CN103339375B - 用于制备更具体用于风力发电系统的叶片的聚氨酯芯层泡沫 - Google Patents
用于制备更具体用于风力发电系统的叶片的聚氨酯芯层泡沫 Download PDFInfo
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- CN103339375B CN103339375B CN201180066373.3A CN201180066373A CN103339375B CN 103339375 B CN103339375 B CN 103339375B CN 201180066373 A CN201180066373 A CN 201180066373A CN 103339375 B CN103339375 B CN 103339375B
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- isocyanates
- weight
- polyurethane foam
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- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 1
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Abstract
本发明涉及一种增强聚氨酯泡沫，其具有高于50至300g/L的密度，高于7.5*10-4MPa(L/g)1.6的与密度无关的压缩强度，高于1.7*10-2MPa(L/g)1.7的与密度无关的压缩弹性模量，高于6.4*10-4MPa(L/g)1.6的与密度无关的拉伸强度，高于2.4*10-2MPa(L/g)1.7的与密度无关的拉伸弹性模量，高于1.25*10-3MPa(L/g)1.6的与密度无关的弯曲强度，高于1.75*10-2MPa(L/g)1.7的与密度无关的弯曲弹性模量，该增强聚氨酯泡沫通过以下方法获得：混合(a)聚异氰酸酯与(b)具有异氰酸酯-反应性基团的化合物、(c)包含水的发泡剂、以及任选地(d)催化剂和(e)其他添加剂，以形成反应混合物以及固化该反应混合物，其中待固化的反应混合物包含1重量%-40重量%的中空微球和/或施用于能够在所述聚氨酯泡沫中形成二维或三维网状结构的多孔增强剂(f)，具有异氰酸酯-反应性基团的化合物(b)包含聚醚多元醇(b1)、聚酯多元醇(b2)、增链剂(b3)和任选地交联剂(b4)和芳族聚醚二醇(b5)，而且组分(b)包含的聚酯多元醇(b2)、增链剂(b3)和芳族聚醚二醇(b5)部分为至少50重量%，基于组分(b)的总重量计。本发明还涉及一种制备这种增强聚氨酯泡沫的方法和其作为叶片或机翼内部的承重、刚性平面元件的增强泡沫的用途，以及作为液化天然气罐的隔热材料的用途。
Description
本发明涉及一种增强聚氨酯泡沫，其具有高于50至300g/L的密度，高于7.5*10- 4MPa(L/g)1.6的与密度无关的压缩强度，高于1.7*10-2MPa(L/g)1.7的与密度无关的压缩弹性模量，高于6.4*10-4MPa(L/g)1.6的与密度无关的拉伸强度，高于2.4*10-2MPa(L/g)1.7的与密度无关的拉伸弹性模量，高于1.25*10-3MPa(L/g)1.6的与密度无关的弯曲强度，高于1.75*10-2MPa(L/g)1.7的与密度无关的弯曲弹性模量，该聚氨酯泡沫通过以下方法获得：混合(a)聚异氰酸酯与(b)具有异氰酸酯-反应性基团的化合物、(c)包括水的发泡剂、以及任选地(d)催化剂和(e)其他添加剂，以形成反应混合物以及固化该反应混合物，其中待固化的反应混合物包含1重量%至40重量%的中空微球和/或应用于能够在该聚氨酯泡沫中形成二维或三维网状结构的多孔增强剂(f)，具有异氰酸酯-反应性基团的化合物(b)包含聚醚多元醇（polyetherol）(b1)、聚酯多元醇（polyesterol）(b2)、增链剂(b3)和任选地交联剂(b4)和芳族聚醚二醇(b5)，而且所述组分(b)包含的聚酯多元醇(b2)、增链剂(b3)和芳族聚醚二醇(b5)部分等于至少50重量%，基于所述组分(b)的总重量计。本发明还涉及用于制备这种增强聚氨酯泡沫的方法和其作为机翼或叶片内部的承重、刚性平面元件的增强泡沫以及作为液化天然气罐的隔热材料的用途。
基于聚氨酯的增强硬质泡沫是已知的而且例如在WO2010/066635或WO2008/083996中有描述。这些泡沫例如被用作液化天然气(LNG)罐的隔热材料，而且更具体地用在LNG运输工具中。这种隔热材料必须符合高机械要求，因为除隔热功能外，它们还执行与LNG罐有关的承重功能。此时特别需要高压缩强度、高压缩弹性模量以及高剪切强度。尽管现有泡沫已经提供了非常好的性能，但是仍期望对这些性能的改进，更具体为弹性的改进。其结果是，LNG运输工具在例如汹涌的海面上运输的过程中遭遇的震动可更有效地吸收。
具有非常好的机械性能的硬质泡沫具有其他应用。例如，这些泡沫用在运动飞行器如滑翔机的机翼中，或者用于例如风力发电系统的动叶片中。目前，最通常用于加固叶片和机翼的材料为轻木、基于交联聚氯乙烯的泡沫和基于聚对苯二甲酸乙二醇酯的泡沫。
用于加固叶片和机翼的这些材料的缺点在于轻木是天然资源，因此较昂贵且不能广泛应用；基于交联聚氯乙烯的泡沫的制备方法非常不方便而且由于高的卤素含量对环境有负面影响；基于聚对苯二甲酸乙二醇酯的泡沫的机械性能需要改进。
此外，风力发电特别表现出倾向于带有更长叶片的越来越大的汽轮机系统的趋势。这种特征通常涉及将承重玻璃纤维/活性树脂层施用至增强泡沫。所使用的活性树脂主要为环氧树脂或聚酯树脂。这些树脂放出反应热，或需要被加热。
越来越大的叶片增加了对这些用作外层的承重玻璃纤维/活性树脂体系的机械要求。为了满足这些机械要求，通常所做的是增加外层的厚度。其结果是，在固化中所涉及的温度升高。
特别是受提高生产量的驱使，还努力缩短制备过程和从而缩短叶片的固化时间，更具体为外层的固化时间。例如通过升高固化温度来做到这些。然而，特别是基于交联聚氯乙烯的增强泡沫一旦加热到高温（如高于75℃的温度）就会产生机械稳定性的永久损失。
风力发电动叶片的另一个基本要求特别是它们能弹性地响应高负重，这是因为它们能挠曲到特定程度。对机翼也是如此。同时，增强泡沫应该能够经受由挠曲/弯曲所产生的剪切力。
叶片或机翼中的增强泡沫的一个重要标准是低重。叶片末端可达到大约100m/s的圆周速率，这可产生大的径向力。为了使这些最小化，期望一种具有极低重量的增强泡沫。
本发明的一个目的是提供具有非常好的机械性能的泡沫，例如高压缩强度和模量，还有拉伸强度和模量和弯曲强度和模量，以及高抗剪强度和高弹性和低密度。该泡沫还应具有高的弯曲弹性模量和高的热稳定性而且该泡沫的制备应该简单以及应该能以环境友好的方式循环和/或处理。
我们已发现该目的通过一种增强聚氨酯泡沫实现，其具有高于50至300g/L的密度，高于7.5*10-4MPa(L/g)1.6的与密度无关的压缩强度，高于1.7*10-2MPa(L/g)1.7的与密度无关的压缩弹性模量，高于6.4*10-4MPa(L/g)1.6的拉伸强度，高于2.4*10-2MPa(L/g)1.7、优选3.0*10-2*10-2MPa(L/g)1.7的拉伸弹性模量，高于1.25*10-3MPa(L/g)1.6、优选1.50*10-3MPa(L/g)1.6的弯曲强度和高于1.75*10-2MPa(L/g)1.7的弯曲弹性模量，该聚氨酯泡沫通过以下方法获得：混合(a)聚异氰酸酯与(b)具有异氰酸酯-反应性基团的化合物、(c)包括水的发泡剂、以及任选地(d)催化剂和(e)其他添加剂，以形成反应混合物以及固化该反应混合物，其中待固化的反应混合物包含1重量%至40重量%的中空微球和/或应用于能够在该聚氨酯泡沫中形成二维或三维网状结构的多孔增强剂(f)，具有异氰酸酯-反应性基团的化合物(b)包含聚醚多元醇(b1)、聚酯多元醇(b2)、增链剂(b3)和任选地交联剂(b4)和芳族聚醚二醇(b5)，而且所述组分(b)包含的聚酯多元醇(b2)、增链剂(b3)和芳族聚醚二醇(b5)部分等于至少50重量%，基于所述组分(b)的总重量计。
