CN102844165B - 具有高压缩强度和刚度的聚氨酯复合材料体系 - Google Patents
具有高压缩强度和刚度的聚氨酯复合材料体系 Download PDFInfo
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- CN102844165B CN102844165B CN201080061620.6A CN201080061620A CN102844165B CN 102844165 B CN102844165 B CN 102844165B CN 201080061620 A CN201080061620 A CN 201080061620A CN 102844165 B CN102844165 B CN 102844165B
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- composite system
- polyurethane
- polyurethane foams
- hard polyurethane
- foam
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
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Abstract
本发明涉及一种聚氨酯复合材料体系,其含有硬质聚氨酯泡沫以及由压实聚氨酯或压实聚脲组成的涂料,其中所述硬质聚氨酯泡沫含有多孔的三维增强剂,其形成网络,所述网络封闭了硬质聚氨酯泡沫的体积的至少50%,或所述硬质聚氨酯泡沫含有至少两层的多孔的至少二维增强剂。本发明还涉及一种制备聚氨酯复合材料体系的方法,以及涉及含有这种聚氨酯复合材料体系的运动设备制品、覆盖部件或家具部件。
Description
本发明涉及一种聚氨酯复合材料体系,其含有硬质聚氨酯泡沫以及由压实聚氨酯或压实聚脲组成的涂料,其中所述硬质聚氨酯泡沫含有形成网络的多孔三维增强材料,其中所述网络封闭了硬质聚氨酯泡沫的体积的至少50%,或所述硬质聚氨酯泡沫含有至少两层的多孔的至少二维增强材料。本发明还涉及一种制备聚氨酯复合材料体系的方法,以及涉及含有这种聚氨酯复合材料体系的运动制品、覆盖部件或家具物品。
基于被涂料涂覆的硬质聚氨酯泡沫的复合材料是在许多领域中公知的。涂覆一般如下进行:将硬质聚氨酯泡沫在预制的外壳中发泡,或制备硬质聚酯酯泡沫并随后连接成覆盖层。在第一种情况下,这是例如用作汽车中的保险杠、或用作冷却箱或冰箱外壳,以及在第二种情况下与具有表面涂层的金属片涂层一起作为外壁覆盖用。这些低密度复合材料的显著优点是它们的低重量与一些机械稳定性的组合。另一个优点是材料的独立性。因此,所需的制品可以各自从硬质聚氨酯泡沫块生产,并随后提供涂层。
低密度泡沫材料的缺点是它们的压缩强度低,压缩强度低以及仅仅具有中等的芯刚度,和挠曲强度低。如果需要同时具有高的刚度和压缩强度以及低的材料重量,例如用于运动制品例如冲浪板,冬季运动设备,小型运动船只或网球架,家具物品,飞机部件例如副翼或方向舵,风力发电机的叶片,或在交通工具结构或建筑工业中的覆盖部件,则硬质聚氨酯泡沫是通过增强材料增强的。这些是例如由木材或金属以及树脂增强的玻璃纤维毡组成的部件。这些增强部件是例如布置在硬质聚氨酯泡沫中的研磨凹处或施用到硬质聚氨酯泡沫的表面上。
为了进一步改进刚度以及改进压缩强度,硬质聚氨酯泡沫的表面被压实的涂料覆盖。这些涂料可以是非柔性的高刚度材料,例如金属或聚苯乙烯板;或部分柔性的材料,例如被环氧树脂浸渍的多层玻璃纤维毡。为了获得具有高表面质量的表面,被环氧树脂浸渍的每层玻璃纤维毡必须在干燥之后研磨。在施用通常2或3层玻璃纤维毡之后,将它们磨平,提供表面涂料,任选地提供印刷图案和透明涂饰层以及任选地花纹区域,把手和固定元件。此方法是非常耗时和耗力的,并且使用插件和用被环氧树脂浸渍的多层玻璃纤维毡进行涂覆导致消除了复合材料的低重量的优点。此外,环氧树脂是较昂贵的。
也已经知道由硬质聚氨酯泡沫和聚脲涂料组成的带涂层的聚氨酯喷涂泡沫材料,其中硬质聚氨酯泡沫含有短纤维材料作为增强材料。这些复合材料体系是通过至少一种用于制备硬质聚氨酯泡沫的已含有增强材料的反应混合物在混合之前制备的,或通过将增强材料与反应混合物一起喷到模具中来制备。这些复合材料例如参见US 2002/0137871或US 2008/299372。这些复合材料的缺点是仅仅少量地改进机械性能,尤其是挠曲强度。此外,生产受到模具形状的限制,所以复合材料的单独成型是不可能的。
本发明的目的是提供一种基于硬质聚氨酯泡沫的聚氨酯复合材料体系,此体系在降低的总重量下具有改进的刚度和压缩强度,并且易于制备。另一个目的是提供一种允许灵活改变复合材料体系的最终形状/构型的方法。
本发明的目的通过一种聚氨酯复合材料体系实现,其含有硬质聚氨酯泡沫以及由压实聚氨酯或压实聚脲组成的涂料,其中所述硬质聚氨酯泡沫含有形成网络的多孔三维增强材料,其中所述网络封闭了硬质聚氨酯泡沫的体积的至少50%,或所述硬质聚氨酯泡沫含有至少两层的多孔的至少二维增强材料。
