CN110382580A - 制备复合元件的聚氨酯制剂 - Google Patents
制备复合元件的聚氨酯制剂 Download PDFInfo
- Publication number
- CN110382580A CN110382580A CN201880016286.9A CN201880016286A CN110382580A CN 110382580 A CN110382580 A CN 110382580A CN 201880016286 A CN201880016286 A CN 201880016286A CN 110382580 A CN110382580 A CN 110382580A
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- Prior art keywords
- polyurethane
- acid
- catalyst
- monomer
- weight
- Prior art date
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Abstract
本发明涉及一种制备聚氨酯增强的复合材料的方法,包括混合(A)包含二异氰酸酯或多异氰酸酯(a)的多异氰酸酯组分和(B)包含具有至少两个与异氰酸酯具有反应性的基团的化合物(b)、催化剂(c)和任选的其他添加剂的多元醇组分,以形成反应混合物,将该反应混合物与增强材料在低于100℃的温度下接触并在高于100℃下固化反应混合物,以形成聚氨酯增强的复合材料,其中催化剂(c)包含微胶囊化的聚氨酯催化剂,其包含含有聚氨酯催化剂的胶囊芯和丙烯酸共聚物胶囊壳,其中微胶囊的平均粒径D(0,5)为1至50μm。本发明还涉及可通过本发明的方法获得的聚氨酯增强的复合材料。
Description
本发明涉及一种制备聚氨酯增强的复合材料的方法,包括混合(A)包含二异氰酸酯或多异氰酸酯(a)的多异氰酸酯组分和(B)包含具有至少两个对异氰酸酯呈反应性的基团的化合物(b)、催化剂(c)和任选的其他添加剂的多元醇组分,以形成反应混合物,将该反应混合物与增强材料在低于100℃的温度下接触并在高于100℃的温度下固化反应混合物,以形成聚氨酯增强的复合材料,其中催化剂(c)包含微胶囊化的聚氨酯催化剂,其包含含有聚氨酯催化剂的胶囊芯和丙烯酸共聚物胶囊壳,其中微胶囊的平均粒径D(0,5)为1至50μm。本发明还涉及可通过本发明的方法获得的聚氨酯增强的复合材料。
聚氨酯纤维增强的复合材料是众所周知的,并且包括通过真空灌注、长丝缠绕和拉挤成型生产的复合材料。在这些应用中,纤维材料用聚氨酯反应混合物润湿,例如在浸渍熔池或浸渍箱中。然后使浸渍的纤维材料成为其最终的形状,并固化反应混合物,例如在烘箱中固化。
该方法对聚氨酯基树脂非常苛刻,因为一旦纤维材料处于其最终形状,其需要快速固化,而另一方面需要长的开放时间以防止浸渍熔池的堵塞。这对于拉挤成型方法尤其如此。在该连续工艺中,制得具有恒定横截面的纤维增强的型材。拉挤成型设备通常由浸渍装置和加热模具以及引出系统组成,引出系统负责该过程的连续性。纤维的浸渍发生在开放熔池或密闭的注射箱中。此处,增强材料,例如玻璃纤维粗纱或玻璃纤维垫用树脂润湿。然后复合材料在加热模具中成型并硬化。引出系统将成品型材从模具中取出,最后将其切割成期望的长度。为了将拉挤成型方法的效率最大化,期望使用高的加工效率,同时拉挤成型具有非常好的机械性能和高的表面质量。
Bayer,Huntsman,Milgard Manufacturing Incorporated,Resin Systems Inc.等已经描述了两组分聚氨酯体系在拉挤成型方法中的用途。所用的材料主要是官能度为3.0的聚醚多元醇,它们在胺以及相应的金属络合物作为催化剂以及各种添加剂的存在下与异氰酸酯(通常是聚合的MDI)反应。这使得找到在润湿过程中保证低粘度和长的开放时间,并且另一方面快速和完全固化的催化剂体系变得更加苛刻。
在WO 2005/049301中,Huntsman通过使用两种金属催化剂来解决这个问题。Bayer使用基于DMC多元醇的体系(US 2008/0090921)或基于接枝多元醇的体系(US 2008/0087373),或使用不混溶的PU体系(US2008/0090996)。此外,Bayer和Huntsman均提及了使用酸用于部分中和,即阻断胺催化的原理。在WO 2005038118中提及的具体实例为甲酸、乙酸、2-乙基己酸和油酸。已发现催化剂的酸阻塞导致额外的缺陷如高拉脱力和成品型材粗糙表面的形成。
已经尝试过包封加聚催化剂,从而延迟催化剂的释放,仅在释放催化剂时进行快速的直接固化。通过胶囊在尺寸、类型和壁厚等方面的性质,可以定义和优选释放前的时间——即开放时间。
US 6224793公开了包封在可结晶或热塑性聚合物中的活性剂,其中包封的活性剂的粒径为3,000微米或更低,其中活性剂在环境条件下不能显著地从颗粒中提取。可结晶的聚合物的缺点是制备方法非常复杂——通过在125℃下融化聚合物并在15 000rpm下旋转熔融的聚合物以形成颗粒。
US 200501563862公开了控释体系,其包含多种有效包封的活性成分和感觉标记物。释放是在潮湿或在长时间内触发的。水分释放不适用于聚氨酯体系中的长丝缠绕和拉挤成型。
Adv.Mater.2016,DOI:10.1002/adma.201600830记载了热潜的催化剂纳米胶囊的生产。胶囊芯由异辛烷和新癸酸二甲基锡组成,聚(甲基丙烯酸甲酯-共-甲基丙烯酸丁酯-共-甲基丙烯酸)的胶囊壳通过二甲基丙烯酸丁二醇酯交联。胶囊通过微乳液技术制备。描述释放催化剂的唯一刺激是由膨胀剂触发的热开口。此处的缺点是低储存稳定性。在胶囊仅储存约两周后,反应特征明显改变。
