙烯-丙烯-二烯弹性体(EPDM)”是指任何弹性体，该弹性体为乙烯与至少一种α烯烃和共聚非共轭二烯(例如降冰片二烯、5-亚乙基-2-降冰片、二环戊二烯、1，4-己二烯等)的三元共聚物。
乙烯酸共聚物(b)可通过乙烯与α，β-不饱和的C3-C8羧酸的共聚作用来制备。优选地，本发明的面板结构的一个或多个接合层中使用的乙烯酸共聚物为乙烯丙烯酸共聚物(EAA)、乙烯甲基丙烯酸共聚物(EMAA)、乙烯马来酸单乙酯共聚物(EMAME)或它们的混合物。优选地，乙烯酸共聚物包含约1至约30重量％(更优选地约2至约10重量％)的α，β-不饱和C3-C8羧酸，所述重量百分比是按乙烯酸共聚物的总重量计的。乙烯酸共聚物也包括更多元的共聚物，例如可描述为E/X/Y共聚物的三元共聚物，其中E为乙烯，X可以为至少一种上述α，β-不饱和C3-C8羧酸，Y为软化共聚单体，例如丙烯酸烷基酯、甲基丙烯酸酯或它们的组合。X的含量可为约3至约30重量％，优选约4至约25重量％，更优选约5至约20重量％。Y的含量为0至约35重量％，优选约0.1至约35重量％，更优选约5至30重量％，所述重量百分比是按E/X/Y共聚物的总重量计的。
可在根据本发明的阻燃面板结构的一个或多个接合层中使用的第三类官能化聚合物为包含乙烯与选自下列共聚单体的共聚单元的聚合物：C4-C8不饱和酸酐、具有至少两个羧酸基团的C4-C8不饱和酸的单酯、具有至少两个羧酸基团的C4-C8不饱和酸的二酯、以及这些共聚物的混合物。乙烯共聚物一般包含约0.5重量％至约25重量％的共聚单体的共聚单元。该共聚物可以为二聚物或更多元的共聚物，例如三元共聚物或四元共聚物。该共聚物优选地为无规共聚物。乙烯共聚物的合适共聚单体的实例包括不饱和酸酐，例如马来酸酐和衣康酸酐；丁烯二酸(例如马来酸、富马酸、衣康酸和柠康酸)的C1-C20烷基单酯，包括马来酸单甲酯、马来酸单乙酯、富马酸单丙酯和富马酸单(2-乙基己基)酯；丁烯二酸的C1-C20烷基二酯，例如马来酸二甲酯、马来酸二乙酯、柠康酸二丁酯、马来酸二辛酯和富马酸二(2-乙基己基)酯。其中，优选马来酸酐、马来酸单乙酯和马来酸单甲酯。最优选的为马来酸酐和马来酸单乙酯。作为乙烯共聚物组分的实例的更多元共聚物包括三元共聚物，例如乙烯/丙烯酸甲酯/马来酸单乙酯、乙烯/丙烯酸丁酯/马来酸单乙酯和乙烯/丙烯酸辛酯/马来酸单乙酯。
接合层的厚度范围优选介于10和500μm之间，更优选介于30和90μm之间。
根据本发明的阻燃面板结构的芯层由玻璃纤维织物制成。芯层可为玻璃纤维的非织造单向织物或织造织物，前提是该织物可以抵抗劣化或分层。此外，在满足抵抗劣化或分层的相同要求下，优选的是织物表面足够平坦，使得各层之间具有良好的粘附力。优选地，根据本发明的阻燃面板结构的芯层由玻璃纤维织物制成，该玻璃纤维为玻璃纤维的织造织物，其中玻璃纤维为E-玻璃长丝，该E-玻璃长丝具有介于0.5和300μm之间的直径，优选具有介于5至30μm之间的直径。由玻璃纤维织物制成的芯层的厚度范围优选介于2和5mm之间，更优选介于3和4mm之间。
为了减少燃烧过程中产生的烟雾和热量并降低燃烧速度，可以用酚醛树脂来浸渍芯层中使用的玻璃纤维织物。
为了进一步改善根据本发明的面板结构的阻燃性，一个或多个接合层还可包含非反应性无机填料。所谓“非反应性填料”是指不与接合层内所用聚合物的有机官能团(即酸酐和酸性官能团)反应的填料。非反应性填料的实例包括但不限于二氧化硅、滑石、煅烧粘土、云母和硼酸锌。惰性填充剂的含量优选为20至80重量％，更优选约40重量％至约60重量％，所述重量百分比是按接合层的总重量计的。
本发明的阻燃面板结构中使用的一个或多个接合层还可包含普通添加剂，例如抗氧化剂、炭黑、UV稳定剂、润滑剂、抗粘连剂、抗静电剂、蜡、颜料、二氧化钛和聚合物配混领域中已知的其他加工助剂。这些添加剂可以本领域已知的含量和形式存在于一个或多个接合层的组合物中。