如果使用多层,则这些层优选均匀地分布在硬质聚氨酯泡沫中。在本文中,均匀分布表示在两个相邻层之间或在泡沫的上层和上侧之间或在泡沫的下层和下侧之间的最大距离与在两层之间或在泡沫的上层和上侧之间或在泡沫的下层和下侧之间的最小距离相比所相差的倍数是不超过4倍,优选不超过2倍,尤其不超过1.5倍。
在本发明聚氨酯复合材料体系中使用的增强硬质泡沫具有的非密度依赖性的压缩强度是至少5*10-4MPa*(l/g)1.6,优选至少5.5*10-4MPa*(l/g)1.6,以及非密度依赖性的压缩E模量是至少8*10-3MPa*(l/g)1.7,优选至少9.5*10-3MPa/(l/g)1.7。非密度依赖性的压缩强度是作为压缩强度*(密度)-1.6计算的,非密度依赖性的压缩E模量是作为压缩E模量*(密度)-1.7计算的。对于在本发明聚氨酯复合材料体系中使用的增强硬质泡沫,这意味着在泡沫密度为45g/l的情况下,压缩强度为至少0.2MPa、优选至少0.25MPa,压缩E模量为至少5MPa、优选至少6MPa。另外,在45g/l的密度下,所述硬质泡沫所具有的挠曲强度为至少0.4MPa,优选至少0.5MPa。本发明的聚氨酯复合材料体系在45g/l的泡沫密度和1mm的涂料层厚度下具有至少400N的表面硬度,优选至少500N。根据本发明使用的增强硬质聚氨酯泡沫具有30-500g/l的密度,优选40-400g/l,特别优选40-300g/l,尤其是40-200g/l,例如40-100g/l,例如40-60g/l。
为了本发明的目的,当用于制备硬质聚氨酯泡沫的反应混合物能穿透进入增强材料并能渗透和完全润湿增强材料时,增强材料被称为是多孔的。增强材料形成在本发明聚氨酯复合材料体系的硬质聚氨酯泡沫中的二维或三维网络。形成网络的材料,例如纤维、粗纱或带,优选彼此连接,例如通过交缠或粘合连接。为了形成三维增强材料,可以连接多种的二维增强材料。此外,扭转或编织的纤维绞线,例如纤维编织物,可以用作三维增强材料。
增强材料可以含有例如玻璃纤维、芳族聚酰胺纤维、碳纤维或聚合物纤维。增强材料也可以含有这些材料的组合。因此,例如三维增强材料可以含有由聚酰胺纤维连接的两个玻璃纤维毡。
增强材料在至少两层中使用。仅仅当三维网络封闭硬质聚氨酯泡沫的体积的至少50%时,才能使用一种三维增强材料。
这些二维或三维网络是例如通过使用叠层、织造筛网或基于纤维的编织结构获得的。这种二维增强材料优选是纤维毡,例如织物、玻璃纤维或碳纤维毡,或带,优选玻璃纤维毡,例如来自Owens Corning Vetrotex的U801或U809。也可以使用玻璃纤维粗纱毡。
增强材料的比例优选是5-40重量%,尤其是10-20重量%,基于包含增强材料的硬质聚氨酯泡沫的总重量计。
本发明的硬质聚氨酯泡沫优选是如下获得的:将(a)异氰酸酯、(b)具有对异氰酸酯有活性的基团的化合物、(c)包含水的发泡剂、(d)催化剂和任选地(e)其它添加剂混合以形成反应混合物,将所述反应混合物施用到增强材料上并固化所述反应混合物。为此目的,增强材料的这些层是已制备好的,并且将聚氨酯反应混合物施用到增强材料的这些层上。反应混合物基本上完全地浸渍增强材料,并且由于在聚氨酯反应混合物中的发泡反应,增强材料的各个层或者三维增强材料的网络均匀地分布在泡沫中,即,由于聚氨酯反应混合物的发泡作用,已经基本上被反应混合物完全浸渍的增强材料发生膨胀和拉伸,使得由三维增强材料形成的网络封闭硬质聚氨酯泡沫的体积的至少50%。
作为异氰酸酯(a),可以使用所有常规的脂族、脂环族和优选芳族的二异氰酸酯和/或多异氰酸酯。这些优选具有小于600mPas的粘度,特别优选小于500mPas,尤其是小于350mPas,在25℃下检测。作为优选的异氰酸酯,可以使用甲苯二异氰酸酯(TDI)和二苯基甲烷二异氰酸酯(MDI),特别优选二苯基甲烷二异氰酸酯和聚合二苯基甲烷二异氰酸酯(PMDI)的混合物。这些特别优选的异氰酸酯可以完全或部分地用脲二酮、氨基甲酸酯、异氰脲酸酯、碳二酰亚胺、脲基甲酸酯和优选氨基甲酸酯基团改性。
此外,预聚物以及上述异氰酸酯和预聚物的混合物可以用作异氰酸酯组分。这些预聚物是从上述异氰酸酯和聚醚、聚酯或者这两者制备的,并且具有通常14-32重量%的NCO含量,优选22-30重量%。
作为具有对异氰酸酯有活性的基团的化合物(b),可以使用所有具有至少两个对异氰酸酯有活性的基团的化合物,所述基团是例如OH-、SH-、NH-和CH-酸性基团。通常使用具有2-8个对异氰酸酯有活性的氢原子的聚醚醇和/或聚酯醇。这些化合物的羟值通常在30-850mg KOH/g的范围内,优选在80-600mg KOH/g的范围内。
聚醚醇是通过公知的方法获得的,例如通过环氧烷与以键合形式含有2-8个、优选2-6个活泼氢原子的至少一种起始分子在催化剂存在下进行阴离子聚合反应。作为催化剂,可以使用碱金属氢氧化物,例如氢氧化钠或氢氧化钾,或碱金属醇盐,例如甲醇钠、乙醇钠、乙醇钾或异丙醇钾,或者在阳离子聚合的情况下使用路易斯酸例如五氯化锑、三氟化硼醚合物或漂白土。此外,双金属氰化物也可以用作催化剂,公知称为DMC催化剂。
作为环氧烷,优选使用一种或多种在亚烷基中具有2-4个碳原子的化合物,例如四氢呋喃、1,3-氧化丙烯,1,2-或2,3-氧化丁烯,在每种情况下单独使用或以混合物的形式使用,并且优选环氧乙烷和/或1,2-氧化丙烯.