通常,聚氨酯反应混合物通过两组分方法获得,其中包含对异氰酸酯具有反应性的化合物以及添加剂如催化剂和加工试剂的多元醇组分与包含异氰酸酯的异氰酸酯组分反应。这些组分必须显示出一定的储存稳定性,并且在储存期间不能分层或改变反应参数。
本发明的目的是提供制备聚氨酯纤维增强的复合材料的方法,该复合材料允许在浸渍过程和快速固化过程中聚氨酯反应混合物长的开放时间和低粘度。此外,期望预定义的多元醇组分和异氰酸酯组分显示一定的优选几个月的储存稳定性而不会分层或改变反应特征。
出于预料地,已发现本发明的目的通过制备聚氨酯增强的复合材料的方法来实现,所述方法包括混合(A)包含二异氰酸酯或多异氰酸酯(a)的多异氰酸酯组分和(B)包含具有至少两个对异氰酸酯具有反应性的基团的化合物(b)、催化剂(c)和任选的其他添加剂的多元醇组分,以形成反应混合物,将该反应混合物与增强材料在低于100℃的温度下接触并在高于100℃的温度下固化反应混合物,以形成聚氨酯增强的复合材料,其中催化剂(c)包含微胶囊化的聚氨酯催化剂,其包含含有聚氨酯催化剂的胶囊芯和丙烯酸共聚物胶囊壳,且其中微胶囊的平均粒径D(0,5)为1至50μm。本发明还涉及可通过本发明的方法获得的聚氨酯增强的复合材料。
在本发明的方法中包括在低于100℃的温度下,如在室温下润湿增强材料如蜂窝材料或纤维,以及在高于100℃的高温下固化增强的部件的步骤。这些方法包括众所周知的方法如真空浇铸法、长丝缠绕法和拉挤成型法。在本发明的一个优选实施方案中,制备聚氨酯纤维增强的复合材料的方法为包括在浸渍熔池中浸渍纤维的步骤的方法,如长丝缠绕法或更优选拉挤成型法。这些方法是本领域众所周知的。
长丝缠绕法通常包括在旋转心轴的张力下缠绕长丝。心轴围绕主轴旋转,同时输送眼(delivery eye)沿着旋转心轴的轴线水平移动,以期望的角度铺设纤维。长丝,通常是碳纤维的玻璃纤维,任选地以粗纱或纤维垫的形式,在它们被缠绕到心轴上之前用树脂浸渍在树脂熔池中。一旦心轴完全覆盖到所需的厚度,树脂就会固化。
拉挤成型法通常在拉挤成型设备中进行,该拉挤成型设备由浸渍装置和加热模具以及引出系统组成,该引出系统负责该方法的连续性。纤维的浸渍在开放熔池或封闭的注射箱中进行。此处,增强材料,例如玻璃纤维或碳纤维粗纱或垫用树脂润湿。然后将复合材料在加热的模具中成型并硬化。一个引出系统将成品型材从模具中拉出,最后将其切割成期望的长度。
所用的二异氰酸酯或多异氰酸酯(a)可以为用于制备聚氨酯已知的脂族、脂环族或芳族异氰酸酯。实例为二苯基甲烷2,2'-、2,4-和4,4'-二异氰酸酯,单体二苯基甲烷二异氰酸酯的混合物和具有更多环的二苯基甲烷二异氰酸酯同系物的混合物(聚合MDI),异佛尔酮二异氰酸酯(IPDI)或其低聚物,甲苯二异氰酸酯(TDI)例如甲苯二异氰酸酯异构体如甲苯2,4-或2,6-二异氰酸酯,或这些物质的混合物,四亚甲基二异氰酸酯或其低聚物,六亚甲基二异氰酸酯(HDI)或其低聚物,亚萘基二异氰酸酯(NDI)或它们的混合物。
所用的二异氰酸酯或多异氰酸酯(a)优选包括基于二苯基甲烷二异氰酸酯的异氰酸酯,特别是包括聚合MDI。二异氰酸酯或多异氰酸酯(a)的官能度优选为2.0至2.9,特别优选2.1至2.8。本文二异氰酸酯或多异氰酸酯(a)在25℃下的粘度根据DIN 53019-1至3优选为5至600mPas且特别优选10至300mPas。
二异氰酸酯或多异氰酸酯(a)还可以以多异氰酸酯预聚物的形式使用。这些多异氰酸酯预聚物可通过将过量的上述多异氰酸酯(组分(a-1))与具有至少两个对异氰酸酯具有反应性的基团的化合物(组分(a-2))例如在30至100℃,优选在约80℃的温度下反应获得,以得到预聚物。本发明的多异氰酸酯预聚物的NCO含量优选为20至33重量%的NCO,特别优选25至32重量%的NCO。
具有至少两个对异氰酸酯具有反应性的基团的化合物(a-2)是本领域技术人员已知的,并例如记载于"Polyurethane Handbook”Hanser-Publishers,第2版,1993,第3.1章中。因此具有至少两个对异氰酸酯具有反应性的基团的化合物的实例为聚醚醇或聚酯醇,如在下文(b)下描述的那些。具有至少两个对异氰酸酯具有反应性的基团的化合物(a-2)优选为包含仲OH基的聚醚醇或聚酯醇,实例为聚环氧丙烷。这些聚醚醇或聚酯醇的官能度优选为2至4,特别优选2至3。
特别优选不使用多异氰酸酯预聚物。
所用的具有至少两个对异氰酸酯具有反应性的基团的化合物(b)——对于本发明的目的还称为“多元醇”——可包括具有至少两个对异氰酸酯具有反应性的基团的任意化合物,实例为OH、SH、NH、NH2、-COOH和CH-酸性基团,其中仲OH基的比例,基于对异氰酸酯具有反应性的基团的数目计,为至少50%,优选至少60%,特别优选至少70%,且特别是至少80%。
通常使用具有2-8个对异氰酸酯具有反应性的氢原子的聚醚醇和/或聚酯醇,并使用低分子量多元醇,例如甘油、二丙二醇和/或三丙二醇。这些化合物的OH值通常为30至2000mg KOH/g,优选40至1000mg KOH/g。本文所用的具有至少两个对异氰酸酯具有反应性的基团的所有化合物(b)的平均OH值为100至1000mg KOH/g,优选300至900mg KOH/g。
聚醚醇通过已知的方法获得,例如在催化剂的存在下加入至少一种起始剂分子通过环氧烷烃的阴离子聚合制备,所述起始剂分子包含2至8个,优选2至6个,且特别是2至4个反应性氢原子。所用的催化剂可包括碱金属氢氧化物例如氢氧化钠或氢氧化钾,或碱金属醇化物例如甲醇钠、乙醇钠、乙醇钾或异丙醇钾,或在阳离子聚合的情况下,路易斯酸例如五氯化锑、三氟化硼醚合物或漂白土。可以使用的其他催化剂为已知为DMC催化剂的双金属氰化物化合物。
