CN102307922B - 低温机械性能改善的水发泡硬质泡沫塑料 - Google Patents
低温机械性能改善的水发泡硬质泡沫塑料 Download PDFInfo
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- CN102307922B CN102307922B CN200980156381XA CN200980156381A CN102307922B CN 102307922 B CN102307922 B CN 102307922B CN 200980156381X A CN200980156381X A CN 200980156381XA CN 200980156381 A CN200980156381 A CN 200980156381A CN 102307922 B CN102307922 B CN 102307922B
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Abstract
本发明涉及一种硬质聚氨酯泡沫塑料,其可通过混合(a)异氰酸酯、(b)含有对异氰酸酯具有反应活性的基团的化合物、(c)含水的发泡剂、(d)催化剂和任选地(e)其它添加剂形成反应混合物,将该反应混合物施用于增强材料并使该反应混合物硬化而制得;其中异氰酸酯(a)在25℃时的粘度不超过500mPas,含有对异氰酸酯具有反应活性的基团的化合物(b)包括官能度不小于4且25℃时的粘度不高于10 000mPas的聚醚醇(b1)、官能度不大于3.5且25℃时的粘度不高于600mPas的聚醚醇(b2)、25℃时的粘度不高于2000mPas的聚酯醇(b3)、含有至少30%仲羟基的增链剂(b4)和任选地交联剂(b5)。本发明还涉及该硬质聚氨酯泡沫塑料的制备方法及该硬质聚氨酯泡沫用于液化天然气罐隔热的用途。
Description
本发明涉及一种硬质聚氨酯泡沫塑料,其可通过混合(a)异氰酸酯、(b)含有对异氰酸酯具有反应活性的基团的化合物、(c)含水的发泡剂、(d)催化剂和任选地(e)其它添加剂形成反应混合物,将该反应混合物施用于增强材料并使其固化而制得;其中异氰酸酯(a)在25℃时的粘度不超过500mPas,含有对异氰酸酯具有反应活性的基团的化合物(b)包括官能度不小于4且25℃时的粘度不高于10000mPas的聚醚醇(b1)、官能度不大于3.5且25℃时的粘度不高于600mPas的聚醚醇(b2)、25℃时的粘度不高于2000mPas的聚酯醇(b3)、含有至少30%仲羟基的增链剂(b4)和任选地交联剂(b5)。本发明还涉及该硬质聚氨酯泡沫塑料的制备方法及该硬质聚氨酯泡沫塑料用于液化天然气罐隔热的用途。
本发明的更多的实施方案在权利要求书、说明书和实施例中有描述。不言而喻,上面提及的和接下来仍然将要解释的本发明主题的特征,不仅可用于各自所示的组合而且还可在不超出本发明范围的情形下用于其它组合。
除了石油,天然气也是我们这个时代的最重要能量来源之一。但是将气从来源处带到消费者身边通常需要运输很长的距离。这例如经由管道来实现。但是经由管道运输天然气至边远地区或运输很长的距离是非常昂贵的。另外,出于政治原因,一些国家可能不允许穿过它们的领土来铺设所述管道。在这些情况下,用天然气罐经海路运输(称为液化天然气(LNG)运输器)经常作为一种替代而被选择。为此,天然气在陆地上被液化并放置在船上的巨大储气罐内。因为天然气只能在非常低的温度约-160℃下液化、且也必须在该温度下存储和运输,因此使储气罐——尤其是船上的储气罐——尽可能好地隔热以降低由液化气蒸发造成的损失是必要的。
作为隔热材料,主要使用硬质聚氨酯泡沫塑料,因为与其它隔热材料如聚苯乙烯泡沫塑料或矿物棉相比,其具有极佳的隔热性能。
液化天然气运输器的整体隔热结构是非常复杂的。例如,储气罐的隔热不仅必须阻止天然气的蒸发,而且必须使储气罐有一定程度的稳定性。因此,除了硬质聚氨酯泡沫塑料,例如胶合板、玻璃纤维和不锈钢层也可用来稳固储气罐。