可能的起始分子是例如乙二醇、二甘醇、甘油、三羟甲基丙烷、季戊四醇,糖衍生物例如蔗糖,六糖衍生物例如山梨醇,甲基胺,乙基胺,异丙胺,丁基胺,苄基胺,苯胺,甲苯胺,甲苯二胺,萘基胺,乙二胺,二亚乙基三胺,4,4’-亚甲基二苯胺,1,3-丙二胺,1,6-己二胺,乙醇胺,二乙醇胺,三乙醇胺,以及其它的二元醇或三元醇或者单官能胺或多官能胺。
所用的聚酯醇通常通过具有2-12个碳原子的多官能醇与具有2-12个碳原子的多官能羧酸进行缩合制备,具有2-12个碳原子的多官能醇是例如乙二醇、二甘醇、丁二醇、三羟甲基丙烷、甘油或季戊四醇,具有2-12个碳原子的多官能羧酸是例如琥珀酸、戊二酸、己二酸、辛二酸、壬二酸、癸二酸、癸烷二甲酸、马来酸、富马酸、邻苯二甲酸、间苯二甲酸、对苯二甲酸,萘二羧酸的异构体或者所述酸的酸酐。
作为在聚酯制备中的其它原料,也可以共同使用疏水性物质。疏水性物质是不溶于水的物质,其含有非极性有机基团并且具有至少一个选自羟基、羧基、羧酸酯或其混合物的活性基团。疏水性物质的当量重量优选在130-1000g/mol的范围内。可以使用例如脂肪酸,例如硬脂酸、油酸、棕榈酸、月桂酸或亚油酸,以及脂肪和油,例如蓖麻油、玉米油、葵花油、豆油、椰壳油、橄榄油或牛油。如果聚酯含有疏水性物质,则疏水性物质在聚酯醇的单体总含量中的比例优选是1-30摩尔%,特别优选4-15摩尔%。
所用的聚酯醇优选具有1.5-5的官能度,特别优选1.8-3.5,尤其是1.9-2.2。
此外,具有对异氰酸酯有活性的基团的化合物优选含有(b)扩链剂和/或交联剂。所用的扩链剂和/或交联剂尤其是双官能或三官能的胺和醇,尤其是二醇、三醇或这两者,在每种情况下其具有小于350g/mol的分子量,优选60-300g/mol,尤其是60-250g/mol。在这里,双官能化合物被称为扩链剂,三官能或更高官能的化合物被称为交联剂。作为起始分子,可以使用具有2-14个、优选2-10个碳原子的脂族、脂环族和/或芳族二醇,例如乙二醇、1,2-丙二醇、1,3-丙二醇、1,2-戊二醇、1,3-戊二醇、1,10-癸二醇、1,2-二羟基环己烷、1,3-二羟基环己烷、1,4-二羟基环己烷、二甘醇、三甘醇、双丙甘醇、三丙甘醇、1,4-丁二醇、1,6-己二醇和双(2-羟基乙基)氢醌;三醇,例如1,2,4-三羟基环己烷、1,3,5-三羟基环己烷、甘油和三羟甲基丙烷,以及低分子量的含羟基的聚环氧烷,其基于环氧乙烷和/或1,2-环氧丙烷以及上述二醇和/或三醇。
具有对异氰酸酯有活性的基团的化合物(b)优选含有具有官能度为4或更大且在25℃下的粘度为10,000mPas或更低的聚醚醇(b1),和含有具有官能度为3.5或更低、优选3或更低且在25℃下的粘度为600mPas或更低、优选500mPas或更低的聚醚醇(b2)。具有对异氰酸酯有活性的基团的化合物(b)特别优选不仅含有聚醚醇(b1)和(b2),而且含有具有在25℃下的粘度为2000mPas或更低的聚酯醇(b3)、扩链剂(b4)和任选地交联剂(b5)。
作为组分(b1)至(b5),在每种情况下可以使用单独的化合物或混合物,其中每种使用的化合物是在(b1)至(b5)的定义范围内。
扩链剂(b4)可以是单独的化合物或混合物。扩链剂(b4)优选含有双丙甘醇、三丙甘醇和/或2,3-丁二醇,它们单独使用或任选地作为彼此的混合物使用或作为与其它扩链剂的混合物使用。
在另一个实施方案中,具有对异氰酸酯有活性的基团的化合物(b)不仅含有聚醚醇(b1)、聚醚醇(b2)、聚酯醇(b3)和扩链剂(b4),而且含有交联剂(b5)。作为交联剂,优选使用1,2,4-三羟基环己烷、1,3,5-三羟基环己烷、甘油和/或三羟甲基丙烷。优选使用甘油作为交联剂。
组分(b1)的比例优选是25-70重量%,特别优选25-55重量%,尤其是30-50重量%,基于组分(b)的总重量计。
组分(b2)的比例优选是10-40重量%,特别优选15-35重量%,基于组分(b)的总重量计。
组分(b3)的比例优选是15-50重量%,特别优选20-40重量%,基于组分(b)的总重量计。
在组分(b)中,扩链剂(b4)的比例优选是1-30重量%,特别优选5-20重量%,基于组分(b)的总重量计。
在组分(b)中,组分(b5)的比例优选是0-10重量%,特别优选1-5重量%,基于组分(b)的总重量计。
在具有对异氰酸酯有活性的基团的化合物(b)中,聚醚醇(b1)、(b2)、(b3)、(b4)和任选(b5)的比例优选是至少80重量%,特别优选至少90重量%,尤其是100重量%,基于具有对异氰酸酯有活性的基团的化合物(b)的总重量计。
组分(b)的总官能度优选大于2.5,特别优选大于2.6,尤其是大于2.75。组分(b)的平均羟值优选是大于300mg KOH/g,特别优选在350-1000mg KOH/g的范围内,尤其是400-600mg KOH/g。
如果异氰酸酯预聚物用作异氰酸酯(a),则具有对异氰酸酯有活性的基团的化合物(b)的含量是在包括用于制备异氰酸酯预聚物的具有对异氰酸酯有活性的基团的化合物(b)的情况下计算的。