所用的环氧烷烃优选包括一种或多种在亚烷基部分具有2至4个碳原子的化合物,例如四氢呋喃、环氧乙烷、丙烯1,2-氧化物、丁烯1,2-氧化物或丁烯2,3-氧化物,在每种情况下以单独的形式或混合物的形式,优选丙烯1,2-氧化物和/或环氧乙烷,特别是丙烯1,2-氧化物。
可使用的起始剂分子的实例为乙二醇、二乙二醇、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,以及其他二元醇或多元醇,或二元胺或多元胺。
所用的聚酯醇主要是通过缩合具有2-12个碳原子的多元醇与具有2至12个碳原子的多元羧酸制备的,所述多元醇例如乙二醇、二乙二醇、丁二醇、三羟甲基丙烷、甘油或季戊四醇,所述多元羧酸例如琥珀酸、戊二酸、己二酸、辛二酸、壬二酸、癸二酸、十二烷二酸、马来酸、富马酸、邻苯二甲酸、间苯二甲酸、对苯二甲酸,以及萘二甲酸的异构体或它们的酸酐。
也可以同时用于制备聚酯的其他起始材料是疏水性物质。疏水性物质是不溶于水的物质,其包含非极性有机部分,并且还具有至少一个选自羟基、羧酸、羧酸酯或其混合物的反应性基团。疏水材料的当量重量优选为130至1000g/mol。可以使用的材料的实例是脂肪酸,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、葵花籽油、大豆油、椰子油、橄榄油或妥尔油。如果聚酯包含疏水性物质,则基于聚酯醇的总单体含量计,疏水性物质的比例优选为1-30mol%,特别优选为4-15mol%。
所用聚酯醇的官能度优选为1.5至5,特别优选为1.8至3.5。
在一个特别优选的实施方案中,具有对异氰酸酯具有反应性的基团的化合物(b)包含聚醚醇,特别是仅含有聚醚醇。聚醚醇的实际平均官能度优选为2至4,特别优选2.5至3.5,特别是2.8至3.2,并且它们的OH值优选为300至900mg KOH/g,以及它们的仲OH基团含量优选至少50%,优选至少60%,特别优选至少70%,特别是至少80%。本文使用的聚醚醇优选包含基于甘油作为起始物并且基于丙烯-1,2-氧化物的聚醚醇。
催化剂(c)包括微胶囊化的聚氨酯催化剂,其包含含有聚氨酯催化剂的胶囊芯和丙烯酸共聚物胶囊壳,并且其中微胶囊的平均粒度D(0,5)为1至50μm。根据本发明使用的微胶囊的平均粒度D(0,5)(体积加权平均值,通过光散射测定)优选为1至50μm,更优选1至20μm,更特别是2至10μm。此处的D(0,5)定义为达到50%的累积颗粒体积的颗粒直径。具有这种直径的胶囊具有足够的机械稳定性,能够在不损坏的情况下进行处理,并且在不损坏待固化的组合物的情况下加入。选择的尺寸使得可以容忍单个胶囊的意外破损,因为单个胶囊的非预期破损仅释放少量聚氨酯催化剂,不会导致组合物的过早硬化。另一方面,通过易于处理的胶囊体积引入足以完全固化的催化剂量。
在某些实施方案中,微胶囊化的聚氨酯催化剂采用干粉、颗粒或附聚物的形式。
胶囊芯与胶囊壳的重量比通常为50:50至95:5,优选为60:40至94:6,特别优选为70:30至93:7。
聚氨酯催化剂可包含任何常规用于生产聚氨酯的催化剂。这些催化剂例如在“Polyurethane Handbook”Carl Hanser Verlag,1993年第2版,第3.4.1章中描述。此处可以使用的那些催化剂的实例是有机金属化合物,例如锡、锌、钛、锆、铁、汞或铋的络合物,优选有机锡化合物,例如有机羧酸的亚锡盐,例如乙酸亚锡、辛酸亚锡、乙基己酸亚锡和月桂酸亚锡;以及羧酸的二烷基锡(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;以及新癸酸苯汞;羧酸铋,如新癸酸铋(III)、2-乙基己酸铋和辛酸铋,或其混合物。其他可能的催化剂是碱性胺催化剂。这些催化剂的实例是脒,例如2,3-二甲基-3,4,5,6-四氢嘧啶;叔胺,例如三乙胺,三亚乙基二胺,三丁胺,二甲基苄胺,N-甲基-、N-乙基-、N-环己基吗啉,N,N,N',N'-四甲基乙二胺,N,N,N',N'-四甲基丁二胺,N,N,N',N'-四甲基己二胺,五甲基二亚乙基三胺,四甲基二氨基乙醚,双(二甲基氨基丙基)脲,二甲基哌嗪,1,2-二甲基咪唑,1-氮杂双环[3.3.0]辛烷,优选1,4-二氮杂双环[2.2.2]辛烷,1,8-二氮杂双环[5.4.0]-十一碳-7-烯和烷醇胺化合物,如三乙醇胺,三异丙醇胺,N-甲基-和N-乙基二乙醇胺和二甲基乙醇胺。催化剂可以单独使用或以混合物的形式使用。任选使用金属催化剂和碱性胺催化剂的混合物作为催化剂(c)。在一个优选的实施方案中,聚氨酯催化剂是基于锡或基于铋的催化剂,例如催化剂选自羧酸的二烷基锡(IV)盐,例如二乙酸二丁基锡、二月桂酸二丁基锡、马来酸二丁基锌和二乙酸二辛基锡、二乙酸锌(II)、二辛酸锌(II)、乙酰丙酮锆和2,2,6,6-四甲基-3,5-庚二酸锆和新癸酸铋(III)、2-乙基己酸铋和辛酸铋或其混合物。特别优选的聚氨酯催化剂选自二月桂酸二丁基锡、二月桂酸二辛基锡、新癸酸铋、二辛酸铋和乙基己酸铋或其两种或更多种的混合物。
胶囊芯优选包含疏水芯材料以及聚氨酯催化剂。伴随使用疏水性芯材料能够制备尺寸分布均匀的明确定义的胶囊,并且一旦胶囊壳被打开就促进在应用介质中释放的聚合催化剂的分布。
聚合催化剂优选占10至100重量%,例如20至90重量%,更特别是30至70重量%,基于聚合催化剂和疏水性芯材料的总重量计。
疏水性芯材料的实例为脂族烃、芳族烃、卤代烃、饱和或不饱和的C6-C30脂肪酸、脂肪醇、羰基合成醇(oxo-process alcohol)、脂肪醇的醚、C6-C30脂肪胺、脂肪酸酯、甘油三酯、脂族或芳族多羧酸的酯、天然蜡和合成蜡以及三烷基磷酸酯。疏水性芯材料还可以以两种或更多种物质的混合物使用。