本文中压缩值和拉伸值在与发泡方向垂直和平行的方向测量而且总是按照由(x*y*z)1/3计算的空间平均值来记录/说明。弯曲值和剪切强度总是在与发泡方向垂直的方向测量并记录/说明。
本文的增强聚氨酯泡沫为其中所述中空微球和/或增强剂(f)以层状的形式或者以层与中空微球的形式存在的增强聚氨酯泡沫。或者，可以存在形成网状结构的三维增强剂，任选地与中空微球结合。优选地，增强剂为至少两层的形式，其在泡沫中均匀分布而且优选与发泡的方向垂直。“均匀分布”在此可理解为是指两个相邻层之间、或上层与泡沫的顶面之间、或下层与泡沫的底面之间的最大间隔分别与两层之间、或上层与泡沫的顶面之间、或下层与泡沫的底面之间的最小间隔相差不超过4倍，优选不超过2倍以及更特别不超过1.5倍。
增强剂(f)例如可由已知的玻璃纤维、芳族聚酰胺纤维、碳纤维或聚合物纤维构成，例如玻璃纤维垫。这些增强材料还可由这些建筑材料的结合物构成。例如，三维增强剂可由通过聚酰胺纤维结合在一起的两种玻璃纤维垫构成。
根据泡沫的密度和所期望的增强效果，层状增强剂的使用量为至少3.5-35kg每m3泡沫。这意味着，例如，在面积为1m2、高度为3cm和泡沫密度为100g/L的泡沫体的情况下，一层增强剂具有450g/m2的密度。层状的增强剂还可具有三维尺度（three-dimensionalextent）。中空微球、层状增强剂和/或三维增强剂的结合也是可行的。
增强剂(f)和/或中空微球的比例优选在1-40重量%、更特别2-20重量%的范围内，基于包含增强剂(f)和/或中空微球的硬质聚氨酯泡沫的总重量计。
在本发明的聚氨酯复合体系中所使用的增强硬质泡沫具有根据DIN53421/DINENISO604高于7.5*10-4MPa(L/g)1.6的与密度无关的压缩强度，高于1.7*10-2MPa(L/g)1.7的与密度无关的压缩弹性模量，根据DIN53292/DINENISO527-1高于6.4*10-4MPa(L/g)1.6的与密度无关的拉伸强度，高于2.4*10-2MPa(L/g)1.7、优选3.0*10-2MPa(L/g)1.7的与密度无关的拉伸弹性模量，根据DIN53423高于1.25*10-3MPa(L/g)1.6、优选1.50*10-3MPa(L/g)1.6的与密度无关的弯曲强度以及高于1.75*10-2MPa(L/g)1.7的与密度无关的弯曲弹性模量。本发明的增强聚氨酯硬质泡沫优选还具有高于3.8*10-4MPa(L/g)1.6、更优选5.5*10-4MPa(L/g)1.6的与密度无关的剪切强度。与密度无关的压缩强度根据压缩强度*(密度)-1.6来计算，与密度无关的压缩E-模量根据压缩E-模量*(密度)-1.7来计算。对于用在本发明聚氨酯复合体系中的增强硬质泡沫这意味着——对于100g/L的泡沫密度——至少1.19MPa且优选至少1.2MPa的压缩强度，以及至少42.7MPa且优选至少44MPa的压缩E-模量，至少1.0MPa的拉伸强度和至少60.3MPa且优选至少75MPa的拉伸E-模量，至少1.98MPa且优选至少2.38MPa的弯曲强度和至少44MPa弯曲E-模量。本发明所使用的增强聚氨酯硬质泡沫的密度高于50g/L至300g/L、优选在80g/L至250g/L的范围内且更优选在100g/L至220g/L的范围内。
本发明增强硬质泡沫优选还具有超过100℃、更优选超过120℃以及甚至更优选超过140℃的软化温度。软化温度为在根据DINENISO6721-2的动态力学分析(DMA)中本发明的聚氨酯硬质泡沫展示出最大损耗模量G’’的温度。高的软化温度使得可在没有泡沫结构改变的情况下在更高温度下制备本发明的复合元件，泡沫结构改变可导致机械性能显著受损。
对于异氰酸酯(a)，可使用所有常用的脂族的、脂环族的和优选芳族的二异氰酸酯和/或多异氰酸酯，其具有在25℃测量的小于600mPas、优选小于500mPas和更优选小于350mPas的粘度。特别优选使用甲苯二异氰酸酯(TDI)、二苯基甲烷二异氰酸酯(MDI)和二苯基甲烷二异氰酸酯(MDI)与聚合的二苯基甲烷二异氰酸酯(PMDI)的混合物作为异氰酸酯。特别使用二苯基甲烷二异氰酸酯与PMDI的混合物。这些特别优选的异氰酸酯可以全部或部分用脲二酮、氨基甲酸酯、异氰脲酸酯、碳二亚胺、脲基甲酸酯改性，且优选用氨基甲酸酯基团改性。
有用的异氰酸酯(a)还包括预聚物以及上述异氰酸酯和预聚物的混合物。这些预聚物可从上述异氰酸酯与下述聚醚、聚酯或两者获得，且具有14重量%至32重量%以及优选22重量%至30重量%的NCO含量。
对于具有异氰酸酯-反应性基团的化合物(b)，可使用任何具有至少两个异氰酸酯-反应性基团例如OH、SH、NH和碳酸基团的化合物。本文这些化合物(b)包括聚醚多元醇(b1)、聚酯多元醇(b2)、增链剂(b3)和任选地交联剂(b4)和/或芳族聚醚二醇(b5)，但这应理解为意指交联剂(b4)和芳族聚醚二醇(b5)可彼此独立地包括在内。
聚醚多元醇(b1)可通过已知的方法获得，例如在催化剂存在下通过环氧烷烃的阴离子聚合，该聚合通过用至少一种包含2-8个、优选2-6个键合形式的活性氢原子的起始分子引发。适用的催化剂包括碱金属氢氧化物，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——在阳离子聚合情况下——路易斯酸，例如五氯化锑、三氟化硼合乙醚和漂白土。有用的催化剂还包括双金属氰化物（称作DMC催化剂）以及胺基催化剂。
所使用的环氧烷烃优选包含一种或多种在亚烷基基团中有2-4个碳原子的化合物，例如四氢呋喃、1,3-环氧丙烷、1,2-环氧丁烷、或2,3-环氧丁烷，各自单独或以混合物的形式，且优选环氧乙烷和/或1,2-环氧丙烷。
有用的起始分子包括乙二醇、二乙二醇、丙二醇、二丙二醇、甘油、三羟甲基丙烷、季戊四醇、糖衍生物例如蔗糖、己糖醇衍生物例如山梨糖醇、甲胺、乙胺、异丙胺、丁胺、苄胺、苯胺、甲苯胺、甲苯二胺、萘胺、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、三乙醇胺以及其他二-或多元醇或单-或者多官能胺。
优选，聚醚多元醇(b1)包括至少一种聚醚多元醇(b1a)，其平均官能度为3.5以上、优选在3.6-8的范围内且更具体在3.8-6的范围，以及25℃下粘度为15000mPas以下、优选10000mPas以下。分子量优选在300-900g/mol范围内、更优选400-800g/mol且更具体为450-750g/mol。由聚醚多元醇(b1a)对组分(b)的总重量所贡献的比例优选为20-50重量%、更优选25-40重量%。聚醚多元醇(b1)还可包括0-20重量%且优选1-10重量%的聚醚多元醇(b1b)，该聚醚多元醇(b1b)的分子量高于300至3000g/mol、优选在400-2500g/mol的范围且更具体在400-1000g/mol的范围。该聚醚多元醇(b1b)优选具有在1.8-3.0范围内、更优选在1.95-2.2范围内的平均官能度且优选具有仲OH基团。