现有的储气罐主要包括一层非常薄的不锈钢隔离层,以致于主要由隔热结构提供所需稳定性。因此大部分所使用的硬质聚氨酯泡沫塑料有非常高的密度。此外,其优选地包含增强材料,通常是玻璃纤维毡片(CSM-长丝束毡),以提供必需的机械性能。为了能保证最佳的稳定性,这些长丝束毡在总泡沫塑料厚度中分布的均匀性是一个重要参数。
这类隔热结构记载于例如韩国专利文本KR2000010021和KR2000010022中,日本专利文本JP2003240198和JP2001150558中,美国专利文本US20050115248、US3319431和US3341050中,欧洲专利申请EP1698649和国际专利申请WO2008083996中。
在硬质泡沫塑料遇到大的温差和温度改变时,泡沫塑料体内会出现剪切力。因为聚氨酯泡沫塑料是热绝缘体,在泡沫塑料体内产生温度梯度,引起收缩/膨胀梯度的产生,其转而导致泡沫塑料体内产生剪切力。剪切强度对于受到横向应力的硬质泡沫塑料来说也是一个重要的特性,其例如在船舶运输液体货物时产生。为此,用于液化天然气罐隔热的硬质聚氨酯泡沫塑料必须不仅有好的机械性能如抗压强度和抗压弹性模量(杨氏模量),而且有特别高的剪切强度。
作为发泡剂,通常使用卤化发泡剂如氯氟烃和氟化烃,因为以此方式可制备出具有特别低导热性的泡沫塑料。但是氯氟烃会导致臭氧层破坏,而且氯氟烃和氟化烃都是有助于全球变暖的气体。为此,必须寻找替代品。
由于具有可燃性,诸如烃类化合物(例如戊烷)的发泡剂不是特别适合。
如果用诸如水的化学发泡剂取代诸如氟化烃的物理发泡剂,则在最终的泡沫塑料中会形成较多的尿素基团,导致泡沫塑料变得更脆(尤其是在低温时)且剪切强度降低。
本发明的目的是提供一种硬质聚氨酯泡沫塑料,该泡沫塑料适合于船运中液化天然气罐的隔热,其中用作发泡剂的氯氟烃或氟化烃已全部地或部分地被替代发泡剂取代,这种泡沫塑料有极好的机械性能(如抗压强度、抗压弹性模量和剪切强度)以及低导热性。
该目的可由以下方法制备的硬质聚氨酯泡沫塑料来实现,即混合(a)异氰酸酯、(b)含有对异氰酸酯具有反应活性的基团的化合物、(c)含水的发泡剂、(d)催化剂和任选地(e)其它添加剂形成反应混合物,将该反应混合物施用于增强材料并将反应混合物固化而制得;其中异氰酸酯(a)在25℃时的粘度不超过500mPas,含有对异氰酸酯具有反应活性的基团的化合物(b)包括官能度不小于4且25℃时的粘度不高于10000mPas的聚醚醇(b1)、官能度不大于3.5且25℃时的粘度不高于600mPas的聚醚醇(b2)、25℃时的粘度不高于2000mPas的聚酯醇(b3)、含有至少30%仲羟基的增链剂(b4)和任选地交联剂(b5)。
作为异氰酸酯(a),可使用所有常见的脂族的、脂环族的以及优选地为芳香族的二异氰酸酯和/或多异氰酸酯,其在25℃时测得的粘度小于600mPas、优选小于500mPas并且特别优选小于350mPas。特别优选甲苯二异氰酸酯(TDI)和二苯基甲烷二异氰酸酯(MDI)以及尤其是二苯基甲烷二异氰酸酯与聚二苯基甲烷二异氰酸酯(PMDI)的混合物作为异氰酸酯。这些特别优选的异氰酸酯可全部地或部分地经脲二酮(uretdione)、氨基甲酸酯、异氰脲酸酯、碳二亚胺、脲基甲酸酯和优选的氨基甲酸酯(urethane)基团修饰。
此外,预聚物以及上述异氰酸酯和预聚物的混合物可用作异氰酸酯成分。这些预聚物是由上面描述的异氰酸酯以及下面描述的聚醚和/或聚酯制得的,其NCO含量为从14至32重量%、优选从22至30重量%。
作为含有对异氰酸酯具有反应活性的基团的化合物(b),可使用所有含有至少两个对异氰酸酯具有反应活性的基团的化合物,所述基团例如OH-、SH-、NH-和CH-酸性基团。通常使用含有2至8个对异氰酸酯具有反应活性的氢原子的聚醚醇和/或聚酯醇。这些化合物中OH数目通常在30至850mgKOH/g范围内、优选80至600mgKOH/g。