作为发泡剂(c),使用含有水的发泡剂。在这里,水可以单独使用,或与其它发泡剂组合使用。水在发泡剂(c)中的含量优选大于40重量%,特别优选大于60重量%,非常特别优选大于80重量%,基于发泡剂(c)的总重量计。尤其是,水用作唯一的发泡剂。如果除了水之外还使用其它发泡剂,则可以使用例如氯氟烃、氟化烃、烃、酸和/或液体或溶解的二氧化碳。发泡剂(c)优选含有小于50重量%、更优选小于20重量%、特别优选小于10重量%、尤其是0重量%的氯氟烃、氟化烃和/或烃,基于发泡剂(c)的总重量计。在另一个实施方案中,水和甲酸和/或二氧化碳的混合物可以用作发泡剂(c)。为了能使得发泡剂(c)更容易地分散在多元醇组分中,发泡剂(c)可以与极性化合物混合,例如双丙甘醇。
发泡剂(c)的用量使得通过组分(a)至(e)反应形成的包含增强材料的硬质聚氨酯泡沫的密度是在30-500g/l的范围内,优选40-400g/l,特别优选40-300g/l,尤其是40-200g/l,例如40-100g/l,例如40-60g/l.
作为催化剂(d),可以使用所有能加速异氰酸酯-水反应或异氰酸酯-醇反应的化合物。这些化合物是公知的,例如参见"Kunststoffhandbuch,第7卷,聚氨酯(Polyurethane)",Carl Hanser Verlag,第3版1993,第3.4.1章。这些包括基于胺的催化剂和基于有机金属化合物的催化剂。
作为基于有机金属化合物的催化剂,可以使用例如有机锡化合物,例如有机羧酸的锡(II)盐,例如乙酸锡(II)、辛酸锡(II)、乙基己酸锡(II)和月桂酸锡(II);以及有机羧酸的二烷基锡(IV)盐,例如二乙酸二丁锡、二月桂酸二丁锡、马来酸二丁锡和二乙酸二辛基锡;以及羧酸铋,例如新癸酸铋(III)、2-乙基己酸铋和辛酸铋;或羧酸的碱金属盐,例如乙酸钾或甲酸钾。
优选使用含有至少一种叔胺的混合物作为催化剂(d)。这些叔胺通常是也可以带有对异氰酸酯有活性的基团的化合物,所述基团是例如OH、NH或NH2基团。一些最常用的催化剂是二(2-二甲基氨基乙基)醚,N,N,N,N,N-五甲基二亚乙基三胺,N,N,N-三乙基氨基乙氧基乙醇,二甲基环己胺,二甲基苄基胺,三乙基胺,三亚乙基二胺,五甲基二亚丙基三胺,二甲基乙醇胺,N-甲基咪唑,N-乙基咪唑,四甲基六亚甲基二胺,三(二甲基氨基丙基)六氢三嗪,二甲基氨基丙基胺,N-乙基吗啉,二氮杂双环十一碳烯和二氮杂双环壬烯。优选使用含有至少两种不同叔胺的混合物作为催化剂(d)。催化剂混合物(d)特别优选含有二甲基环己胺(d1)和二(2-二甲基氨基乙基)醚(d2)或二甲基环己胺(d1)和N,N,N,N,N-五甲基二亚乙基三胺(d3)。二甲基环己胺(d1):胺(d2)的比率和/或二甲基环己胺(d1):胺(d3)的比率优选是0.25-4:1,特别优选0.5-2:1。特别当在封闭空间中使用本发明的聚氨酯复合材料体系、例如在交通工具内部中使用时,也可以使用能减少释放的其它催化剂。这些催化剂是例如可引入的催化剂。也可以完全省去催化剂。
作为增强材料,可以使用所有上述增强材料。
作为其它添加剂(e),可以使用阻燃剂、增塑剂、泡沫稳定剂、其它填料和其它添加剂例如抗氧化剂。
作为阻燃剂,一般可以使用本领域公知的阻燃剂。合适的阻燃剂是例如溴化醚(Ixol B 251),溴化醇例如二溴新戊二醇、三溴新戊二醇和PHT-4-二醇,以及氯化磷酸酯,例如三(2-氯乙基)磷酸酯、三(2-氯异丙基)磷酸酯(TCPP)、三(1,3-二氯异丙基)磷酸酯、三(2,3-二溴丙基)磷酸酯和四(2-氯乙基)亚乙基二磷酸酯,或它们的混合物。
除了上述被卤素取代的磷酸酯之外,也可以使用无机阻燃剂,例如红磷、含红磷的制剂、可膨胀的石墨、氧化铝水合物、三氧化锑、氧化砷、多磷酸铵和硫酸钙,或氰尿酸衍生物例如蜜胺,或至少两种阻燃剂的混合物,例如多磷酸铵和蜜胺,以及任选地淀粉,用于使得根据本发明制备的硬质聚氨酯泡沫成为阻燃性的。
作为其它液态的不含卤素的阻燃剂,可以使用二乙基乙烷膦酸酯(DEEP)、磷酸三乙基酯(TEP)、二甲基丙基膦酸酯(DMPP)、二苯基甲酚基磷酸酯(DPC)等。
为了本发明目的,阻燃剂的用量优选是0-25重量%,基于组分(b)至(e)的总重量计。
泡沫稳定剂是能在泡沫形成期间促进形成具有规则泡孔结构的物质。可以提到的例子是:含硅的泡沫稳定剂,例如硅氧烷-氧亚烷基共聚物和其它有机聚硅氧烷。也可以使用以下物质的烷氧基化产物:脂肪醇、羰基合成醇、脂肪胺、烷基酚、二烷基酚、烷基甲酚、氨基间苯二酚、萘酚、烷基萘酚、萘基胺、苯胺、烷基苯胺、甲苯胺、双酚A、烷基化双酚A、聚乙烯基醇;以及以下物质的缩合产物的烷氧基化产物:甲醛和烷基酚,甲醛和二烷基酚,甲醛和烷基甲酚,甲醛和烷基间苯二酚,甲醛和苯胺,甲醛和甲苯胺,甲醛和萘酚,甲醛和烷基萘酚,以及甲醛和双酚A;或者两种或多种这些泡沫稳定剂的混合物。
泡沫稳定剂的用量优选是0.5-4重量%,特别优选1-3重量%,基于组分(b)至(e)的总重量计。