有用的聚酯醇(b2)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的缩合获得，所述多官能醇为例如乙二醇、二乙二醇、丁二醇、三羟甲基丙烷、甘油或季戊四醇，所述多官能羧酸为例如琥珀酸、戊二酸、己二酸、辛二酸、壬二酸、癸二酸、癸烷二羧酸、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所提及的酸的酸酐。优选使用芳族二酸例如邻苯二甲酸、间苯二甲酸和/或对苯二甲酸以及它们的酸酐作为酸组分，使用乙二醇、二乙二醇、1,4-丁二醇和/或甘油作为醇组分。
在另一个实施方案中，聚酯醇(b2)可通过由相应的单体酯（如对苯二甲酸二甲酯）或聚合酯（如聚对苯二甲酸乙二醇酯(PET)）置换二酸或其酸酐获得。
制备这些聚酯的适合的原料还包括疏水性物质。该疏水性物质包括不溶于水的物质，该不溶于水的物质含有非极性有机基团并且具有至少一个选自羟基、羧酸、羧酸酯或其混合物的活性基团。该疏水性物质的当量优选为130-1000g/mol。可以使用脂肪酸，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、向日葵油、大豆油、椰子油、橄榄油或妥尔油。当聚酯包含疏水性物质时，疏水性物质占聚酯醇总单体含量的比例优选在1-30mol%的范围、更优选为4-15mol%的范围。这些包含疏水性物质的聚酯以下称为疏水性聚酯。基于聚酯多元醇(b2)的总重量计，疏水性聚酯的比例优选在0-80重量%的范围内、更优选在5-60重量%的范围内。
有用的聚酯多元醇(b2)优选具有1.5-5、更优选1.8-3.5、甚至更优选1.9-2.2的平均官能度，而且在25℃下的粘度优选低于3000mPas、更优选低于2500mPas。分子量优选在290-1000g/mol范围内、更优选在320-800g/mol范围内而且甚至更优选在340-650g/mol范围内。
在一个优选的实施方案中，基于组分(b)的总重量计，组分(b)包含至少50重量%的聚酯多元醇(b2)。在这种情况下，极特别优选聚酯(b2)包含疏水性聚酯。
具有异氰酸酯-反应性基团的化合物(b)还包含增链剂(b3)和/或交联剂(b4)。所使用的增链剂和/或交联剂更具体为二官能的或三官能的胺或醇，更具体为二醇、三醇或这两者，各自分子量小于300g/mol、优选在60-300g/mol范围内、更优选在60-250g/mol范围内。已知二官能化合物为增链剂(b3)且已知三-或更高官能的化合物为交联剂(b4)。可能的实例包括具有2-14个碳原子、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、二乙二醇、三乙二醇、二丙二醇、三丙二醇、1,4-丁二醇、1,6-己二醇和双(2-羟乙基)氢醌；三醇和更高级的多元醇，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、N,N,N’,N’-四(2-羟丙基)乙二胺和基于环氧乙烷和/或1,2-环氧丙烷的低分子量的含羟基聚环氧烷，和上述作为起始分子的二醇和/或三醇。
交联剂(b4)占组分(b)总重量的比例优选在0-40重量%范围内、更优选在1-30重量%范围内。用于液化天然气罐的隔热泡沫的制备特别优选使用0.5-8重量%、更具体1-5重量%的交联剂，而且该交联剂优选甘油。
增链剂(b3)具有平均至少30%、优选至少40%、更优选至少50%以及甚至更优选至少60%仲OH基。增链剂(b3)可包含单个化合物或混合物。增链剂(b3)优选单独包含单丙二醇、二丙二醇、三丙二醇和/或2,3-丁二醇或任选与各自或彼此或与其他增链剂混合。在一个特别优选的实施方案中，二丙二醇与第二种增链剂一起用作增链剂(b3)，该第二种增链剂为例如2,3-丁二醇、单丙二醇或二乙二醇。交联剂(b4)优选包含1,2,4-三羟基环己烷、1,3,5-三羟基环己烷、甘油、N,N,N’,N’-四(2-羟丙基)乙二胺和/或三羟甲基丙烷。优选用作交联剂的是甘油或N,N,N’,N’-四(2-羟丙基)乙二胺，更具体为甘油。
芳族聚醚二醇(b5)为芳族二醇（优选双酚A）和环氧乙烷和/或环氧丙烷的烷氧基化产物。因此芳族聚醚二醇(b5)具有优选的官能度2以及高于300g/mol且优选高于300g/mol至600g/mol的数均分子量。
组分(b)例如可包括5-50重量%的增链剂(b3)。包含在组分(b)中的增链剂(b3)的量优选在8-50重量%范围内、更优选在10-30重量%范围内。
对本发明而言重要的是组分(b)包含一定比例的聚酯多元醇(b2)、增链剂(b3)和芳族聚醚多元醇(b5)，基于组分(b)的总重量计，该比例等于至少50重量%、优选在50-80重量%范围内、更优选在55-75重量%范围内、甚至更优选在60-70重量%范围内。组分(b1)-(b5)可各自包含单个组分或混合物，在这种情况下所使用的化合物各自落入(b1)-(b5)定义范围内。
优选地，组分(b)包括至少50重量%、更优选至少55-85重量%、甚至更优选60-75重量%的具有两个或三个异氰酸酯-反应性基团的化合物。这些具有两个或三个异氰酸酯-反应性基团的化合物优选具有低于2500g/mol的分子量，更优选为低于1000g/mol，且更具体为低于800g/mol。这些化合物的数均分子量优选不超过500g/mol、更优选在150-450g/mol范围内，更具体在250-450g/mol范围内。
由聚醚多元醇(b1)、(b2)、(b3)和任选地(b4)和(b5)对具有异氰酸酯-反应性基团的化合物(b)所贡献的比例优选至少80重量%、更优选至少90重量%、更具体为100重量%，基于具有异氰酸酯-反应性基团的化合物(b)的总重量计。
组分(b)的总摩尔官能度优选小于3.0、更优选为2.0-2.9且甚至更优选为2.4-2.8。组分(b)的平均OH数优选大于300mgKOH/g、更优选为350-1000mgKOH/g且甚至更优选为400-600mgKOH/g。
当异氰酸酯预聚物被用作异氰酸酯(a)时，具有异氰酸酯-反应性基团的化合物(b)的水平被认为是包括用于制备异氰酸酯预聚物的具有异氰酸酯-反应性基团的化合物(b)。
发泡剂(c)包括含有水的发泡剂。水可用作单独的发泡剂或可与其他发泡剂结合使用。发泡剂(c)的水含量优选大于40重量%、更优选大于60重量%、甚至更优选大于80重量%，基于发泡剂(c)的总重量计。更具体而言，水用作单独的发泡剂。当使用除水之外的其他发泡剂时，例如可使用含氯氟烃、含氟烃（hydrofluorocarbon）、烃、酸和液态/溶解二氧化碳。优选地，基于发泡剂(c)的总重量计，发泡剂(c)包含少于50重量%、优选小于20重量%、更优选小于10重量%、甚至更优选0重量%的含氯氟烃、含氟烃和/或烃。另一个实施方案可包括使用水和甲酸和/或二氧化碳的混合物作为发泡剂(c)。为了简化发泡剂在多元醇组分中的分散，发泡剂(c)可与极性化合物如二丙二醇掺和。
发泡剂(c)以这样的量使用：使组分(a)-(e)反应形成的硬质聚氨酯泡沫的密度（包含增强剂(f)和/或中空微球）在高于50g/L-300g/L的范围、优选在80g/L-250g/L的范围内且更优选在100g/L-220g/L的范围内。当本发明的硬质聚氨酯泡沫仅用中空玻璃球来增强时，发泡剂(c)以这样的量使用：使组分(a)-(e)反应形成的硬质聚氨酯泡沫的密度（包含中空微球）在高于30g/L至250g/L的范围内、优选在60g/L至低于160g/L的范围内、且更优选在80g/L至低于110g/L的范围内。
催化剂(d)可为加速异氰酸酯-水反应或异氰酸酯-多元醇反应的任何化合物。这些化合物是已知的且例如在“Kunststoffhandbuch,第7卷,Polyurethane”，CarlHanserVerlag，第3版1993，3.4.1章中有描述。这些包括胺基催化剂和基于有机金属化合物的催化剂。