合适的物质的实例包括以下:
-脂族烃,例如饱和或不饱和的C10-C40烃,其是支链的或优选直链的,例如正十四烷、正十五烷、正十六烷、正十七烷、正十八烷、正十九烷、正二十烷、正二十一烷、正二十二烷、正二十三烷、正二十四烷、正二十五烷、正二十六烷、正二十七烷、正二十八烷以及环状烃,例如环己烷、环辛烷、环癸烷;
-芳族烃,例如苯、萘、联苯、邻-或间-三联苯、C1-C40烷基取代的芳族烃,例如十二烷基苯、十四烷基苯、十六烷基苯、己基萘或癸基萘;
-卤代烃,例如氯化石蜡、溴代十八烷、溴代十五烷、溴代十九烷、溴代二十烷、溴代二十二烷;
-饱和或不饱和的C6-C30脂肪酸,例如月桂酸、硬脂酸、油酸或二十二烷酸;
-脂肪醇,例如月桂醇、硬脂醇、油醇、肉豆蔻醇和鲸蜡醇,混合物如椰子脂肪醇,以及羰基合成醇,其是通过α-烯烃的加氢甲酰化和进一步反应得到的;
-C6-C30脂肪胺,如癸胺、十二烷胺、十四烷胺或十六烷胺;
-脂肪酸酯,如脂肪酸的C1-C10烷基酯,如棕榈酸丙酯、硬脂酸甲酯或棕榈酸甲酯,还优选它们的低共熔混合物,或肉桂酸甲酯;
-直链或支链的C3-C21羧酸的甘油三酯,例如橄榄油、大豆油、玉米油、棉籽油、向日葵油、花生油、棕榈油、椰子油和小麦胚芽油;
-脂族或芳族多羧酸的酯,尤其是己二酸、癸二酸、琥珀酸、柠檬酸、乙酰基柠檬酸、环己烷-1,2-二羧酸或邻苯二甲酸的酯,如己二酸二-2-乙基己酯、己二酸二正己酯、己二酸二正辛酯、己二酸二异辛酯、己二酸二正癸酯、己二酸二异癸酯、癸二酸乙基己酯、癸二酸二异癸酯、邻苯二甲酸二正丁酯,邻苯二甲酸二正辛酯,邻苯二甲酸二正己酯,邻苯二甲酸二正癸酯,邻苯二甲酸二环己酯,邻苯二甲酸二异癸酯,邻苯二甲酸丁基环己酯,邻苯二甲酸二异辛酯,邻苯二甲酸异辛异癸酯;
-天然蜡和合成蜡,如褐煤酸蜡、褐煤酯蜡、棕榈蜡、聚乙烯蜡、氧化蜡、聚乙烯醚蜡、乙烯-乙酸乙烯酯蜡或硬菲舍尔-托法蜡(hard Fischer-Tropsch process waxes);
-三烷基磷酸酯,例如磷酸三甲酯。
其中,脂族或芳族多羧酸的酯,尤其是己二酸酯,1,2-环己烷二甲酸酯,邻苯二甲酸酯,甘油三酯和三烷基磷酸酯通常是优选的,因为它们容易获得并且与通常固化的组合物相容。特别优选的疏水性芯材料是1,2-环己烷二甲酸二异壬酯。
通常,丙烯酸共聚物由以下单元构成:
(i)50至90重量%,优选55至80重量%的至少一种选自丙烯酸的C1-C24烷基酯、甲基丙烯酸的C1-C24烷基酯和乙烯基芳族化合物的单体,
(ii)5至20重量%,优选10至15重量%的至少一种具有至少两个烯键式不饱和度的单体,和
(iii)0至30重量%,优选0至20重量%的一种或多种其他单体,各自基于单体的总重量计。
合适的单体(i)为丙烯酸和/或甲基丙烯酸的C1-C24烷基酯。合适的单体(b)是丙烯酸异丙基酯、丙烯酸异丁基酯、丙烯酸仲丁基酯和丙烯酸叔丁基酯和相应的甲基丙烯酸酯,更优选丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丙酯和丙烯酸正丁酯以及相应的甲基丙烯酸酯。通常,甲基丙烯酸酯是优选的。其他合适的单体(i)为乙烯基芳族化合物,例如苯乙烯或α-甲基苯乙烯。
在某些实施方案中,单体(i)包含至少一种在聚合反应后具有70℃或更高的玻璃化转变温度Tg的单体和至少一种在聚合反应后具有50℃或更低的玻璃化转变温度Tg的单体的组合。在聚合反应后玻璃化转变温度Tg为70℃或更高的优选单体是甲基丙烯酸甲酯;在聚合反应后玻璃化转变温度Tg为50℃或更低的优选单体是丙烯酸正丁酯或甲基丙烯酸正丁酯。
单体(ii)具有至少两个烯键式不饱和度。它们在聚合过程中引起胶囊壳的交联,并赋予胶囊壳机械稳定性。合适的单体(ii)是具有两个、三个、四个或更多个非共轭的烯键式不饱和度的烯键式不饱和单体。优选使用具有乙烯基、烯丙基、丙烯酸和/或甲基丙烯酸基团的单体。优选的单体是那些不溶于水或微溶于水但在亲脂性物质中具有良好至有限溶解度的单体。微溶是指在20℃下溶解度小于60g/L。
具有两个烯键式不饱和度的合适单体是二乙烯基苯和二乙烯基环己烷,二醇与丙烯酸或甲基丙烯酸的二酯,以及这些二醇的二烯丙基醚和二乙烯基醚。实例包括二丙烯酸乙二醇酯、二甲基丙烯酸乙二醇酯、二甲基丙烯酸1,3-丁二醇酯、甲基烯丙基甲基丙烯酰胺、丙烯酸烯丙酯和甲基丙烯酸烯丙酯。特别优选的是二丙烯酸丙二醇酯、二丙烯酸丁二醇酯、二丙烯酸戊二醇酯和二丙烯酸己二醇酯以及相应的甲基丙烯酸酯。
具有三个、四个或更多个非共轭烯键式不饱和度的优选单体是多种醇与丙烯酸和/或甲基丙烯酸的酯,以及这些多种醇的烯丙基醚和乙烯基醚,三乙烯基苯和三乙烯基环己烷。可提及的多种醇特别包括三羟甲基和季戊四醇。特别优选的是三羟甲基丙烷三丙烯酸酯和三羟甲基丙烷三甲基丙烯酸酯、季戊四醇三烯丙基醚、季戊四醇四烯丙基醚、季戊四醇三丙烯酸酯和季戊四醇四丙烯酸酯,以及它们的工业混合物。因此,季戊四醇四丙烯酸酯通常在工业混合物中混合有季戊四醇三丙烯酸酯和少量低聚产物。
特别优选的单体(ii)是1,4-丁二醇二丙烯酸酯、季戊四醇三丙烯酸酯、季戊四醇四丙烯酸酯和二甲基丙烯酸三乙二醇酯。
考虑的任选单体(iii)是与单体(a)至(c)不同的其他单体,例如乙酸乙烯酯、丙酸乙烯酯、乙烯基吡啶、丙烯酸、甲基丙烯酸、马来酸、衣康酸、乙烯基膦酸、马来酸酐、丙烯酸2-羟基乙酯和甲基丙烯酸酯、丙烯酰胺基-2-甲基丙磺酸、甲基丙烯腈、丙烯腈、甲基丙烯酰胺、N-乙烯基吡咯烷酮、N-羟甲基丙烯酰胺、N-羟甲基甲基丙烯酰胺、甲基丙烯酸二甲基氨基乙酯和甲基丙烯酸二乙基氨基乙酯。
丙烯酸共聚物可以多种方式获得,但优选通过在水包油乳液或油包水乳液中的自由基悬浮聚合获得。本领域技术人员将根据待包封的催化剂的亲水性或亲油性在水包油或油包水方案之间进行选择。