其它填料,尤其是增强填料,是常规的有机和无机填料,增强材料等,它们是本身公知的。具体例子是:无机填料,例如含硅的矿物,例如片状硅酸盐,例如叶蛇纹石、蛇纹石、角闪石、闪石、纤蛇纹石、滑石;金属氧化物,例如高岭土、氧化铝、氧化钛和氧化铁;金属盐,例如白垩、锌钡白;以及无机颜料,例如硫化镉、硫化锌,以及玻璃等。优选使用高岭土(粘土)、硅酸铝,以及硫酸钡和硅酸铝的共沉积物,以及天然和和合成的纤维矿物,例如硅灰石、金属纤维和尤其是具有各种长度的玻璃纤维,其可以用胶料涂覆。也可以使用中空玻璃微球。可能的有机填料是例如:碳,蜜胺,松香,环戊二烯基树脂,以及接枝聚合物和纤维素纤维,聚酰胺,聚丙烯腈,聚氨酯,基于芳族和/或脂族二羧酸酯的聚酯纤维,以及碳纤维。
无机和有机填料可以单独使用,或作为混合物使用,并且向反应混合物中的添加量有利地是0.5-30重量%,优选1-15重量%,基于组分(a)至(e)的总重量计。
本发明的硬质聚氨酯泡沫优选作为块状泡沫材料连续地在带上制备,或不连续地在模具中制备。为此目的,组分(b)至(d)和任选的(e)混合形成多元醇组分。此多元醇组分随后与异氰酸酯组分(a)混合,优选在低压混合设备中、在高压混合物设备中在小于100巴的减压下或在高压机器中进行。作为另一个选择,组分(a)至(d)和任选的(e)也可以各自引入混合设备中。以此方式获得的反应混合物随后施用到增强材料上、优选施用到玻璃纤维毡或玻璃纤维编织物叠层上,它们优选连续地从多个转鼓卷绕出来到带上,或放置在模具的底部和任选地在那里形成合适数目的层。所获得的泡沫材料然后优选在带上或在模具中固化,达到能在无损坏的情况下切成小块的程度。这可以在室温或升高的温度下进行,例如在连续生产的情况下经过烘箱,或在不连续生产的情况下使用可加热的模具。所获得的泡沫块然后优选再储存一定时间,从而达到完全的机械强度。使用的玻璃纤维毡的数目可以自由选择,并取决于玻璃纤维在泡沫材料中的所需比例和取决于这些毡能均匀分布的设定泡沫高度。对于20-25cm的泡沫高度,优选例如具有毡密度为约450g/m2的3-10个毡层,尤其是5-8个毡层。
异氰酸酯(a)和具有对异氰酸酯有活性的基团的化合物(b)、包含水的发泡剂(c)、催化剂(d)和任选地其它添加剂(e)优选按照这样的量反应,使得异氰酸酯指数是在100-400的范围内,优选100-200,特别优选100-150。
为了本发明目的,异氰酸酯指数是异氰酸酯基团与对异氰酸酯有活性的基团之间的化学计算比率乘以100所得到的值。在这里,对异氰酸酯有活性的基团是所有对异氰酸酯有活性且存在于反应混合物中的基团,包括化学发泡剂,但不包括异氰酸酯基团本身。
特别有利的是,本发明的反应混合物快速穿透进入增强材料,并因此帮助增强材料均匀地和以高度空间填充的方式分布在所得的硬质聚氨酯泡沫中。本发明反应混合物的长乳化时间与短反应时间的组合也是有利的。另一个优点是本发明的反应混合物具有低粘度和良好的流动行为,从而将大面积的模具充分填充到角落。
本发明的增强和尤其涂覆的硬质聚氨酯泡沫是机械稳定的,具有低的热导率,显示出优异的泡沫性能,例如不含孔和裂纹,具有优良的机械性能例如压缩强度和冲击强度以及优异的压缩E模量,并且具有增强材料层的均匀分布。本发明的复合材料体系也具有优异的耐UV性。在这里,压缩强度和压缩E模量都是根据DIN 53421/DIN EN ISO 604沿着与发泡方向垂直和平行的方向(沿着x/y和z方向)检测的。在空间上平均的压缩强度和压缩E模量可以根据(x*y*z)1/3计算。挠曲强度是用具有120mmx25mmx20mm尺寸的试样根据DIN 53423于25℃检测的;检测与发泡方向垂直的泡沫平面的挠曲强度。本发明的硬质聚氨酯泡沫可以作为块料制备,并且可以从块料进行切割或研磨以得到用于具体应用的泡沫体。尤其是,多于一种的泡沫体可以从较大的泡沫块料获得。这使得泡沫体可以具有任何可能的复杂形状,也允许单独制备本发明泡沫的短试样或单独制件。
本发明的硬质聚氨酯泡沫使用用于制备压实聚氨酯、压实聚脲或聚氨酯-聚脲混杂体系的涂料涂覆。在这里,通过至少一种具有至少两个异氰酸酯基团的化合物与具有至少两个对异氰酸酯有活性的基团的化合物之间的反应获得的且基本上不含气体内含物的任何反应产物可以用作涂料,此涂料包含压实聚氨酯或压实聚脲或由它们组成。压实聚氨酯或压实聚脲的密度优选大于0.8g/cm3,特别优选大于0.9g/cm3,尤其是大于1.0g/cm3。在这里,术语“聚氨酯”表示能当具有至少两个对异氰酸酯有活性的基团的化合物中的活性基团主要是羟基时获得的化合物,术语聚脲表示能当具有至少两个对异氰酸酯有活性的基团的化合物中的活性基团主要是伯胺或仲胺基团时获得的化合物。在与异氰酸酯反应之前,这些胺通常与其它助剂和添加剂混合以形成胺组分。