基于有机金属化合物的有用的催化剂包括例如有机锡化合物，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（例如二乙酸二丁基锡、二月桂酸二丁基锡、马来酸二丁基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。
催化剂(d)优选为包含至少一种叔胺的混合物。这些叔胺通常包含还可具有异氰酸酯-反应性基团如OH、NH或NH2基团的化合物。一些最频繁使用的催化剂为双(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、二甲基苄胺、三乙胺、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、二甲基氨基丙胺、N-乙基吗啉、二氮杂双环十一碳烯和二氮杂双环壬烯。当期望催化剂低迁移出本发明泡沫和/或低排放VOC化合物时，也可以使用可结合的催化剂。而且也可完全省掉催化剂。
中空微球优选选自中空热塑性微球、中空玻璃微球和由玻璃陶瓷制成的中空微球。由玻璃和玻璃陶瓷制成的中空微球的实例分别为购自ZeelanIndustries的市售中空微球Z-LiteW-1000和购自3M的Scotchlite以及购自PQCorporation的CEL300和650。
优选使用中空热塑性微球。本文使用的中空热塑性微球对本领域技术人员来说是已知的而且自GmbH(EssenGermany)以产品名称Expancel(AkzoNobel)市售可得。此处，就中空微球而言，它们的壳由基于丙烯腈的共聚物构成，而且它们的空隙空间由吹入气体填充。通常，未膨胀的中空微球的直径在6-45μm的范围内且密度在1000-1300g/L的范围内。吹入气体通常包含挥发性烃类，例如丁烷、戊烷、己烷、庚烷、异丁烯、异戊烷、新戊烷、环丙烷、环丁烷和环丙烷。如果需要，这些中空球还可用任何其他的低沸点溶剂制备和生产。当中空微球被加热时，气体将提高内部压力，聚合物层软化且膨胀过程开始。在完全膨胀之后，中空微球的直径将增加至原始直径的3-4倍而且其体积超过原始体积40倍。膨胀后的密度为30g/L。膨胀温度通常在80-190℃范围内。冷却之后，热塑性材料再次固化，保持膨胀体积。
能够在聚氨酯泡沫中形成层状，即二维或三维网状结构的多孔增强剂(f)可以是使硬质聚氨酯泡沫获得甚至更高的机械稳定性并且在本发明的硬质聚氨酯泡沫中以二维或三维网状结构形式存在的任何物质。形成二维网状结构的增强剂的实例为纤维垫，例如玻璃纤维垫，三维增强剂的实例为多个相互交联的纤维垫或优选同样相互交联的粗纱。在本发明上下文中，对于具有多孔形式的增强剂，用于制备硬质聚氨酯泡沫的反应混合物必须能够渗透进入和穿透该增强剂同时完全润湿该增强剂。形成三维增强剂的物质（如粗纱或缎带/带材/韧带）优选例如通过交织或互联而彼此接合。为形成三维增强剂，两个以上二维增强剂如纤维垫还可连接在一起。此外，合股纤维或织股纤维（例如纤维辫绳）可用作三维增强剂。
这种在聚氨酯泡沫中能够形成层状或三维网状结构的多孔增强剂(f)是例如基于纤维的织物或针织品。优选使用的多孔、二维增强剂的实例为纤维垫，例如玻璃纤维垫、芳族聚酰胺纤维垫或碳纤维垫或包括塑料的纤维垫或包括这些材料的缎带/带材/韧带，优选玻璃纤维垫，例如购自OwensCorningVetrotex的U801或U809。也可使用玻璃纤维粗纱垫。基于组分(a)-(f)的总重量计，增强剂(f)的比例优选为1-40重量%，更优选为2-20重量%。
可能的其他添加剂(e)包括阻燃剂、增塑剂、泡沫稳定剂、其他填料和其他添加剂，例如抗氧化剂。优选地，至少使用阻燃剂或增塑剂。
所使用的阻燃剂可以是现有技术中通常所知的阻燃剂。适合的阻燃剂包括例如溴化醚(IxolB251)、溴化醇（例如二溴新戊醇、三溴新戊醇和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），或其混合物。
除了上述卤素取代磷酸酯，无机阻燃剂例如红磷、包含红磷的制剂、可膨胀石墨、水合氧化铝、三氧化锑、五氧化二砷、聚磷酸铵和硫酸钙或氰尿酸衍生物（例如三聚氰胺）、或至少两种阻燃剂的混合物（例如聚磷酸铵和三聚氰胺）、以及任选地淀粉也可用来使根据本发明制备的聚氨酯硬质泡沫具有阻燃性。
乙烷膦酸二乙酯(DEEP)、磷酸三乙酯(TEP)、丙基膦酸二甲酯(DMPP)、磷酸甲苯二苯酯(DPC)以及其他化合物可用作其他液体无卤阻燃剂。
本文的阻燃剂的使用量优选在0%-25%的范围，基于组分(b)-(e)的总重量计。
有用的增塑剂包括，例如多元羧酸、优选二元羧酸与一元醇的酯。这些酯的酸组分衍生自例如琥珀酸、间苯二甲酸、对苯二甲酸、偏苯三酸、柠檬酸、邻苯二甲酸酐、四氢和/或六氢邻苯二甲酸酐、内亚甲基四氢邻苯二甲酸酐、戊二酸酐、马来酸酐、富马酸和/或二聚和/或三聚脂肪酸（例如油酸），任选与单体脂肪酸掺和。这些酯的醇组分衍生自例如支链和/或未支化的具有1-20个碳原子的脂族醇，例如甲醇、乙醇、丙醇、异丙醇、正丁醇、仲丁醇、叔丁醇、戊醇的各种异构体、己醇的各种异构体、辛醇的各种异构体（例如，2-乙基己醇)、壬醇的各种异构体、癸醇的各种异构体、月桂醇的各种异构体、肉豆蔻醇的各种异构体、鲸蜡醇的各种异构体、硬脂醇的各种异构体和/或衍生自天然存在的脂肪醇和蜡质醇或通过天然存在的羧酸的氢化得到的脂肪醇和蜡质醇。作为醇组分，还可使用脂环族和/或芳族羟基化合物，例如环己醇和其同系物、苯酚、甲酚、百里酚、香芹酚、苄醇和/或苯乙醇。有用的增塑剂还包括一元酸酸与二元醇的酯，例如texanol酯醇，例如2,2,4-三甲基-1,3-戊二醇二异丁酸酯(TXIB)或2,2,4-三甲基-1,3-戊二醇二苯甲酸酯；由低聚亚烷基二醇与烷基羧酸形成的二酯，例如三甘醇二己酸酯或四甘醇二庚酸酯和类似化合物。
有用的增塑剂还包括上述醇与磷酸的酯。任选地，可使用卤化醇的磷酸酯，例如磷酸三氯乙酯。在卤化醇的磷酸酯的情况下，除增塑剂效果外还可获得阻燃效果。应理解还可使用上述醇与羧酸的混合酯。
增塑剂还可是所谓的聚合增塑剂，例如己二酸、癸二酸和/或邻苯二甲酸的聚酯。
还可使用苯酚的烷基磺酸酯（例如石蜡烃磺酸苯酯）和芳族磺酰胺（例如乙基甲苯磺酰胺）作为增塑剂。类似地，聚醚（例如三甘醇二甲醚）可用作增塑剂。
增塑剂的使用量优选在0.1-15重量%，更优选在0.5-10重量%范围内，基于组分b)-e)的总重量计。含有增塑剂特别是在低温下进一步提高硬质聚氨酯泡沫的机械性能的一种方式。
泡沫稳定剂促进了在泡沫形成过程中规则孔结构的形成。实例包括含硅氧烷的泡沫稳定剂，例如硅氧烷-氧化烯共聚物和其他的有机聚硅氧烷。以及以下物质的烷氧基化产物：脂肪醇、羰基合成醇、脂肪胺、烷基苯酚、二烷基苯酚、烷基甲酚、烷基间苯二酚、萘酚、烷基萘酚、萘胺、苯胺、烷基苯胺、甲苯胺、双酚A、烷基化双酚A、聚乙烯醇；以及由以下物质形成的缩合产物的烷氧基化产物：甲醛和烷基苯酚、甲醛和二烷基苯酚、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；或者两种以上这些泡沫稳定剂的混合物。
这些泡沫稳定剂的使用量优选在0.5-4重量%、更优选1-3重量%范围内，基于组分(b)-(e)的总重量计。
其他填料——特别是增强填料——为本身已知的常规有机和无机填料。具体的实例为无机填料例如硅化（silicatic）矿物质，例如层状硅酸盐，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、重晶石和无机颜料，例如硫化镉、硫化锌以及玻璃和其他。优选使用高岭土（陶土）、硅酸铝和由硫酸钡与硅酸铝形成的共沉淀物，以及天然和合成的纤维矿物质例如硅灰石、金属纤维以及特别是不同长度的玻璃纤维，其可任选进行尺寸定型。有机填料包括例如碳、三聚氰胺、松香、环戊二烯树脂和接枝聚合物以及纤维素纤维、聚酰胺纤维、聚丙烯腈纤维、聚氨酯纤维、基于芳族和/或脂族二羧酸酯的聚酯纤维，且更具体为碳纤维。