例如,WO 2013/092158和WO 2014/198531中描述了一种在油包水乳液中进行自由基悬浮聚合的方法,本文全部引用。
微胶囊优选通过在稳定的水包油乳液的油相中聚合构成胶囊壳的单体混合物而获得,该油相由包含聚合催化剂的疏水性材料组成。该制备方法本身是已知的,并且例如在DE 4321205或WO 2014/127951中描述。
微胶囊的芯由可在水中乳化的疏水材料形成。疏水性材料同时用作通过聚合制备胶囊壳中所用的单体混合物的溶剂或分散剂。然后聚合在稳定的水包油乳液的油相中进行。该乳液通过例如首先将单体和聚合引发剂以及任选的链转移剂溶解在疏水材料中,并将所得溶液乳化在含有乳化剂和/或保护胶体的水性介质中而获得。另一种可能性是首先在水相中乳化疏水相或其组分,然后向乳液中加入单体或聚合引发剂以及仍然使用的助剂,任选地如保护胶体或链转移剂。在该方法的另一个变型中,疏水性材料和单体也可以在水中乳化,然后仅加入聚合引发剂。由于疏水性材料要在乳液中尽可能充分地微囊化,因此所用的疏水性材料优选仅是在水中具有有限溶解度的那些。在25℃下溶解度应优选不超过5重量%。为了将疏水性材料完全包封在水包油乳液的油相中,根据它们在疏水性材料中的溶解度来选择单体是有用的。尽管单体基本上可溶于油中,但它们在单独的油滴聚合时产生低聚物和随后的聚合物,所述聚合物既不溶于油相,也不溶于水包油乳液的水相中,并且迁移到油滴和水相之间的界面。在那里,在进一步聚合的过程中,它们形成壁材料,其最终包封疏水材料作为微胶囊的芯。
为了形成稳定的水包油乳液,通常也使用保护胶体和/或皮克林稳定剂。保护胶体和皮克林稳定剂都可以是离子的或中性的。保护胶体和皮克林稳定剂可以单独使用,也可以以两种或更多种具有相同或不同电荷的代表物的混合物使用。
保护胶体优选是水溶性聚合物,其将水的表面张力从最大73mN/m降低至45-70mN/m,从而确保形成封闭的胶囊壁。
阴离子保护胶体是海藻酸钠、聚甲基丙烯酸及其共聚物、丙烯酸磺基乙酯和甲基丙烯酸磺基乙酯的共聚物、丙烯酸磺基丙酯和甲基丙烯酸磺基丙酯的共聚物、N-(磺基乙基)马来酰亚胺的共聚物、2-丙烯酰胺基-2-烷基磺酸的共聚物、苯乙烯磺酸以及乙烯基磺酸的共聚物。优选的阴离子保护胶体是萘磺酸和萘磺酸-甲醛缩合物,特别是聚丙烯酸和苯酚磺酸-甲醛缩合物。
中性保护胶体是例如纤维素衍生物,例如羟乙基纤维素、甲基羟乙基纤维素、甲基纤维素和羧甲基纤维素、聚乙烯吡咯烷酮、乙烯基吡咯烷酮的共聚物、明胶、阿拉伯树胶、黄原胶、酪蛋白、聚乙二醇、聚乙烯醇和部分水解的聚乙酸乙烯酯以及甲基羟丙基纤维素。优选的中性保护胶体是聚乙烯醇和部分水解的聚乙酸乙烯酯以及甲基羟基-(C1-C4)-烷基纤维素。
皮克林稳定剂是无机固体颗粒。这种皮克林体系可以由单独的固体颗粒或另外的助剂组成,所述助剂增强颗粒在水中的分散性或增强亲脂相对颗粒的润湿性。其作用方式和使用记载于EP-A-1 029 018和EP-A-1321 182中,其内容通过引用明确地纳入本文中。
无机固体颗粒可以是金属盐,例如钙、镁、铁、锌、镍、钛、铝、硅、钡和锰的盐、氧化物和氢氧化物。它们包括氢氧化镁、碳酸镁、氧化镁、草酸钙、碳酸钙、碳酸钡、硫酸钡、二氧化钛、氧化铝、氢氧化铝和硫化锌。还可提及硅酸盐、膨润土、羟磷灰石和水滑石。特别优选的是SiO2-基硅石,焦磷酸镁和磷酸三钙。
合适的SiO2基皮克林稳定剂是细分散的二氧化硅。它们可以作为细小的固体颗粒分散在水中。但是,也可以使用所谓的在水中的二氧化硅胶体分散体。这种胶体分散体是碱性的二氧化硅水性混合物。在碱性pH范围内,颗粒溶胀并在水中稳定。对于这些用作皮克林稳定剂的分散体,有利的是将水包油乳液的pH用酸调节至pH为2至7。优选的二氧化硅胶体分散体在pH为9.3时,比表面积为70-90m2/g。
优选的SiO2基皮克林稳定剂是细分散的二氧化硅,其平均粒度在40至150nm的范围内,pH水平为8至11。实例包括50/50(H.C.Starck)、3550(CWKBad Kostritz)和50/80(Akzo Nobel Chemicals)。
聚合通常在形成自由基的聚合引发剂存在下进行。为此目的,可以使用所有常规过氧化合物和偶氮化合物,其通常使用量为例如0.1至5重量%,基于待聚合单体的重量计。优选的聚合引发剂是可溶于油相或单体的那些。这种引发剂的实例是过氧新癸酸叔丁酯、过氧新戊酸叔丁酯、过氧新戊酸叔戊酯,过氧化二月桂酰、过氧-2-乙基己酸叔戊酯等。
水包油乳液的聚合通常在20至100℃,优选40至90℃下进行。聚合通常在大气压下进行,但也可以在减压或增压下例如0.5至20巴内进行。一种有用的方法是使用高速分散器将水、保护胶体和疏水材料、聚合引发剂和单体的混合物乳化成所需的疏水材料的液滴尺寸,并在搅拌下将稳定的乳液加热至聚合引发剂的分解温度。在这种情况下的聚合速率可以通过以已知方式选择温度和聚合引发剂的量来控制。当达到聚合温度时,有用的是继续聚合一段时间,例如2至6小时,以完成单体的转化。
在特别优选的操作中,聚合反应混合物的温度在聚合过程中连续或周期性地升高。这是通过温度上升的程序完成的。为此目的,总聚合时间可以细分为2个或更多个时期。第一聚合期通过聚合引发剂的缓慢分解为标记。在第二聚合期和任何进一步的聚合期间,升高反应混合物的温度以加速聚合引发剂的分解。温度可以以一步或两步或多步升高或以线性或非线性方式连续升高。聚合开始和结束之间的温差可高达50℃。通常,该差值为3至40℃,优选3至30℃。聚合结束后,将微胶囊分散体冷却至室温。
如果要将微胶囊分散体储存相对长的时间,可以加入增稠剂例如 AS1125、 AT 120、 AS 1130(可从BASF SE,德国获得)或黄原胶,为了稳定悬浮液和防止乳液分层。