硬质聚氨酯泡沫的涂覆操作优选在铸塑或喷涂工艺中进行,特别优选喷涂工艺,其中硬质聚氨酯泡沫使用用于制备涂料的反应混合物喷涂。任选地,本发明的聚氨酯复合材料体系也可以在模具中制备。为此,模具的内壁完全或部分地使用用于制备涂料的反应混合物喷涂,并且将增强材料和用于制备硬质聚氨酯泡沫的反应混合物随后引入模具中,并使其反应完全。在这里,可以使用所有公知的聚氨酯或聚脲喷涂体系。这些体系例如参见Becker/Braun,Kunststoffhandbuch No.7,聚氨酯(Polyurethane),第10章。聚脲喷涂体系可以详细参见DE102004022683。优选使用压实聚脲来涂覆硬质聚氨酯泡沫。
作为用于根据本发明制备压实聚氨酯或压实聚脲的具有至少两个异氰酸酯基团的化合物,可以使用例如所有在(a)中描述的异氰酸酯。基于二苯基甲烷二异氰酸酯(MDI)的异构体或异构体混合物和聚醚醇(例如聚丙二醇)的预聚物优选用作具有至少两个异氰酸酯基团的化合物。这些异氰酸酯预聚物是通过尤其羟基封端的、以及胺封端的聚环氧乙烷或聚环氧丙烷与多异氰酸酯的反应制备的。根据本发明使用的预聚物优选具有10-25重量%的异氰酸酯含量,特别优选15-20重量%,在25℃下的粘度是不超过2000mPas,尤其是300-1000mPas。
胺组分通常是脂族伯聚醚胺和一般芳族胺扩链剂的混合物。
聚脲配料的胺组分中的主要成分是聚醚胺的混合物,即,胺封端的双官能或更高官能的聚环氧乙烷或聚环氧丙烷,其分子量为200-5000g mol-1。脂族胺比扩链剂的芳族组分更快速地反应,并且主要用于生产聚脲喷涂弹性体中的软相。
通常用于聚脲配料中的扩链剂是二乙基甲苯二胺(DETDA)。作为比脂族胺的活性更低的组分,DETDA决定了体系的固化性能。为了合成光稳定性聚脲,也使用脂族扩链剂。通常芳族的扩链剂主要被引入聚脲喷涂弹性体中的硬相中。此外,聚脲配料可以含有如上述(e)中所述的其它添加剂和助剂,尤其是上述阻燃剂和消泡剂和/或吸水性添加剂,例如沸石。在本发明的另一个实施方案中,涂料可以含有长度小于2cm的短纤维,它们单独地储存并与反应混合物平行地喷涂,或预先悬浮在一种或多种聚脲组分中。
将涂料施用到硬质聚氨酯泡沫表面的至少30%上,优选至少50%,特别优选至少80%,尤其是100%。特别优选涂覆本发明聚氨酯复合材料体系的所有可见表面。
在用压实聚氨酯或压实聚脲涂覆之后,聚氨酯复合材料体系可以例如进一步用装饰性涂料涂覆。因此,例如可以施用装饰漆。此外,聚氨酯复合材料体系也可以完全或部分地用功能涂料涂覆,例如防滑涂料。
本发明的聚氨酯复合材料体系不仅具有低重量,而且具有优异的压缩强度、挠曲强度、刚度、冲击韧性和表面质量。此外,它们具有优异的隔热性能和耐UV性。聚氨酯复合材料体系可以例如用于生产运动制品,例如网球架,冬季运动设备或水上运动设备,例如冲浪板或运动船只,家具例如桌子、操作表面或商业展示用结构,或在交通工具结构中的光稳定性部件,例如分隔壁、地板、屋顶和衬里部件,用于物品运输车辆的装载区域覆盖件,冷却容器的外壁,用于风力发电机的叶片,飞机部件例如副翼或方向舵,或用于建筑工业中,例如作为隔热板,尤其是在建筑外部或作为具有隔热性能的负载构件。尤其是,可以使用本发明的聚氨酯复合材料体系生产冲浪板、风浪板和风筝滑板,其具有低的材料密度和因此在水中的浮力高,并同时具有高的总硬度、表面硬度、刚度和挠曲强度。
本发明的优点将通过以下实施例说明:
为了制备本发明的硬质泡沫1,、聚氨酯复合材料体系2和对比实施例C1,所用的多元醇是与催化剂、稳定剂和发泡剂按照表1所示一起搅拌的,随后与异氰酸酯混合,并将反应混合物倒入具有基底面积为225mmx225mm的箱子中并在其中发泡。为了制备增强硬质泡沫,将反应混合物引入相同的箱子,但其中现在含有许多层的类型Unifilo U809-450的玻璃纤维毡。穿透进入毡的反应混合物,并且这些毡与在箱子中上升的泡沫一起溶胀,并均匀地分布在泡沫的整个高度上。通过发泡剂设定了45g/l的恒定泡沫密度。用1mm厚的层涂覆硬质泡沫的操作是使用表2所示的聚脲喷涂体系涂料1进行的。
根据DIN 53421于25℃沿着与发泡方向平行的方向检测压缩强度和压缩E模量。表面硬度是使用Tiratest 2602仪器用直径为20mm的半球形压头于25℃检测的。在这里,检测沿着与发泡方向平行的方向将压头压入试样10mm所需要的力。
表1
表2
聚醚胺,MW 2000 | 60 |
聚醚胺,MW 400 | 20 |
二乙基甲苯二胺 | 20 |
基于MDI的预聚物,NCO含量15% | 112 |
使用以下原料:
多元醇1:基于糖的聚醚醇,OH值=500mg KOH/g,粘度=8000mPas
多元醇2:基于甘油的聚醚醇,OH值=400mg KOH/g,粘度=350mPas
多元醇3:基于邻苯二甲酸酐/二甘醇的聚酯醇,OH值=300mg KOH/g,
粘度=1000mPas
异氰酸酯:聚合的亚甲基二(苯基异氰酸酯)(PMDI),粘度=200mPas
粘度数据在每种情况下表示在25°C下的粘度。
稳定剂:含硅的泡沫稳定剂,来自Evonik Goldschmidt GmbH
表1显示出本发明的硬质聚氨酯复合材料体系具有高的压缩强度,尤其是表面硬度,并具有高的压缩E模量。