有机和无机填料可单独或混合使用，基于组分(a)-(e)的重量计以0-30重量%、优选1-15重量%的量纳入反应混合物是有利的。就本发明而言，上述增强剂(f)和/或中空微球不看作填料且在推算比例时不包含在组分(e)中。
本发明还提供了一种用于制备增强聚氨酯泡沫的方法，包括混合(a)聚异氰酸酯与(b)具有异氰酸酯-反应性基团的化合物、(c)包含水的发泡剂、(d)催化剂混合物和任选地中空微球和(e)其他添加剂以形成反应混合物，将该反应混合物施用于至少一种增强剂(f)且固化该反应混合物，其中具有异氰酸酯-反应性基团的化合物(b)包含聚醚多元醇(b1)、聚酯多元醇(b2)、增链剂(b3)和任选地交联剂(b4)和芳族聚醚二醇(b5)，而且所述组分(b)包含的聚酯多元醇(b2)和增链剂(b3)部分等于至少50重量%，基于所述组分(b)的总重量计。本发明的方法采用上述原料。所述聚氨酯反应混合物优选渗透进入增强剂且将其均匀润湿。然后发泡聚氨酯反应混合物导致增强剂在泡沫中的均匀分布，其中层状增强剂的多个层例如与发泡的方向垂直取向。
本发明硬质聚氨酯泡沫优选在带上以连续的方式生产。为此，优选将组分(b)-(d)和任选地中空玻璃微球和(e)混合在一起形成多元醇组分。然后优选将这些与异氰酸酯组分(a)在低压混合设备、处于低于100bar的减压下的高压混合设备或高压机器中混合。或者，组分(a)-(d)和任选地中空微球和(e)可各自单独引入混合设备中。这样获得的反应混合物随后被放在增强剂(f)上（优选玻璃纤维垫），所述增强剂(f)优选从多个（例如4-10，优选5、6或7个）转鼓连续铺展至带上，在所述带上形成相应数目的层。然后所获得的泡沫优选在带上固化到这样的程度：其可无损坏地被切成块。这可发生在高温下，例如在通过烘箱的过程中。所获得的泡沫块然后优选进一步存储从而可获得充分的机械强度。
另一种制备本发明硬质聚氨酯泡沫的方式为在模具中分批发泡所述反应混合物。在这种情况下，本发明的增强剂可在反应混合物之前或同时被引入模具中。
所获得的硬质聚氨酯泡沫然后被切成用于进一步加工所需的形状。
异氰酸酯(a)和具有异氰酸酯-反应性基团的化合物(b)、含有水的发泡剂(c)和任选地催化剂(d)和其他添加剂(e)优选以这样的量反应：使异氰酸酯指数在100-400范围内，优选在100-200范围内，更优选在100-150范围内。
用于本发明目的的异氰酸酯指数为异氰酸酯基团与异氰酸酯-反应性基团的化学计量比再乘以100。异氰酸酯-反应性基团为在反应混合物中存在的任何异氰酸酯-反应性基团，包括化学发泡剂，但是不包含异氰酸酯基团本身。
特别有利的是本发明反应混合物快速渗透进入增强剂(f)，这有利于在所得到的硬质聚氨酯泡沫中实现增强剂(f)的均匀分布。另一个优势在于本发明反应混合物的长的乳稠时间（creamtime）和短的反应时间。
本发明增强聚氨酯泡沫展示出优异的机械性能，例如高的压缩强度和模量以及拉伸强度和模量和弯曲强度和模量，以及高的剪切强度和高弹性和低密度。本发明增强聚氨酯泡沫还具有高的弯曲弹性模量和高的热稳定性而且可以简单和环境友好的方式获得。也可环境友好地处理所述聚氨酯泡沫。例如，聚氨酯泡沫可例如通过酵解而分解成其初始化合物，其可作为原材料被再利用。
本发明的泡沫优选用作结构夹层组件中的泡沫，结构夹层组件的外层优选由纤维增强树脂构成。所使用的树脂例如可为已知的环氧树脂、聚酯树脂或聚氨酯树脂，其以常规的方式被层压到聚氨酯泡沫上。或者，本发明的聚氨酯泡沫还可粘附在这种外层上或在这种外层上制备。纤维增强树脂可用作模具或模具的部件。除了纤维增强树脂之外，外层还可由热塑性材料、木质材料或金属构成。外层可包住部分泡沫或整个泡沫。当泡沫被外层包围时，本发明的泡沫可部分填充或完全填充结构夹层组件的内部。当仅部分结构夹层组件被本发明的泡沫填充时，该泡沫优选在结构夹层组件中形成增强层，其中结构夹层组件内部的剩余空间优选构成未填充的气体空间。
因此，本发明的增强聚氨酯泡沫可在叶片例如动叶片和飞机的机翼中用作增强泡沫，更具体用作芯层泡沫。芯层泡沫为叶片或机翼中的增强层，其或者填充整个芯，或者在中空叶片的情况下形成内部增强层，该内部增强层置于表面材料之下，该表面材料例如由玻璃纤维树脂构成。本发明的结构夹层组件优选用作叶片或机翼。结构夹层组件其他可能的用途为船体或承重、刚性平面元件。
本发明的增强聚氨酯泡沫还可用作液化天然气罐的隔热材料，特别是在船上时。
以下实施例说明本发明。
增强聚氨酯硬质泡沫的制备(变量1):
表1：
| 1 | 2 | V1 | V2 | V3 | |
| 聚醚1 | 40 | 40 | 40 | ||
| 聚醚2 | 25 | 25 | 25 | ||
| 聚醚3 | 28 | 28 | |||
| 聚醚4 | 20 | 20 | |||
| 聚酯1 | 37 | 17 | 25 | 25 | 25 |
| 增链剂1 | 12 | 12 | 10 | 10 | 10 |
| 芳族二醇 | 20 | ||||
| 水 | 2 | 2 | 1.0 | 1.0 | 1.0 |
| 催化剂1 | 0.08 | 0.08 | 0.08 | ||
| 稳定剂1 | 1 | 1 | 1.5 | 1.5 | 1.5 |
| 异氰酸酯1 | 126 | 126 | 126 | ||
| 异氰酸酯2 | 142 | 152 | |||
| 玻璃纤维垫层 | 0 | 0 | 0 | 7 | |
| 中空玻璃球 | 17 | 8.2 | 8.0 |
| 泡沫密度（g/L） | 100 | 100 | 100 | 112 | 100 |
| 压缩强度（MPa） | 1.42 | 1.39 | 0.91 | 1.15 | 0.84 |
| 压缩E-模量（MPa） | 52.1 | 43.6 | 24.8 | 43.1 | 23.4 |
| 拉伸强度（MPa） | 1.11 | 1.16 | n.d. | n.d. | n.d. |
| 拉伸E-模量（MPa） | 63.4 | 62.4 | n.d. | n.d. | n.d. |
| 3-点弯曲强度（MPa） | 2.03 | 2.11 | 1.62 | 1.91 | n.d. |
| 3-点弯曲E-模量（MPa） | 55.1 | 51.2 | n.d. | n.d. | n.d. |
| 剪切强度（MPa） | 0.62 | 0.69 | 0.83 | 0.79 | 0.41 |
使用以下原料：
聚醚1：蔗糖/甘油基聚环氧丙烷，Fn=4.5，数均分子量=515g/mol，25℃下粘度=8000mPa*s
聚醚2:聚丙二醇，Fn=2，数均分子量=1100g/mol,25℃下的粘度=150MPa*s
聚醚3:乙二胺基聚环氧丙烷，Fn=3.9，数均分子量=470g/mol,25℃下的粘度=4975MPa*s
聚醚4:乙二胺基聚环氧丙烷，Fn=4.0,数均分子量=300g/mol
聚醚4:山梨糖醇基聚环氧丙烷，OH数=490mgKOH/g(购自BASFSE的3422)
聚酯1:邻苯二甲酸酐/二乙二醇基，Fn=2，数均分子量=360g/mol
聚酯2:芳族聚酯多元醇，OH数=240mgKOH/g(购自BASFSE的8007)
增链剂1:丙二醇基,Fn=2,分子量=134g/mol
芳族二醇:双酚-A-引发的基于环氧丙烷的聚醚多元醇,Fn=2,数均分子量400g/mol
增链剂2:丙二醇基,Fn=2,MW=190g/mol
增链剂3:二乙二醇
催化剂1:脂族叔胺
稳定剂1:用于聚氨酯泡沫的含硅氧烷的稳定剂
异氰酸酯1:二苯基甲烷二异氰酸酯与聚合的二苯基甲烷二异氰酸酯的混合物,25℃下粘度为200mPa*s