聚醚醇可用已知的方法制得,例如在催化剂存在下加入至少一种含有2至8个——优选2至6个——以结合形式存在的活泼氢原子的起始分子(starter molecule)的环氧烷烃的阴离子聚合反应。作为催化剂,可使用碱金属氢氧化物如氢氧化钠或氢氧化钾,或碱金属醇盐如甲醇钠、乙醇钠或乙醇钾、或异丙醇钾,或在阳离子聚合反应中作为催化剂可使用路易斯酸如五氯化锑、醚合三氟化硼或漂白土。此外,被称为DMC催化剂的双金属氰化物也可用作催化剂。
作为环氧烷烃,优选使用一种或更多种亚烷基部分含有2至4个碳原子的化合物,例如四氢呋喃、1,3-环氧丙烷、1,2-或2,3-环氧丁烷(其各自均可单独或以混合物形式使用),并且优选为环氧乙烷和/或1,2-环氧丙烷。
可选用的起始分子有例如:乙二醇、二甘醇、丙三醇、三羟甲基丙烷、季戊四醇、糖类衍生物(如蔗糖)、己糖醇衍生物(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、三乙醇胺和其它二羟基或多羟基醇或者单官能或多官能胺类。
使用的聚酯醇通常由以下物质发生缩合反应而制得:含有2至12个碳原子的多官能醇类,例如乙二醇、二甘醇、丁二醇、三羟甲基丙烷、丙三醇或季戊四醇;与含有2至12个碳原子的多官能羧酸,如丁二酸、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、间苯二酸、对苯二酸、萘二羧酸的各种异构体或所述酸的酸酐。
作为聚酯制备中的其它起始材料,也可伴随使用疏水性材料。疏水性材料是包括非极性有机基团和至少一个反应基团的非水溶性材料,这些反应基团选自羟基、羧酸、羧酸酯和它们的混合物。这些疏水性材料的当量优选在130至1000g/mol范围内。例如可使用脂肪酸,如硬脂酸、油酸、棕榈酸、月桂酸或亚油酸;和油脂类,如蓖麻油、玉米油、葵花油、大豆油、椰子油、橄榄油或松浆油。如果聚酯含有疏水性材料,则该疏水性材料占整个聚酯醇单体含量的1至30mol%、特别优选从4至15mol%。
使用的聚酯醇优选官能度为1.5至5,尤其优选为1.8–3.5,并且特别是从1.9至2.2。
含有对异氰酸酯具有反应活性的基团的化合物(b)还包括增链剂和/或交联剂。作为增链剂和/或交联剂,尤其使用双官能或三官能胺类和醇类,特别是二醇和/或三醇,所述物质的分子量各自小于350、优选从60至300、并且特别是从60至250。在此,双官能化合物称为增链剂,三官能或更多官能化合物称为交联剂。例如可使用含有2至14个、优选2至10个碳原子的脂族的、脂环族的和/或芳香族二醇,例如乙二醇、1,2-、1,3-丙二醇、1,2-、1,3-戊二醇、1,10-癸二醇、1,2-、1,3-、1,4-二羟基环己烷、二甘醇、三甘醇、双丙甘醇、三丙二醇、1,4-丁二醇、1,6-己二醇和二(2-羟乙基)对苯二酚;三元醇,如1,2,4-、1,3,5-三羟基环己烷、丙三醇和三羟甲基丙烷以及基于环氧乙烷和/或1,2-环氧丙烷以及上面提到的二醇和/或三醇作为起始分子的低分子量的含有羟基的聚环氧烷。
对于本发明而言重要的是,含有对异氰酸酯具有反应活性的基团的化合物(b)包括官能度不小于4且25℃时的粘度不高于10000mPas的聚醚醇(b1)、官能度不大于3.5(优选不大于3)且25℃时的粘度不高于600mPas(优选不高于500mPas)的聚醚醇(b2)、25℃时的粘度不高于2000mPas的聚酯醇(b3)、增链剂(b4)和任选地交联剂(b5)。作为成分(b1)至(b5),各自可使用单独的化合物或混合物,其中使用的每个化合物都依照(b1)至(b5)的定义。
增链剂(b4)平均含有至少30%、优选至少40%、特别优选至少50%且特别是至少60%的仲羟基。增链剂(b4)可以是单独的化合物或混合物。增链剂(b4)优选地包括双丙甘醇、三丙二醇和/或2,3-丁二醇,所述物质单独或任选地互相混合或与其它增链剂混合使用。例如,在一个特别优选的实施方案中,双丙甘醇与另一种增链剂(如2,3-丁二醇、单丙二醇或二甘醇)一起作为增链剂(b4)使用。