Claims (16)
1.一种聚氨酯复合材料体系,其含有硬质聚氨酯泡沫以及由压实聚氨酯或压实聚脲组成的涂料,其中所述硬质聚氨酯泡沫含有形成网络的多孔三维增强材料,其中所述网络封闭了硬质聚氨酯泡沫的体积的至少50%,或所述硬质聚氨酯泡沫含有至少两层的多孔的至少二维增强材料,其中在两个相邻层之间或在泡沫的上层和上侧之间或在泡沫的下层和下侧之间的最大距离与在两层之间或在泡沫的上层和上侧之间或在泡沫的下层和下侧之间的最小距离相比所相差的倍数是不超过4倍。
2.权利要求1的聚氨酯复合材料体系,其中增强材料是玻璃纤维毡。
3.权利要求1或2的聚氨酯复合材料体系,其中硬质聚氨酯泡沫可以如下获得:
将(a)多异氰酸酯,
(b)具有对异氰酸酯有活性的基团的化合物,
(c)包含水的发泡剂,
(d)含有叔胺的催化剂混合物,和任选地
(e)其它添加剂,
混合以形成反应混合物,将所述反应混合物施用到增强材料上,并固化所述反应混合物。
4.权利要求3的聚氨酯复合材料体系,其中具有对异氰酸酯有活性的基团的化合物(b)含有具有官能度为4或更大且在25℃下的粘度为10,000mPas或更低的聚醚醇(b1),和含有具有官能度为3.5或更低且在25℃下的粘度为600mPas或更低的聚醚醇(b2)。
5.权利要求4的聚氨酯复合材料体系,其中具有对异氰酸酯有活性的基团的化合物(b)不仅含有聚醚醇(b1)和聚醚醇(b2),而且含有具有在25℃下的粘度为2000mPas或更低的聚酯醇(b3)、扩链剂(b4)和任选地交联剂(b5)。
6.权利要求1或2的聚氨酯复合材料体系,其中硬质聚氨酯泡沫含有PMDI作为异氰酸酯组分。
7.权利要求1或2的聚氨酯复合材料体系,其中硬质聚氨酯泡沫具有30-500g/l的密度。
8.权利要求1或2的聚氨酯复合材料体系,其中硬质聚氨酯泡沫具有的非密度依赖性的压缩强度是至少5*10-4MPa*(l/g)1.6。
9.权利要求8的聚氨酯复合材料体系,其中硬质聚氨酯泡沫具有的非密度依赖性的压缩强度是至少5.5*10-4MPa*(l/g)1.6。
10.权利要求1或2的聚氨酯复合材料体系,其中硬质聚氨酯泡沫具有的非密度依赖性的压缩E模量是至少8*10-3MPa*(l/g)1.7。
11.权利要求10的聚氨酯复合材料体系,其中硬质聚氨酯泡沫具有的非密度依赖性的压缩E模量是至少9.5*10-3MPa*(l/g)1.7。
12.权利要求1或2的聚氨酯复合材料体系,其中涂料是压实聚脲,其可以通过将具有至少两个异氰酸酯基团的化合物与具有至少两个伯氨基或仲氨基的化合物混合获得。
13.一种制备权利要求1-12中任一项的聚氨酯复合材料体系的方法,其中用压实聚氨酯或压实聚脲涂覆硬质聚氨酯泡沫,所述硬质聚氨酯泡沫含有形成网络的多孔三维增强材料,其中所述网络封闭了硬质聚氨酯泡沫的体积的至少50%,或所述硬质聚氨酯泡沫含有至少一层的多孔的至少二维增强材料,其中在两个相邻层之间或在泡沫的上层和上侧之间或在泡沫的下层和下侧之间的最大距离与在两层之间或在泡沫的上层和上侧之间或在泡沫的下层和下侧之间的最小距离相比所相差的倍数是不超过4倍。
14.权利要求13的方法,其中硬质聚氨酯泡沫是通过将用于制备压实聚氨酯或压实聚脲的反应混合物喷涂到硬质聚氨酯泡沫上来涂覆的。
15.一种制备权利要求1-12中任一项的聚氨酯复合材料体系的方法,其中将用于制备压实聚氨酯或压实聚脲的反应混合物喷涂到模具的部分或模具的全部表面上,并随后将增强材料和用于制备硬质聚氨酯泡沫的反应混合物引入模具中,并使其反应完全。
16.一种运动制品、用于交通工具结构的部件、冷却容器、用于风力发电机的叶片、用于飞机的部件、家具物品或用于建筑工业中的构件,它们含有权利要求1-12中任一项的聚氨酯复合材料体系。
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PCT/EP2010/069907 WO2011073325A1 (de) | 2009-12-18 | 2010-12-16 | Polyurethanverbundsystem mit hoher druckfestigkeit und steifigkeit |
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EP2584567B1 (de) | 2011-10-20 | 2016-02-10 | Nexans | Leicht abzumantelndes elektrisches kabel |
EP2623532A1 (de) * | 2012-01-31 | 2013-08-07 | Technische Fachhochschule Wildau | Polyurethan-Kompositwerkstoff und Verfahren zur Herstellung desselben |