异氰酸酯2:95.2份的二苯基甲烷二异氰酸酯与聚合的二苯基甲烷二异氰酸酯的混合物和4.8份由1份己二酸、6份油酸和2份季戊四醇形成的聚酯多元醇所形成的预聚物，25℃下的粘度为250mPa*s。
玻璃纤维垫:玻璃纤维的连续切毡，购自OwensCorningVetrotex的U809-450
中空玻璃球:购自3M的iM30K中空玻璃球，密度为600g/L且平均直径为15μm
增强聚氨酯硬质泡沫的制备(变量2):
表2：
| V4 | V5 | 3 | V1 | V2 | V6 | V7 | V8 | |
| 聚醚1 | 31 | 31 | 31 | 40 | 40 | 39 | ||
| 聚醚 2 | 25 | 25 | 24 | |||||
| 聚醚4 | 20 | 20 | ||||||
| 聚酯1 | 56 | 28 | 28 | 25 | 25 | 24 | ||
| 聚酯2 | 40 | 40 | ||||||
| 增链剂 1 | 10 | 10 | 10 | 10 | 10 | 10 | ||
| 增链剂 2 | 28 | 28 | ||||||
| 增链剂3 | 40 | 40 | ||||||
| 甘油 | 3 | 3 | 3 | 3 | 11 --> | |||
| 水 | 1.4 | 1.45 | 1.45 | 1.0 | 1.0 | 1.05 | 1.6 | |
| 1,1,1,3,3-五氟丙烷 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 10 |
| 催化剂 1 | 0.11 | 0.07 | 0.07 | 0.08 | 0.08 | 0.08 | 0.12 | 0.13 |
| 稳定剂1 | 2.0 | 2.0 | 2.0 | 1.5 | 1.5 | 1.5 | 2 | 2 |
| 异氰酸酯 1 | 166 | 183 | 183 | 126 | 126 | 140 | 209 | 187 |
两表中记录了以重量份计的所使用的物质的量。为了按照本发明实施例1-3和对比(V)实施例1-8制备硬质泡沫，按照表1或表2所使用的多元醇与催化剂、稳定剂和发泡剂一起搅拌，然后再与异氰酸酯混合，之后将反应混合物倒入底部面积为225mmx225mm的箱中，在其中发泡。选择的水的量为使未增强的泡沫具有100g/L的自由泡沫密度。在表中记录的泡沫密度是基于包括增强剂（如果使用的话）的泡沫立方体的总密度。为按照本发明实施例3和对比实施例2制备增强硬质泡沫，将反应该混合物引入同样的箱中，但是现在所述箱中包含多层玻璃纤维垫。反应混合物渗透进入这些垫中且随着泡沫在箱中升起，垫膨胀且在整个泡沫高度内均匀分布。为按照本发明实施例1和2以及对比实施例3制备增强硬质泡沫，将中空的玻璃球与所使用的多元醇、催化剂、稳定剂以及发泡剂一起搅拌，然后同对比实施例4-8以及对比实施例1一样进行。为了测定机械性能，从泡沫的内部锯出立方体状的试验样品。当这些试验样品具有除100g/L之外的密度时，将在机械测试中所获得的值转化成100g/L的密度。
如在表1和表2中所示，本发明的配方导致了硬质聚氨酯泡沫相比迄今已知的抗压和抗剪切硬质泡沫具有特别高的机械性能。即使没有使用增强剂，这些硬质聚氨酯泡沫也表现出这种聚氨酯泡沫已经显示良好的机械性能，如对比实施例5中明显所示。这一点在对比实施例V1和V2的对比中尤其清楚，在对比实施例V1和V2中再次制备按照WO2010/066635的实施例1的泡沫，一次采用增强剂而一次未采用增强剂。对比实施例V6展示出改进的WO2010/066635的配方，还包括交联剂甘油。该非增强泡沫的机械性能相对于按照对比实施例5的非增强泡沫的机械性能要差。根据本发明实施例与对比实施例V1和V2，聚氨酯反应混合物的处理和应用以及泡沫的视觉印象是非常好的。对比实施例V7和V8显示了根据EP2236537的实施例1制备的泡沫，一次采用物理发泡剂，一次采用发泡剂水。非增强泡沫的机械性能相对于对比实施例5的非增强泡沫的机械性能明显较差，尤其是拉伸强度、拉伸E-模量和剪切强度。此外，制备类似本发明实施例3和对比实施例V2的增强聚氨酯泡沫的尝试失败，因为对比试验V7和V8的聚氨酯反应混合物没有充分润湿玻璃纤维垫，所以在上升的泡沫中这些玻璃纤维垫没有均匀分布。
表3显示了根据本发明实施例1的增强聚氨酯硬质泡沫相对于PVC泡沫和相对于按照对比实施例1的泡沫具有明显改进的耐热性。
表3：
| 泡沫 | 交联PVC泡沫 | 对比实施例1 | 本发明实施例1 |
| 软化温度[℃] | 82℃ | 123℃ | 144℃ |
Claims (17)
1.一种增强聚氨酯泡沫，其具有高于50至300g/L的密度，高于7.5*10-4MPa(L/g)1.6的与密度无关的压缩强度，高于1.7*10-2MPa(L/g)1.7的与密度无关的压缩弹性模量，高于6.4*10-4MPa(L/g)1.6的与密度无关的拉伸强度，高于2.4*10-2MPa(L/g)1.7的与密度无关的拉伸弹性模量，高于1.25*10-3MPa(L/g)1.6的与密度无关的弯曲强度和高于1.75*10-2MPa(L/g)1.7的与密度无关的弯曲弹性模量，该增强聚氨酯泡沫通过以下方法获得：混合
a)聚异氰酸酯与
b)具有异氰酸酯-反应性基团的化合物，
c)包含水的发泡剂，以及任选地
d)催化剂和
e)其他添加剂，
以形成反应混合物以及固化该反应混合物，其中待固化的反应混合物包含1重量％-40重量％的中空微球和/或施用于能够在所述聚氨酯泡沫中形成二维或三维网状结构的多孔增强剂(f)，所述具有异氰酸酯-反应性基团的化合物(b)包含聚醚多元醇(b1)、聚酯多元醇(b2)、增链剂(b3)和任选地交联剂(b4)和芳族聚醚二醇(b5)，而且所述具有异氰酸酯-反应性基团的化合物(b)包含的聚酯多元醇(b2)、增链剂(b3)和芳族聚醚二醇(b5)部分等于至少50重量％，基于所述具有异氰酸酯-反应性基团的化合物(b)的总重量计，其中所述增链剂(b3)为包含至少30％仲OH基的二醇，增链剂(b3)部分为5重量％-50重量％，基于所述具有异氰酸酯-反应性基团的化合物(b)的总重量计。
2.如权利要求1所述的增强聚氨酯泡沫，其中至少50重量％的所述具有异氰酸酯-反应性基团的化合物(b)包含具有2个或3个异氰酸酯-反应性基团的化合物。
3.权利要求2的增强聚氨酯泡沫，其中所述具有2个或3个异氰酸酯-反应性基团的化合物的分子量小于2500g/mol。
4.如权利要求2或3所述的增强聚氨酯泡沫，其中所述具有2个或3个异氰酸酯-反应性基团的化合物的数均分子量小于500g/mol。
5.如权利要求1所述的增强聚氨酯泡沫，其中所述具有异氰酸酯-反应性基团的化合物(b)包含至少50重量％的具有2个异氰酸酯-反应性基团且分子量小于2500g/mol的化合物，基于所述具有异氰酸酯-反应性基团的化合物(b)的总重量计。
6.如权利要求1所述的增强聚氨酯泡沫，其中聚酯多元醇(b2)的比例为至少50重量％，基于所述具有异氰酸酯-反应性基团的化合物(b)的总重量计。
7.如权利要求1所述的增强聚氨酯泡沫，其中所述聚酯多元醇(b2)包含疏水性聚酯多元醇。
8.如权利要求1所述的增强聚氨酯泡沫，其中交联剂(b4)的比例在1-30重量％范围内，基于所述具有异氰酸酯-反应性基团的化合物(b)的总重量计。
9.如权利要求1所述的增强聚氨酯泡沫，其中增链剂(b3)的比例在8-50重量％范围内，基于所述具有异氰酸酯-反应性基团的化合物(b)的总重量计，交联剂(b4)的比例在0-10重量％范围内，基于所述具有异氰酸酯-反应性基团的化合物(b)的总重量计。
10.如权利要求1所述的增强聚氨酯泡沫，其中所述具有异氰酸酯-反应性基团的化合物(b)的平均官能度低于3.0。
11.权利要求1所述的增强聚氨酯泡沫，其中所述聚醚多元醇(b1)的平均官能度在3.6-8范围内。