在另一个实施方案中,含有对异氰酸酯具有反应活性的基团的化合物(b)除聚醚醇(b1)、聚醚醇(b2)、聚酯醇(b3)和增链剂(b4)外还包括交联剂(b5)。作为交联剂,优先使用1,2,4-、1,3,5-三羟基环己烷、丙三醇和/或三羟甲基丙烷。优先使用丙三醇作为交联剂。
成分(b1)的比例优选为从25至70重量%、特别优选从25至55重量%、特别是30至50重量%,基于成分(b)的总重量。
成分(b2)的比例优选为从10至40重量%、特别优选为从15至35重量%,基于成分(b)的总重量。
成分(b3)的比例优选为从15至50重量%、特别优选为从20至40重量%,基于成分(b)的总重量。
成分(b)中增链剂(b4)的比例优选为从1至30重量%、特别优选为从5至20重量%,基于成分(b)的总重量。
成分(b)中成分(b5)的比例优选为从0至10重量%、特别优选为从1至5重量%,基于成分(b)的总重量。
在一个优选的实施方案中,聚醚醇(b1)的比例为从30至60重量%,增链剂(b4)的比例为从2至30重量%,各自均基于聚醇混合物b)的总重量。
含有对异氰酸酯具有反应活性的基团的化合物(b)中聚醚醇(b1)、(b2)、(b3)、(b4)和任选地(b5)的比例优选为至少80重量%、特别优选至少90重量%、特别是100重量%,基于含有对异氰酸酯具有反应活性的基团的化合物(b)的总重量。
成分(b)的总官能度优选为大于2.5,特别优选大于2.6,特别是大于2.75。成分(b)的平均羟基数目优选为大于300mgKOH/g,特别优选在320至1000mgKOH/g范围内且特别在340至600mgKOH/g范围内。
如果异氰酸酯预聚物用作异氰酸酯(a),计算含有对异氰酸酯具有反应活性的基团的化合物(b)的含量时,同时需要将用于制备异氰酸酯预聚物时使用的含有对异氰酸酯具有反应活性的基团的化合物(b)包括在内。
作为发泡剂(c),使用含水的发泡剂。在这里,水既可单独使用也可与其它发泡剂一起使用。发泡剂(c)的水含量优选为大于40重量%、特别优选为大于60重量%且极特别优选为大于80重量%,基于发泡剂(c)的总重量。特别是,水用作唯一发泡剂。如果除了水还使用其它发泡剂,可使用如氯氟烃、氟化烃、烃类、酸类和液态或溶解的二氧化碳。发泡剂(c)优选含有小于50重量%、更优选小于20重量%、尤其优选小于10重量%、特别是0重量%的氯氟烃、氟化烃和/或烃类,基于发泡剂(c)的总重量。在另一个实施方案中,水和甲酸和/或二氧化碳的混合物可用作发泡剂(c)。为了使发泡剂在聚醇成分中更易分散,发泡剂(c)可与极性化合物(如双丙甘醇)混合。
发泡剂(c)的使用量为,使由成分(a)至(e)反应制得的硬质聚氨酯泡沫塑料的密度在50-200g/l、优选80-120g/l范围内,该密度值没有将增强材料计算在内。
作为催化剂(d),可使用所有能加速异氰酸酯-水或异氰酸酯-聚醇反应的化合物。这些化合物已知并在例如“Kunststoffhandbuch,第7卷,Polyurethane”,Carl Hanser Verlag,第三版1993,3.4.1章中有描述。其中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,可使用例如:有机锡化合物,例如有机羧酸的锡(II)盐如醋酸锡(II)、辛酸锡(II)、乙基己酸锡(II)和月桂酸锡(II),和有机羧酸的二烷基锡(IV)盐如二醋酸二丁锡、二月桂酸二丁锡、马来酸二丁锡和二醋酸二辛锡;以及羧酸铋,例如新癸酸铋(III)、2-乙基己酸铋和辛酸铋;或碱金属羧酸盐,例如醋酸钾或甲酸钾。