通过上述方法获得的微胶囊分散体可被干燥,例如以常规方式喷雾干燥。通常获得粉末,其中剩余水含量小于5重量%,优选小于3重量%,基于粉末的总重量计。为了促进喷雾干燥的微胶囊的再分散,任选地,可以在喷雾干燥之前将额外量的乳化剂和/或保护胶体加入到分散体中。微胶囊分散体的喷雾干燥可以以常规方式进行。通常,该方法涉及干燥气体(通常为氮气或空气)的进入温度为100至200℃,优选120至160℃,以及干燥气体的出口温度为30至90℃,优选60至80℃。将水性微胶囊分散体喷雾在干燥气体流中可以例如通过单流体或多流体喷嘴或通过旋转盘进行。微胶囊分散体通常在2至200巴的范围内进料。使用具有涡流发生器的单流体喷嘴是有利的。通过选择涡流发生器,还可以影响液滴尺寸和喷射角度。例如,可以使用来自Delavan的单流体喷嘴,其具有包括影响喷射角度的涡流室以及影响产量的多孔板的典型的结构。
通常使用旋风分离器或过滤分离器沉积颗粒微胶囊组合物。喷雾的含水微胶囊分散体和干燥气流优选平行引导。优选将干燥气流与微胶囊分散体同向从上方吹入塔中。
根据一种方法变型,可以在干燥器的下游插入流化床,以除去任何残留的水分。其中喷雾干燥之后进行流化床干燥的方法是优选的,因为它们得到具有较小细粒级分的微胶囊组合物。
本文中催化剂(c)的比例优选为0.05至10重量%,特别优选0.1至5重量%,特别是0.1至2.5重量%,基于组分(b)至(d)的总重量计。本文中催化剂的使用方式优选使得在混合组分(a)-(d)后,本发明的聚氨酯反应混合物在23℃下的凝胶时间大于10分钟,更优选大于15分钟,特别优选大于20分钟且小于60分钟,特别是大于15分钟且小于60分钟。催化剂的选择优选使得本发明的聚氨酯反应混合物的完全硬化在更高的温度下,优选高于100℃、最优选高于150℃、特别是200℃-240℃下进行。例如,在220℃下,在组分(a)至(d)混合后60秒内,更优选0至45秒,特别是5至35秒,特别是5至30秒发生硬化。在一个优选的实施方案中,除了包封的催化剂之外,还可以加入另外的聚氨酯催化剂,只要本发明的聚氨酯反应混合物的凝胶时间在23℃下大于10分钟即可。这些另外的催化剂可以是封端的胺催化剂,如用羧酸封端的1,8-二氮杂双环[5.4.0]十一碳-7-烯。在更优选的实施方案中,催化剂(c)由微胶囊化的聚氨酯催化剂组成,并且不添加另外的聚氨酯催化剂。
为了确定本文中在23℃下的凝胶时间,在室温下将用于制备聚氨酯反应混合物的组分称重到烧杯中,并在高速混合器中以2000转/分钟彼此混合30秒。然后将100g整个体系称入单独的烧杯中,并借助木制刮刀测定凝胶时间。凝胶时间对应于混合过程开始和硬化之间的时间差,即凝块的初始形成。
为了在高于120℃的温度下测定完全硬化,在室温下将用于制备聚氨酯反应混合物的组分称重到烧杯中,并在高速混合器中以2000转/分钟彼此混合30秒。借助Pasteur移液管将10mL体系置于表面温度为120℃的板上的金属环内。将反应性混合物在环的内边界处开始硬化的时间(以s计)定义为开始时间,将反应性混合物不再粘附到木制刮刀上的时间定义为固化的结束时间。
所用的其他添加剂(d)可包括已知用于生产聚氨酯的任何添加剂。可提及的实例是表面活性剂物质、脱模剂、偶联剂、填料、染料、颜料、阻燃剂、水解稳定剂、降粘剂、除水剂、消泡剂,以及具有抑真菌和抑菌作用的物质。这种类型的物质是已知的,并且例如记载于“Polyurethane Handbook,第2版,Hanser Publishers,1993,第3.4.4和3.4.6至3.4.11节”中。
因此,可用于水吸附的添加剂的实例是硅铝酸盐,选自硅铝酸钠、硅铝酸钾、硅酸钙、硅铝酸铯、硅铝酸钡、硅铝酸镁、硅铝酸锶、铝磷酸钠、铝磷酸钾、铝磷酸钙及其混合物。特别优选在蓖麻油中使用硅铝酸钠、硅铝酸钾和硅铝酸钙的混合物作为载体物质。
水吸附添加剂的数均粒径优选不大于200μm,特别优选不大于150μm,特别是不大于100μm。本发明的水吸附添加剂的孔宽优选为2至5埃。
如果加入水吸附添加剂,则此处的量优选大于1重量份,特别优选0.5-5重量份,基于组分(b)-(d)的总重量计。
可以使用的偶联剂包括硅烷,例如异氰酸酯硅烷,环氧硅烷或氨基硅烷。这种类型的物质例如记载于E.P.Plueddemann,Silane Coupling Agents,第2版,Plenum Press,NewYork,1991和K.L.Mittal编辑,Silanes and Other Coupling Agents,VSP,Utrecht,1992中。
可以使用的内部脱模剂是用于生产聚氨酯的任何常规脱模剂,实例是长链羧酸,特别是脂肪酸,例如硬脂酸;长链羧酸的胺,例如硬脂酰胺;脂肪酸酯;长链羧酸的金属盐,例如硬脂酸锌或有机硅。特别合适的材料是专门为拉挤成型方法可获得的内部脱模剂,例如,来自Axel Plastics或Technick Products。来自Technick Products的内部脱模剂可能含有磷酸和脂肪酸。来自Axel Plastics的内部脱模剂可能含有脂肪酸。
可以使用的降粘剂的实例是γ-丁内酯、碳酸亚丙酯,以及反应性稀释剂,例如二丙二醇、二乙二醇和三丙二醇。
本发明的聚氨酯树脂优选包含小于2重量%,特别优选小于1重量%的在标准压力下沸点低于200℃的物质。在混合组分(a)-(d)后,聚氨酯树脂体系在25℃下根据DIN53019-1至3的立即具有的粘度优选小于1500mPas,特别优选小于1200mPas,特别是小于1000mPas。其中此处组分(a)-(d)混合的定量比例优选使得异氰酸酯指数为90-140,特别优选100-130,特别是115-125。出于本发明的目的,此处的异氰酸酯指数是异氰酸酯基团与对异氰酸酯具有反应性的基团的化学计量比乘以100。此处对异氰酸酯具有反应性的基团是反应混合物中包含的对异氰酸酯具有反应性但并不是异氰酸酯基本身的任何基团。