12.如权利要求1所述的增强聚氨酯泡沫，其中所述增强剂(f)包含玻璃纤维垫。
13.如权利要求1所述的增强聚氨酯泡沫，其中所述增强剂(f)包含中空微球。
14.一种制备增强聚氨酯泡沫的方法，包括混合
a)聚异氰酸酯与
b)具有异氰酸酯-反应性基团的化合物，
c)包含水的发泡剂，以及任选地
d)催化剂和
e)其他添加剂，
以形成反应混合物以及固化该反应混合物，其中待固化的反应混合物包含1重量％-40重量％的中空微球和/或施用于能够在所述聚氨酯泡沫中形成二维或三维网状结构的多孔增强剂(f)，所述具有异氰酸酯-反应性基团的化合物(b)包含聚醚多元醇(b1)、聚酯多元醇(b2)、增链剂(b3)和任选地交联剂(b4)和芳族聚醚二醇(b5)，而且所述具有异氰酸酯-反应性基团的化合物(b)包含的聚酯多元醇(b2)、增链剂(b3)和芳族聚醚二醇(b5)部分等于至少50重量％，基于所述具有异氰酸酯-反应性基团的化合物(b)的总重量计，其中所述增链剂(b3)为包含至少30％仲OH基的二醇，增链剂(b3)部分为5重量％-50重量％，基于所述具有异氰酸酯-反应性基团的化合物(b)的总重量计。
15.如权利要求1-13中任一项所述的增强聚氨酯泡沫在结构夹层组件中的用途。
16.如权利要求1-13中任一项所述的增强聚氨酯泡沫作为叶片和机翼中的增强泡沫或作为液化天然气罐的隔热材料的用途。
17.如权利要求16所述的用途，其中所述叶片为风力发电系统的动叶片。
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP10193263A EP2461022A1 (de) | 2010-12-01 | 2010-12-01 | Kernschäume aus Polyurethan für die Herstellung von Flügeln, insbesondere für Windkraftanlagen |
| EP10193263.0 | 2010-12-01 | ||
| PCT/EP2011/071400 WO2012072687A1 (de) | 2010-12-01 | 2011-11-30 | Kernschäume aus polyurethan für die herstellung von flügeln, insbesondere für windkraftanlagen |
Publications (2)
| Publication Number | Publication Date |
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| CN103339375A CN103339375A (zh) | 2013-10-02 |
| CN103339375B true CN103339375B (zh) | 2016-07-06 |
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| CN201180066373.3A Active CN103339375B (zh) | 2010-12-01 | 2011-11-30 | 用于制备更具体用于风力发电系统的叶片的聚氨酯芯层泡沫 |
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|---|---|
| EP (2) | EP2461022A1 (zh) |
| CN (1) | CN103339375B (zh) |
| AU (1) | AU2011335016B2 (zh) |
| BR (1) | BR112013013577A2 (zh) |
| CA (1) | CA2818999A1 (zh) |
| DK (1) | DK2646683T3 (zh) |
| ES (1) | ES2522865T3 (zh) |
| MX (1) | MX343463B (zh) |
| PT (1) | PT2646683E (zh) |
| RU (1) | RU2596189C2 (zh) |
| WO (1) | WO2012072687A1 (zh) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MA35040B1 (fr) * | 2011-04-15 | 2014-04-03 | Basf Se | Procédé de fabrication de mousses de polyuréthane dures |
| US9334383B2 (en) | 2011-04-15 | 2016-05-10 | Basf Se | Process for producing rigid polyurethane foams |
| EP2708354A1 (de) * | 2012-09-12 | 2014-03-19 | Basf Se | Verfahren zur Herstellung von Sandwichelementen |
| EP3147303A1 (en) * | 2015-09-25 | 2017-03-29 | Ernesto Monton Martin | Solid surface product comprising aliphatic isocyanate and process for manufacturing thereof |
| CN108713933A (zh) * | 2018-05-24 | 2018-10-30 | 福建大方睡眠科技股份有限公司 | 一种散热性能好的抗菌床垫及其制作方法 |
| CN118103423A (zh) * | 2021-10-18 | 2024-05-28 | 巴斯夫欧洲公司 | 基于芳香族聚酯多元醇和环氧乙烷基聚醚多元醇的改进型聚异氰脲酸酯硬质泡沫塑料的制备方法 |
| WO2023138967A1 (en) * | 2022-01-18 | 2023-07-27 | Basf Se | Gasket for a transition piece of a wind turbine and method for mounting such a gasket |
| FR3135268A1 (fr) * | 2022-05-03 | 2023-11-10 | Gaztransport Et Technigaz | Formulation d’une mousse de polyurethane/polyisocyanurate |
| TW202348668A (zh) * | 2022-06-10 | 2023-12-16 | 美商陶氏全球科技有限責任公司 | 剛性聚胺甲酸酯發泡體配方及製造適用於低溫應用之纖維強化聚胺甲酸酯發泡體之方法 |
| CN115536800A (zh) * | 2022-11-01 | 2022-12-30 | 中车长春轨道客车股份有限公司 | 一种硬质聚氨酯泡沫及其制备方法 |
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| DE3435458A1 (de) * | 1984-09-27 | 1986-06-12 | Erich Herter | Windturbine |
| CN1404503A (zh) * | 2000-02-25 | 2003-03-19 | 爱赛克斯特种产品公司 | 硬质聚氨酯泡沫塑料 |
| CN101578312A (zh) * | 2007-01-09 | 2009-11-11 | 巴斯夫欧洲公司 | 用于液化天然气罐绝热的水发泡硬质泡沫 |