优先使用含有至少一种叔胺的混合物作为催化剂(d)。这些叔胺通常为也含有对异氰酸酯具有反应活性的基团的化合物,如OH、NH或NH2基团。一些最常用的催化剂是二(2-二甲氨基乙基)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、二甲氨基丙胺、N-乙基吗啉、二氮杂二环十一碳烯和二氮杂二环壬烯。优先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)特别优选地包括二甲基环己胺(d1)和一种二环胺(d2)、或二甲基环己胺(d1)和一种单环胺(d3)。二甲基环己胺(d1)和二环胺(d2)、或二甲基环己胺(d1)和单环胺(d3)的比例优选为0.2-4:1,特别优选为0.5-1.5:1。环胺d2)和d3)优先选自上面提到的环胺。
二甲基环己胺(d1)、二环胺(d2)和单环胺(d3)在催化剂混合物(d)中的比例优选为至少80重量%、特别优选为至少90重量%并且尤其是100重量%,基于催化剂(d)的总重量。
作为增强材料,可使用所有能使硬质聚氨酯泡沫塑料具有更高机械稳定性的材料。这种增强材料例如是玻璃纤维、玻璃纤维毡片或碳纤维毡片,优选为玻璃纤维毡片,如来自Owens Corning Vetrotex的U801或U809。增强材料的比例优选为从5至15重量%,基于含有增强材料的硬质聚氨酯泡沫塑料的总重量。
作为其它添加剂(e),可使用阻燃剂、增塑剂、泡沫稳定剂、其它填料和其它添加剂(如抗氧化剂)。优先至少使用阻燃剂或增塑剂。
作为阻燃剂,通常可使用现有技术已知的阻燃剂。合适的阻燃剂有例如:溴化醚(Ixol B251);溴化醇,如二溴新戊醇、三溴新戊醇和PHT-4-二醇;以及氯化磷酸酯,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。
除了上面提到的卤代磷酸酯,还可使用无机阻燃剂(如红磷,含有红磷的配制剂、可膨胀石墨、氧化铝水合物、三氧化锑、五氧化二砷、多磷酸铵和硫酸钙)、或三聚氰酸的衍生物(如三聚氰胺)、或至少两种阻燃剂的混合物(如多磷酸铵和三聚氰胺)以及任选地淀粉,来使得本发明制备的硬质聚氨酯泡沫塑料具有耐燃性。
作为其它不含卤素的液态阻燃剂,可使用乙烷膦酸二乙酯(DEEP)、磷酸三乙酯(TEP)、丙基膦酸二甲酯(DMPP)、磷酸甲苯.联苯酯(DPC)和其它。
为了本发明目的,阻燃剂的使用量优选为0%至25%,基于成分(b)至(e)的总重量。
作为增塑剂,可提及的实例有多元羧酸——优选二元羧酸——与一元醇生成的酯。所述酯的酸组分可来自例如:琥珀酸、间苯二酸、对苯二酸、偏苯三酸、柠檬酸、邻苯二甲酸酐、四氢邻苯二甲酸酐和/或六氢邻苯二甲酸酐、亚内甲基四氢邻苯二甲酸酐、戊二酸酐、马来酸酐、富马酸以及/或者二聚和/或三聚脂肪酸(如油酸),上述酸任选与单体脂肪酸混合。所述酯的醇组分可来自例如含有1至20个碳原子的支化的和/或无支链的脂族醇,如甲醇、乙醇、丙醇、异丙醇、正丁醇、仲丁醇、叔丁醇以及以下醇的各种异构体:戊醇、己醇、辛醇(如2-乙基己醇)、壬醇、癸醇、月桂醇、肉豆蔻醇、十六烷醇、十八烷醇和/或自然存在或可由自然存在的羧酸氢化制得的脂肪醇和蜡醇。可使用的醇组分也包括脂环族的和/或芳香族羟基化合物,例如环己醇和其同系物、苯酚、甲酚、麝香草酚、香芹酚、苄醇和/或苯基乙醇。一元羧酸与二元醇生成的酯如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;低聚亚烷基二醇和烷基羧酸生成的二酯,如三甘醇二己酸酯或四甘醇二庚酸酯和类似化合物,也可用作增塑剂。
其它可使用的增塑剂有上面提到的醇与磷酸生成的酯。也可任选使用卤代醇的磷酸酯,如磷酸三氯乙酯。在使用卤代醇的磷酸酯的情况下,阻燃效果与增塑效果可同时达到。当然也可使用上面提到的醇与羧酸生成的混合酯。
增塑剂也可为高分子型增塑剂,如己二酸、癸二酸和/或邻苯二甲酸的聚酯。
此外,苯酚的烷基磺酸酯(如苯基石蜡磺酸酯)以及芳香族磺酰胺(如乙基甲苯磺酰胺)也可用作增塑剂。聚醚(如三甘醇二甲醚)也可用作增塑剂。
增塑剂的使用量优选为0.1至15重量%、特别优选为0.5至10重量%,基于成分b)至e)的总重量。增塑剂的加入能进一步改善硬质聚氨酯泡沫塑料的机械性能,尤其是在低温时。