CN102617825B (zh) * | 2012-03-16 | 2014-07-23 | 青岛宇田化工有限公司 | 连续长纤维增强复合材料及其制造方法 |
US20130343822A1 (en) * | 2012-06-20 | 2013-12-26 | Mark Swarny | Liner system for mines, tunnels and other ground structures |
US20140017963A1 (en) * | 2012-07-11 | 2014-01-16 | Shlomo Lazarovits | Paddleboard and paddle devices and systems |
CN104045806B (zh) * | 2013-03-13 | 2021-01-19 | 科思创德国股份有限公司 | 用于制备聚氨酯复合材料的聚氨酯组合物 |
FR3008630B1 (fr) * | 2013-07-16 | 2015-12-18 | Filippo Mariagiuseppina Di | Traitement de surface des materiaux plastiques expanses |
RU2534536C1 (ru) * | 2013-07-23 | 2014-11-27 | АйПи ПОЛИУРЕТАН ТЕКНОЛОДЖИС ЛТД | Полиоловая композиция для получения жесткого пенополиуретана для производства скорлуп |
EP3071404B1 (en) * | 2013-11-19 | 2023-12-27 | LM Wind Power A/S | A system and method for manufacturing a wind turbine blade component |
FR3026049B1 (fr) * | 2014-09-24 | 2018-01-05 | Societe Francaise D'assainissement - Sfa | Structure en materiau composite multicouche, son procede de mise en œuvre et article sanitaire ainsi realise |
FR3073168B1 (fr) * | 2017-11-06 | 2020-12-11 | Boreal Dev | Procede de fabrication d'une piece aeronautique tridimensionnelle |
CN109849442B (zh) * | 2018-12-29 | 2021-05-07 | 浙江华江科技股份有限公司 | 一种轻质高强度低气味备胎盖板及其制备方法 |
CN109823015A (zh) * | 2018-12-29 | 2019-05-31 | 浙江华江科技股份有限公司 | 一种聚氨酯三维增强gmt复合板及其制备方法 |
CN112280290A (zh) * | 2020-11-19 | 2021-01-29 | 嘉兴学院 | 一种阻燃型聚氨酯硬质泡沫及其制备方法 |
CN113773463B (zh) * | 2021-08-16 | 2023-01-06 | 佳化化学科技发展(上海)有限公司 | 聚醚组合物和以其为原料的聚氨酯硬泡及其制备方法 |
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EP2512768B1 (de) | 2016-11-16 |
BR112012014986A2 (pt) | 2016-04-05 |
BR112012014986B1 (pt) | 2019-10-08 |
CA2784241A1 (en) | 2011-06-23 |
MY159951A (en) | 2017-02-15 |
CA2784241C (en) | 2019-01-08 |
EP2512768A1 (de) | 2012-10-24 |
US10125230B2 (en) | 2018-11-13 |
MX2012006873A (es) | 2012-07-25 |
ZA201205263B (en) | 2013-09-25 |
NZ600956A (en) | 2013-05-31 |
WO2011073325A1 (de) | 2011-06-23 |
AU2010332880A1 (en) | 2012-07-19 |
CN102844165A (zh) | 2012-12-26 |
AU2010332880B2 (en) | 2016-01-07 |
US20120263937A1 (en) | 2012-10-18 |
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