| EP2236537A2 (de) * | 2009-04-01 | 2010-10-06 | Astrium GmbH | Polyurethanschaum zur thermalen Isolation bei Tiefsttemperaturen |
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| US3878634A (en) * | 1973-03-19 | 1975-04-22 | Jacob R Quimpo | Floating fishing device |
| US5478494A (en) * | 1993-09-22 | 1995-12-26 | Basf Corporation | Polyol composition having good flow and formic acid blown rigid polyurethane foams made thereby having good dimensional stability |
| UA61089C2 (uk) * | 1996-11-08 | 2003-11-17 | Хантсмен Ай Сі Ай Кемікалз, Ллс | Спосіб одержання жорстких та еластичних пінополіуретанових матеріалів |
| CA2394169C (en) * | 1999-12-16 | 2010-02-09 | Bayer Aktiengesellschaft | Method for producing soft to semi-rigid polyurethane integral foamed materials |
| EP1219674A1 (en) * | 2000-12-29 | 2002-07-03 | Huntsman International Llc | Process for making polyurethane integral skin foams |
| CA2534237A1 (fr) * | 2005-03-04 | 2006-09-04 | Gaz Transport Et Technigaz | Mousse de polyurethanne/polyisocyanurate renforcee de fibres de verre |
| CA2745920A1 (en) | 2008-12-10 | 2010-06-17 | Basf Se | Water-blown rigid foams with improved mechanical properties at low temperatures |
| US9258986B2 (en) * | 2010-11-22 | 2016-02-16 | Justice Tackle & Co., Llc | Chambered leader lure |
-
2010
- 2010-12-01 EP EP10193263A patent/EP2461022A1/de not_active Ceased
-
2011
- 2011-11-30 CA CA2818999A patent/CA2818999A1/en not_active Abandoned
- 2011-11-30 MX MX2013006026A patent/MX343463B/es active IP Right Grant
- 2011-11-30 AU AU2011335016A patent/AU2011335016B2/en not_active Ceased
- 2011-11-30 EP EP11796944.4A patent/EP2646683B1/de active Active
- 2011-11-30 RU RU2013129606/04A patent/RU2596189C2/ru not_active IP Right Cessation
- 2011-11-30 PT PT117969444T patent/PT2646683E/pt unknown
- 2011-11-30 CN CN201180066373.3A patent/CN103339375B/zh active Active
- 2011-11-30 BR BR112013013577A patent/BR112013013577A2/pt not_active IP Right Cessation
- 2011-11-30 WO PCT/EP2011/071400 patent/WO2012072687A1/de active Application Filing
- 2011-11-30 ES ES11796944.4T patent/ES2522865T3/es active Active
- 2011-11-30 DK DK11796944.4T patent/DK2646683T3/en active
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|---|---|---|---|---|
| DE3435458A1 (de) * | 1984-09-27 | 1986-06-12 | Erich Herter | Windturbine |
| CN1404503A (zh) * | 2000-02-25 | 2003-03-19 | 爱赛克斯特种产品公司 | 硬质聚氨酯泡沫塑料 |
| CN101578312A (zh) * | 2007-01-09 | 2009-11-11 | 巴斯夫欧洲公司 | 用于液化天然气罐绝热的水发泡硬质泡沫 |
| EP2236537A2 (de) * | 2009-04-01 | 2010-10-06 | Astrium GmbH | Polyurethanschaum zur thermalen Isolation bei Tiefsttemperaturen |
Also Published As
| Publication number | Publication date |
|---|---|
| RU2013129606A (ru) | 2015-01-10 |
| EP2461022A1 (de) | 2012-06-06 |
| ES2522865T3 (es) | 2014-11-18 |
| MX343463B (es) | 2016-11-07 |
| CN103339375A (zh) | 2013-10-02 |
| EP2646683B1 (de) | 2014-09-10 |
| DK2646683T3 (en) | 2014-12-15 |
| WO2012072687A1 (de) | 2012-06-07 |
| AU2011335016B2 (en) | 2016-05-12 |
| MX2013006026A (es) | 2013-07-29 |
| AU2011335016A1 (en) | 2013-06-27 |
| BR112013013577A2 (pt) | 2016-09-06 |
| EP2646683A1 (de) | 2013-10-09 |
| RU2596189C2 (ru) | 2016-08-27 |
| PT2646683E (pt) | 2014-10-27 |
| CA2818999A1 (en) | 2012-06-07 |
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