术语泡沫稳定剂指的是能在泡沫塑料形成过程中促进规则泡孔结构形成的材料。可提及的实例有:含有硅氧烷的泡沫稳定剂,如硅氧烷-氧化烯共聚物和其它有机聚硅氧烷化合物。也可使用脂肪醇、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、聚乙烯醇的烷氧基化产物;以及以下物质的缩合产物的其它烷氧基化产物: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;或者这些泡沫稳定剂中两种或更多种的混合物。
泡沫稳定剂的使用量优选为从0.5至4重量%、特别优选为1至3重量%,基于成分(b)至(e)的总重量。
其它填料,尤其是增强填料,为通常使用的已知的有机和无机填料以及增强材料等。可提及的具体实例有:无机填料如硅质矿物,例如层状硅酸盐如叶蛇纹石、蛇纹石、角闪石、闪石、温石棉、滑石;金属氧化物如高岭土、氧化铝、氧化钛和氧化铁,金属盐如白垩、重晶石和无机颜料如硫化镉、硫化锌以及玻璃和其它。优先使用高岭土(陶土)、硅酸铝、硫酸钡和硅酸铝的共沉淀物以及天然的和合成的纤维状矿石(如硅灰石)、金属纤维以及尤其是任选可经胶料涂覆的不同长度的玻璃纤维。也可使用空心玻璃微球。可使用的有机填料有例如:碳、三聚氰胺、松香、环戊二烯基树脂和接枝聚合物以及纤维素纤维、聚酰胺、聚丙烯腈、聚氨酯和基于芳香族和/或脂族二羧酸酯的聚酯纤维以及尤其是碳纤维。
无机和有机填料既可单独使用也可作为混合物使用,且加入反应混合物中的有利使用量为从0.5至30重量%、优选从1至15重量%,基于成分(a)至(e)的重量。
本发明还提供了一种用于液化天然气罐的隔热材料,特别是用于船运中的液化天然气罐的隔热材料,其包括本发明的硬质聚氨酯泡沫塑料。
本发明中的硬质聚氨酯泡沫塑料优选在传送带上连续生产。为此,成分(b)至(d)和任选地(e)优选混合形成聚醇组分。然后将其与异氰酸酯成分(a)混合,优选在低压混合器、压力降低至不高于100bar的高压混合器或高压机器中进行。另一种办法是,成分(a)至(d)和任选地(e)也可各自分别加入混合装置中。将这样得到的反应混合物接下来置于增强材料上,优选玻璃纤维毡片上,所述玻璃纤维毡片优选不断地从多个(例如4-10个,优选5、6或7个)鼓上铺开至传送带上并在那里形成合适数量的层。然后所制得的泡沫塑料优选在传送带上固化以至可无损伤地将其切成片。这一过程可在高温下进行,例如在烤箱的通道中。然后所得到的泡沫塑料片优选进一步储存以获得充分的机械强度。
得到的硬质聚氨酯泡沫塑料接下来进一步加工成隔热板。为了这个目的,本发明的硬质聚氨酯泡沫塑料片被切割成固定大小,并优选粘接成胶合板和浸渍树脂的玻璃纤维毡片。然后这些聚氨酯泡沫塑料元件配以其它辅助设备(如铁板、螺丝钉和细线),用来制备最终的隔热元件,然后其可直接用于生产液化天然气罐的隔热屏障。生产这种隔热板的详细描述可例如在Finetec和Kangrim(韩国)公司的主页中找到。
异氰酸酯(a)和含有对异氰酸酯具有反应活性的基团的化合物(b)、含水的发泡剂(c)、催化剂(d)和任选地其它添加剂(e)反应时优选的加入量为,异氰酸酯指数在100至400、优选100–200、更优选100–150的范围内。
基于本发明的目的,这里的异氰酸酯指数是异氰酸酯基团和对异氰酸酯具有反应活性的基团的化学计量比再乘以100。这里的对异氰酸酯具有反应活性的基团是在反应混合物中所有对异氰酸酯具有反应活性的基团,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渗入增强材料中并从而能促进在形成的硬质聚氨酯泡沫塑料中增强材料的分布均匀性。本发明反应混合物的长乳白时间与短反应时间结合起来,也同样是有利的。