本发明还提供了一种生产聚氨酯增强复合材料的方法。在该方法中,将本发明的聚氨酯树脂体系的组分混合以得到聚氨酯反应混合物,并且所得的反应混合物用于在低于100℃、优选0至75℃、更优选10至50℃、特别是15至35℃的温度下润湿增强材料,例如纤维材料。优选在形成反应混合物之前,将组分(b)-(d)混合,得到一种多元醇组分(B),然后将其与包含异氰酸酯(A)的异氰酸酯组分(A)混合。优选的异氰酸酯组分(A)不包含任何催化剂(c),更优选仅由异氰酸酯(a)组成。
对于长丝缠绕法,然后将湿润的纤维材料在张力下缠绕在旋转的心轴上。一旦心轴完全覆盖到所需的厚度,树脂就会固化。对于拉挤成型法,将湿润的纤维材料在加热的模具中模塑,并且优选在通过加热的模具期间使反应混合物硬化。
对于本发明的目的而言,当相对于异氰酸酯基团,反应中的转化率小于90%时,组分(a)至(d)的混合物被称为反应混合物。
本发明的聚氨酯反应混合物的组分的混合在本文中可以以生产基于聚氨酯的反应混合物的常规方式进行,例如以高压或低压方法。
增强材料可以是聚氨酯领域中已知的任何增强材料。这包括蜂窝材料,如纸板蜂窝材料和纤维材料。根据本发明使用的纤维材料可包括任何类型的纤维材料,优选任何种类的连续长丝纤维。此处的连续长丝纤维是指长度至少为几米的纤维材料。这些材料例如是从辊上展开的。此处使用的纤维材料可包括单根纤维,已知为纤维粗纱、编织纤维、纤维垫、纤维平纹棉麻织物和织造纤维。特别是在纤维复合材料例如编织纤维、加捻纤维、平纹棉麻织物或织造纤维的情况下,在所述纤维结构内包含的单根纤维中也可以包含较短的单根纤维,但纤维复合材料本身必须采取连续长丝材料的形式。纤维材料优选包含或由玻璃纤维、玻璃垫、碳纤维、聚酯纤维、天然纤维、芳纶纤维、玄武岩纤维或尼龙纤维构成,特别优选使用碳纤维或玻璃纤维。
本文中纤维材料的润湿可以在敞口模具中或优选在封闭的模具中进行。湿润纤维材料期间的温度优选低于100℃,优选0至75℃,特别优选10至50℃,特别是15至35℃。本文中纤维材料的比例优选为10至90重量%,特别优选30至90重量%,特别是60至90重量%,基于成品拉挤成型件计。
对于本发明的拉挤成型法而言,在润湿过程之后,用反应混合物润湿的纤维材料优选通过模具拉出。该模具可以具有任何期望的横截面形状,垂直于湿润纤维材料的拉伸方向,但是该形状优选尽可能恒定,例如槽形或圆形,或L形或T形,或更复杂的形状。该模具的温度优选为100至250℃,最优选为150至230℃,因此聚氨酯反应混合物硬化得到成品聚氨酯。
优选地,拉挤成型件以大于一米/分钟的速度从模具中拉出。引出速度特别优选地大于1.5米/分钟,特别是大于2.0米/分钟。通常将所得的拉挤成型件切成所需的长度。在一个特别优选的实施方案中,拉挤成型件的横截面不同于扁平部分,如L形、V形或U形轮廓,或具有更高复杂性的轮廓。
本发明还提供了可通过本发明的方法获得的拉挤成型件。这种拉挤成型件具有优异的表面质量和润湿质量。对于0.5米/分钟的引出速度和1.5米/分钟的引出速度,拉挤成型件的机械性能相同。此外,多元醇组分储存稳定超过一个月,优选超过两个月。
使用以下实施例来说明本发明。
使用以下材料:
多元醇1甘油引发的OH值为400mg KOH/g的环氧丙烷
多元醇2甘油引发的OH值为42mg KOH/g的环氧丙烷/聚环氧乙烷
多元醇3甘油引发的OH值为805mg KOH/g的环氧丙烷
Kat 1Tinstab OTS 16硫醇辛基锡
Kat 2Polycat SA 1/10mit被苯酚封端的1,8-二氮杂-双环(5.4.0)-十一碳-7-烯(摩尔比1:1)
Kat 3DBTL(二月桂酸二丁基锡)
Kat 4包封的DBTL,含有40重量%的纯DBTL
IMR 1内部脱模剂,
IMR 2内部脱模剂
Iso 1Lupranat聚合MDI,平均官能度为2.7;NCO含量为31,5g/100g
Iso 2 2,4'-和4,4'-二苯基甲烷二异氰酸酯的混合物,NCO含量为33,5g/100g
Kat.4的制备:
水相:
171.9g DI水(DI=完全的去离子水)
36g的50重量%硅溶胶于水中(比表面积计算为80m2/g)
1.68g的5重量%的平均分子量为26 000g/mol的甲基羟基丙基纤维素的水溶液
0.48g的2.5重量%亚硝酸钠水溶液
0.60g的20重量%硝酸水溶液
进料1
96g二月桂酸二丁基锡
19.2g甲基丙烯酸甲酯
2.4g丙烯酸正丁酯
2.4g季戊四醇三丙烯酸酯
进料2:
0.25g过氧新癸酸叔丁酯(97%纯度)
进料3:
2.4g的10重量%浓度的叔丁基羟基过氧化物(tert.-butyl hydroxoperoxide)水溶液
进料4:
0.48g的溶解于20g DI水中的抗坏血酸
上述水相在25℃下引入。加入进料1,用高速溶解搅拌器以21000rpm分散混合物。3分钟的分散得到稳定的乳液。在引入进料2之后,将反应批料进行以下温度程序:在60分钟内加热至55℃,在60分钟内加热至80℃,保持该温度60分钟。加入进料3,在冷却至20℃的过程中,在60分钟内进料4。随后,将批料再搅拌30分钟。
这得到分散体,其固体含量为42.2重量%,平均粒径(D0.5)为4.13μm(通过光散射测定的z-平均值)。
随后,将分散体冷冻干燥以除去水,得到灰白色粉末。
使用Malvern Mastersizer 2000,Hydro 2000S样品分散单元,用在文献中记载的标准测量方法测量微胶囊的粒度分布。指定的值是平均值,即D(0,5)。