如果芯层表面不够平坦，无法在各层之间形成良好的粘附力，则可以在一个或多个接合层与芯层之间增加一个或多个附加层。为了进一步改善根据本发明的面板结构的阻燃性，一个或多个附加层优选地包含阻燃组合物。典型的阻燃组合物取材于例如聚乙烯和/或乙烯共聚物与阻燃添加剂例如三水合铝和氢氧化镁以及任选地与惰性填充剂例如碳酸钙、滑石、煅烧粘土、云母或硼酸锌的共混物。可用于一个或多个附加层的阻燃组合物的实例可见于WO 2006124658和美国专利7279520。如果一个或多个附加层与芯层之间的粘附力不够，则可以在它们之间增加一个或多个常规的粘合剂层。
为了提高根据本发明的阻燃面板的抗刮擦性和耐磨损性，这类面板还可包括外部层，该外部层邻近外部金属层，因而面向环境，并且可以保护阻燃面板结构，使其不受气候条件的影响。这类外部层可以包含或由离聚物组合物制成。离聚物及其作为抗刮擦和耐磨损顶层的使用和优点在EP0730622或WO95/07178中有所描述。
采用本领域已知的任何熔融混合方法将聚合物组分和非聚合组分混合在一起可得到一个或多个接合层中所用的组合物和一个或多个附加层中所用的组合物。例如，可将聚合物组分与非聚合组分加入到熔融混合器，例如单螺杆或双螺杆挤出机、共混机、单螺杆或双螺杆捏合机、哈克混合器、希拉本德混合器、班伯里密炼机或辊式混合机(一次全部加入，或逐步加入)中，然后再熔融混合。当逐步加入聚合物组分和非聚合组分时，首先加入一部分聚合物组分和/或非聚合组分并熔融混合，然后再加入剩余聚合物组分和非聚合组分，并进一步熔融混合，直到获得混合充分的组合物。
一个或多个接合层与一个或多个附加层可以通过上述熔融混合挤出法直接制造，或者首先制备组合物，然后再利用任何常规技术(例如挤出、压延和热层压)进行加工。
根据本发明的阻燃面板结构可采用常规工艺进行制造，例如，首先将接合层的聚合材料预层压或挤压涂布到芯层上，然后再将所得多层结构与外部金属层层压到一起。
当根据本发明的阻燃面板结构在接合层与芯层之间具有一个或多个附加层(例如，由阻燃组合物制成)时，可以采用常规工艺制造此类面板结构，例如：a)首先将阻燃组合物层压或挤压涂布到芯层上，接着将接合层的聚合材料层压或挤压涂布到所得多层结构上，然后再将所得多层结构与外部金属层层压到一起；或者b)将阻燃组合物与接合层的聚合材料共挤出涂布到芯层上，然后再将所得多层结构与外部金属层层压到一起。
当根据本发明的阻燃面板结构在附加层与芯层之间具有一个或多个常规粘合剂层时，可采用常规工艺制造此类面板结构，例如：a)首先将常规粘合剂层层压或挤压涂布到芯层上，然后再进行挤出或层压；或者b)将阻燃组合物与常规粘合剂共挤出涂布到芯层上，接着将接合层的聚合材料层压或挤压涂布到所得多层结构上，然后再将所得多层结构与外部金属层层压到一起。
作为另外一种选择，本发明的阻燃面板结构的制造工艺可以包括液压机以便适当控制温度和压力。
由于阻燃性较好，根据本发明的阻燃面板结构尤其适用于有阻燃和/或防火要求的各种应用。这类应用的实例包括建筑与工程构件，如外墙板、内墙板、视频显示板、地板、隔板和/或装饰墙；家具；以及汽车、火车、医疗设备和行李箱的载体部件。
实施例
下列材料用于制备根据本发明的样本以及对照样本：
共聚物A：MFI为20的乙烯丙烯酸甲酯共聚物(24重量％的MA)，得自E.I.du Pont de Nemours and Company(Wilmington，Delaware)(DuPont)。
官能化共聚物B：与马来酸酐接枝的乙烯丙烯酸甲酯共聚物(7.7重量％的MA，0.13重量％的接枝马来酸酐)，得自DuPont。
官能化共聚物C：与马来酸酐接枝的乙烯乙酸乙烯酯共聚物(8.1重量％的VA，0.13重量％的接枝马来酸酐)，得自DuPont。
ATH：
Figure GPA00001159750100071
8，得自德国Nabaltec公司。
玻璃纤维织物：3mm厚织造织物(Doubled LT 1700，单位重3400g/m2)，得自法国Sicomin公司。
比较实施例1(C1)：30重量％的共聚物A和70重量％的ATH。通过熔融混合法制备包含30重量％的共聚物A和70重量％的ATH的共混物(C1)。熔融混合法在双辊开炼机上进行，批量为250g，在190℃下进行约12分钟。在190℃下，用液压机将上述产物压成试片，无压状态下保持1分钟，150巴压力下保持约2分钟，然后在保持150巴压力的情况下，将试片以10℃/分的速度冷却15分钟。