本发明的硬质聚氨酯泡沫塑料优选地用于隔热目的。本发明的硬质聚氨酯泡沫塑料特别优选地用于液化天然气罐的隔热,尤其是用于船运中(LNG运输器)。它们是机械稳定的,具有低导热性,呈现极佳的泡沫特性(如不含孔洞或裂缝),具有良好的机械性能(如剪切强度、抗压强度和极佳的杨氏模量),以上所有这些特性即使在较低温度下也如此;且增强材料层的分布均匀。本发明的增链剂混合物(b4)尤其会显著改善剪切强度。抗压强度和杨氏模量依照DIN53421/DIN EN ISO604沿垂直于和平行于发泡方向(在x/y和z方向)均进行了测量。剪切强度是依照DIN53427在25℃或-80℃下用尺寸为170mm×35mm×17mm的试样以沿垂直于发泡方向(在x/y方向)的延伸率1mm/min测量的。
本发明的优势由下面的实施例进行示例说明。
实施例
为了制备实施例1至6的本发明硬质聚氨酯泡沫塑料和对比实施例C1至C4的泡沫塑料,如表1所示将使用的聚醇与催化剂、稳定剂和发泡剂一起搅拌,然后与异氰酸酯混合并发泡来制备硬质聚氨酯泡沫塑料。通过调节催化剂的用量使得所有情况下的纤维时间都为540秒。通过发泡剂的使用使泡沫塑料的密度保持不变,为100g/l。所有情况下的异氰酸酯指数均为120。这些实施例是为了说明本发明的聚醇混合物对于泡沫性能的影响,且由于实际原因这些泡沫塑料在生产过程中未加入增强材料。
尺寸为225mm×225mm×225mm的硬质聚氨酯泡沫塑料是在模具中制备的。固化之后,将试样从该立方体锯下,用于参照所示标准来测试剪切强度、抗压强度和杨氏模量。
抗压强度和杨氏模量按DIN53421/DINENISO604取三个维度的平均值来测量。剪切强度是依照DIN53427在25℃或-80℃用尺寸为170mm×35mm×17mm的试样以沿垂直于发泡方向(在x/y方向)的延伸率1mm/min测量的。
实施例1至6和对比实施例C1至C4中用于制备硬质聚氨酯泡沫塑料的反应混合物的组成和它们的机械性能示于表1中。
表1
使用如下的原料:
聚醇1:基于糖的共引发的聚醚醇,官能度=4.4,羟基数目=500mgKOH/g,粘度=8000mPas
聚醇2:基于丙二醇的聚醚醇,官能度=2,羟基数目=100mgKOH/g,粘度=150mPas
聚醇3:基于邻苯二甲酸酐/二甘醇的聚酯醇,
官能度=2,羟基数目=300mgKOH/g,粘度=1000mPas
异氰酸酯:聚二苯基甲烷二异氰酸酯(PMDI),粘度=200mPas,
(来自BASFAG的LupranatM20S)
(所有情况的粘度数据均指的是25℃下的粘度)
稳定剂:含有硅氧烷的泡沫稳定剂
催化剂:二甲基环己胺,为溶于聚醇2的10重量%浓度的溶液
发泡剂:水
增塑剂:二羧酸二烷基酯
表1中显示本发明的硬质聚氨酯泡沫塑料有高剪切强度、高抗压强度和高杨氏模量。额外使用增塑剂能使每种泡沫性能得到进一步改善。
Claims (16)
1.一种硬质聚氨酯泡沫塑料,其可通过混合
a)异氰酸酯,
b)含有对异氰酸酯具有反应活性的基团的化合物,
c)含水的发泡剂,
d)催化剂,以及任选地
e)其它添加剂
形成反应混合物,将该反应混合物施用于增强材料并将该反应混合物固化而制得,
其中异氰酸酯(a)在25℃时的粘度不超过500mPas,并且
含有对异氰酸酯具有反应活性的基团的化合物(b)包括官能度不小于4且25℃时的粘度不高于10000mPas的聚醚醇(b1)、官能度不大于3.5且25℃时的粘度不高于600mPas的聚醚醇(b2)、25℃时的粘度不超过2000mPas的聚酯醇(b3)、含有至少30%仲羟基且分子量为60至300的增链剂(b4)和任选地交联剂(b5),成分(b1)的比例为从25至70重量%,成分(b2)的比例为从10至40重量%,成分(b3)的比例为从15至50重量%,成分(b4)的比例为从1至30重量%,成分(b5)的比例为从0至10重量%,各自基于成分(b)的总重量。
2.如权利要求1所述的硬质聚氨酯泡沫塑料,其中增链剂(b4)包含2,3-丁二醇、单丙二醇、二丙二醇和/或三丙二醇。
3.如权利要求1或2所述的硬质聚氨酯泡沫塑料,其中增链剂(b4)包含二丙二醇和另一种增链剂。
4.如权利要求3所述的硬质聚氨酯泡沫塑料,其中另一种增链剂为2,3-丁二醇或二乙二醇。