对于冷冻干燥,将样品在深度为25mm的金属托盘中的干冰上冷冻。在具有LDC-1M温度控制器的Christ Alpha 2-4冷冻干燥机中,在1.013mbar下进行干燥。样品温度调节在-20℃。冰冷凝器的温度<-60℃。当样品和基材的温度均<0℃时结束干燥操作。干燥时间取决于被干燥材料的数量和物理性质。在进行干燥之后,用环境空气对设备充气,并使用刮刀从模具中刮下样品并分配。
根据表1,制备异氰酸酯组分(A)和多元醇组分(B),并在异氰酸酯指数121下反应。测定在23℃下的凝胶时间和在120℃下的完全硬化。为了确定此处的凝胶时间,在室温下将用于制备聚氨酯反应混合物的组分称重到烧杯中,并在高速混合器中以2000转/分钟彼此混合30秒。然后将100g整个体系称入单独的烧杯中,并借助木制刮刀测定凝胶时间。凝胶时间对应于混合过程开始和硬化之间的时间差,即凝块的初始形成。
为了测定在120℃下的完全硬化,在室温下将用于制备聚氨酯反应混合物的组分称重到烧杯中,并在高速混合器中以2000转/分钟彼此混合30秒。借助Pasteur移液管将10mL体系置于表面温度为120℃的板上的金属环内。将施加到板上和在环的内边界处开始硬化之间的时间(以s计)定义为“完全硬化开始”,反应性混合物不再粘附到木制刮刀上的时间定义为固化结束时间。
表1
GT:凝胶时间
FH:开放时间
根据表1获得的聚氨酯的特征在于表2::
表2
C2 | C3 | C4 | E2 | C5 | E3 | |
硬度 | 85 | 84 | 86 | 85 | 85 | 83 |
拉伸强度 | 127,1 | 129,3 | 125,5 | 134,6 | 129,8 | 124,7 |
E-模量 | 2838 | 2938 | 2848 | 2873 | 2919 | 2701 |
断裂伸长率 | 5,2 | 10,5 | 6,1 | 10,1 | 11,1 | 9,3 |
弯曲强度 | 75,1 | 87,7 | 79,4 | 90,2 | 87,5 | 81,7 |
弯曲的E-模量 | 3007 | 3150 | 3097 | 3065 | 3108 | 3108 |
Tg,最大G“ | 105 | 110 | 100 | 110 | 95 | 95 |
表2中的数值按照如下测定:
硬度(肖氏D),根据DIN 53505
拉伸强度(N/mm2),根据DIN 53504
E-模量(MPa),根据DIN EN ISO 527
断裂伸长率(%),根据DIN EN ISO 527
弯曲强度(N/mm2),根据DIN EN ISO 178
弯曲的E-模量(MPa),根据DIN EN ISO 178
玻璃化温度Tg(℃),根据DIN EN ISO 179
实施例1、2和3的储存稳定性示于表3中:
表3
表3示出了储存后的反应性不随新鲜样品的反应性而变化。
Claims (15)
1.制备聚氨酯增强的复合材料的方法,包括混合
(A)多异氰酸酯组分,其包含二异氰酸酯或多异氰酸酯(a)和
(B)多元醇组分,其包含
b)具有至少两个对异氰酸酯具有反应性的基团的化合物,
c)催化剂,
d)任选的其他添加剂,
以形成聚氨酯反应混合物,
将该反应混合物与增强材料在低于100℃的温度下接触并在高于100℃的温度下固化反应混合物,以形成聚氨酯增强的复合材料,
其中催化剂(c)包含微胶囊化的聚氨酯催化剂,其包含含有聚氨酯催化剂的胶囊芯和丙烯酸共聚物胶囊壳,且其中微胶囊的平均粒径D(0,5)为1至50μm。
2.权利要求1的方法,其特征在于,聚氨酯增强的复合材料为聚氨酯纤维增强的复合材料。
3.权利要求1或2的方法,其中聚氨酯催化剂选自二月桂酸二丁基锡、二月桂酸二辛基锡、新癸酸铋、二辛酸铋和乙基己酸铋或其两种或更多种的混合物。
4.权利要求1至3中任一项的方法,其中催化剂(c)的胶囊芯包含疏水性芯材料和聚氨酯催化剂。
5.权利要求1至4中任一项的方法,其中丙烯酸共聚物由以下单元构成:
(i)50至90重量%的至少一种选自丙烯酸的C1-C24烷基酯、甲基丙烯酸的C1-C24烷基酯和乙烯基芳族化合物的单体,
(ii)5至20重量%的至少一种具有至少两个乙烯基不饱和度的单体,和
(iii)0至30重量%的一种或多种其他单体,各自基于单体的总重量计。
6.权利要求1至5中任一项的方法,其中单体(i)包含至少一种在聚合反应后具有70℃或更高的玻璃化转变温度Tg的单体和至少一种在聚合反应后具有50℃或更低的玻璃化转变温度Tg的单体的组合。
7.权利要求1至6中任一项的方法,其中所用的二异氰酸酯和多异氰酸酯(a)包括平均官能度为2.1至2.8的聚合MDI。
8.权利要求1至7中任一项的方法,其中具有至少两个对异氰酸酯具有反应性的基团的化合物(b)包含平均官能度为2至4且具有至少50%的仲OH基团的聚醚醇。
9.权利要求1至8中任一项的方法,其中具有至少两个对异氰酸酯具有反应性的基团的化合物(b)的平均OH值为100至1000mg KOH/g。
10.权利要求1至9中任一项的方法,其中在混合组分(a)-(d)后,反应混合物在25℃下立即具有的粘度小于1500mPas。
11.权利要求1至10中任一项的方法,其中加入小于2.0重量%的在标准压力下具有小于200℃的沸点的物质,以形成聚氨酯反应混合物,基于聚氨酯反应混合物的总重量计。
12.权利要求1至11中任一项的方法,其中将润湿的纤维材料通过模具拉出并硬化,其中模具的温度为100℃至250℃。
13.权利要求1至12中任一项的方法,其中润湿的纤维材料从模具中拉出的速度大于一米/分钟。
14.权利要求1至13中任一项的方法,其中纤维材料的含量为30至90重量%。
15.一种聚氨酯增强的复合材料,其能够通过权利要求11至14中任一项的方法制备。
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