实施例1(E1)：首先将官能化共聚物B和官能化共聚物C共挤出以制备两层聚合物膜。然后在150℃下，使用液压机将这些薄膜(官能化共聚物B层：25μm和官能化共聚物C层：50μm)层压到3mm厚的玻璃织物两侧约5分钟时间。
为了进行比较，测量符合DIN 4102 A2类规范的、可商购获得的复合材料面板(C2)的限氧指数。该复合材料面板(C2)(可以商品名
Figure GPA00001159750100081
A2从Alcan商购获得)由包含聚烯烃聚合物的芯层和夹在其两侧的两层铝制成，芯层含有80重量％以上的无机阻燃填料。用机械方法移除两层铝，并测量芯层的限氧指数。
按照ASTM D2863测量限氧指数(LOI)。结果示于表1中。
表1
  实施例编号   C1   C2   E1
  LOI  (％)   40   ＞55   ＞55
表1显示，本发明的样本(E1)的LOI值高于含有70重量％的ATH阻燃添加剂的对照样本(C1)。本发明的样本(E1)的LOI值与填料含量非常高的对照样本(C2)相同，该对照样本符合非常严格的DIN 4102A2等级的要求。

Claims (13)

1.阻燃面板结构，所述阻燃面板结构依次包括：
(i)至少一个外部金属层；
(ii)一个或多个包含一种或多种官能化聚合物的接合层；和
(iii)由玻璃纤维织物制成的芯层。
2.根据权利要求1的结构，其中所述官能化聚合物选自：(a)酸酐官能化的聚合物、(b)乙烯酸共聚物、(c)包含乙烯与共聚单体的共聚单元的共聚物，或者(a)、(b)和(c)中的两种或更多种的混合物，其中所述共聚单体包括C4-C8不饱和酸酐、具有至少两个羧酸基团的C4-C8不饱和酸的单酯、具有至少两个羧酸基团的C4-C8不饱和酸的二酯、或它们中的两种或更多种的混合物。
3.根据权利要求1或2的结构，其中所述官能化聚合物为接枝聚乙烯、接枝聚丙烯、接枝乙烯乙酸乙烯酯共聚物、接枝乙烯(甲基)丙烯酸烷基酯共聚物、或它们中的两种或更多种的混合物。
4.根据权利要求2或3的结构，其中所述酸酐接枝聚合物为乙烯乙酸乙烯酯、乙烯(甲基)丙烯酸甲酯、乙烯(甲基)丙烯酸乙酯、乙烯(甲基)丙烯酸丁酯、或它们中的两种或更多种的混合物。
5.根据权利要求2或4的结构，其中
所述酸酐接枝聚合物用约0.01至约3重量％的不饱和二元羧酸酐进行接枝，所述重量百分比是按所述酸酐接枝聚合物的总重量计的；并且
所述乙烯酸共聚物为乙烯丙烯酸共聚物、乙烯甲基丙烯酸共聚物、乙烯马来酸单乙酯共聚物、或它们中的两种或更多种的混合物。
6.根据任何前述权利要求的结构，其中
所述乙烯酸共聚物包含约1至约30重量％的α，3-不饱和C3-C8羧酸，所述重量百分比是按所述乙烯酸共聚物的总重量计的；并且
所述接合层具有介于10和500μm之间的厚度。
7.根据权利要求2的结构，其中
所述外部金属层由铝、不锈钢、铜、钢、黄铜、或它们的合金制成，并且优选由铝制成；并且
所述金属层具有介于100和500μm之间的厚度。
8.根据任何前述权利要求的结构，所述结构包括邻近玻璃纤维织物制成的芯层设置在所述第一金属层相对侧上的附加金属层，所述附加金属层由一个或多个接合层粘附到由玻璃纤维制成的织物上，其中所述接合层还包含非反应性无机填料；
由玻璃纤维织物制成的芯层具有介于2和5mm之间的厚度；并且
所述芯层的玻璃纤维织物用酚醛树脂浸渍。
9.根据任何前述权利要求的结构，所述结构还包括介于由玻璃纤维织物制成的芯层和所述接合层之间的一个或多个附加层。
10.根据权利要求9的结构，其中所述一个或多个附加层由阻燃组合物制成。
11.根据权利要求2的结构，所述结构还包括邻近所述外部金属层的外部层，所述外部层由离聚物组合物制成。
12.根据权利要求11的结构，其中所述接合层为接枝聚乙烯、接枝聚丙烯、接枝乙烯乙酸乙烯酯共聚物、接枝乙烯(甲基)丙烯酸烷基酯共聚物、或它们中的两种或更多种的混合物。
13.如权利要求1至12中任一项所表征的阻燃面板结构用于建筑应用、汽车或铁路应用、或医疗设备的用途。
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