5.如权利要求1或2所述的硬质聚氨酯泡沫塑料,其中聚醚醇(b1)的比例为从30至60重量%,增链剂(b4)的比例为从2至30重量%,各自均基于聚醇混合物b)的总重量。
6.如权利要求1或2所述的硬质聚氨酯泡沫塑料,其中含有对异氰酸酯具有反应活性的基团的化合物(b)中聚醚醇(b1)、(b2)、(b3)、(b4)和任选地(b5)的比例是100重量%,基于含有对异氰酸酯具有反应活性的基团的化合物(b)的总重量。
7.如权利要求1或2所述的硬质聚氨酯泡沫塑料,其中不含增强材料的聚氨酯泡沫塑料的平均密度在50–200g/l范围。
8.如权利要求1或2所述的硬质聚氨酯泡沫塑料,其中不含增强材料的聚氨酯泡沫塑料的平均密度在80–120g/l范围。
9.如权利要求1或2所述的硬质聚氨酯泡沫塑料,其中水是唯一的发泡剂。
10.如权利要求1或2所述的硬质聚氨酯泡沫塑料,其中使用含有叔胺的催化剂混合物作为催化剂d)。
11.如权利要求1或2所述的硬质聚氨酯泡沫塑料,其中增强材料是玻璃纤维毡片,且该增强材料的使用量是从5至15重量%,基于含有增强材料的硬质聚氨酯泡沫塑料的总重量。
12.如权利要求1或2所述的硬质聚氨酯泡沫塑料,其中其它添加剂e)包括增塑剂。
13.一种制备硬质聚氨酯泡沫塑料的方法,包括:混合
a)异氰酸酯与
b)含有对异氰酸酯具有反应活性的基团的化合物、
c)含水的发泡剂、
d)含有叔胺的催化剂混合物,以及任选地
e)其它添加剂
形成反应混合物,将该反应混合物施用于增强材料并使该反应混合物固化以形成聚氨酯泡沫塑料;其中
异氰酸酯(a)在25℃时的粘度不超过500mPas,并且
含有对异氰酸酯具有反应活性的基团的化合物(b)包括官能度不小于4且25℃时的粘度不高于10000mPas的聚醚醇(b1)、官能度不大于3.5且25℃时的粘度不高于600mPas的聚醚醇(b2)、25℃时的粘度不高于2000mPas的聚酯醇(b3)、含有至少30%仲羟基且分子量为60至300的增链剂(b4)和任选地交联剂(b5),成分(b1)的比例为从25至70重量%,成分(b2)的比例为从10至40重量%,成分(b3)的比例为从15至50重量%,成分(b4)的比例为从1至30重量%,成分(b5)的比例为从0至10重量%,各自基于成分(b)的总重量。
14.一种用于液化天然气罐的隔热材料,其含有如权利要求1至11中任一项所述的硬质聚氨酯泡沫塑料。
15.如权利要求1至11中任一项所述的硬质聚氨酯泡沫塑料用于液化天然气罐的隔热的用途。
16.如权利要求15所述的用途,其中所述硬质聚氨酯泡沫塑料用于船运中液化天然气罐的隔热。
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Also Published As
Publication number | Publication date |
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US20110251297A1 (en) | 2011-10-13 |
JP5677974B2 (ja) | 2015-02-25 |
KR20110112326A (ko) | 2011-10-12 |
US8940803B2 (en) | 2015-01-27 |
EP2376554B1 (de) | 2015-03-04 |
EP2376554A1 (de) | 2011-10-19 |
CN102307922A (zh) | 2012-01-04 |
WO2010066635A1 (de) | 2010-06-17 |
CA2745920A1 (en) | 2010-06-17 |
JP2012511600A (ja) | 2012-05-24 |
KR101683316B1 (ko) | 2016-12-06 |
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