CN102264788B - 制备粘弹性柔性聚氨酯泡沫体的方法 - Google Patents
制备粘弹性柔性聚氨酯泡沫体的方法 Download PDFInfo
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- CN102264788B CN102264788B CN200980152364.9A CN200980152364A CN102264788B CN 102264788 B CN102264788 B CN 102264788B CN 200980152364 A CN200980152364 A CN 200980152364A CN 102264788 B CN102264788 B CN 102264788B
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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
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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Abstract
本发明涉及一种制备粘弹性柔性聚氨酯泡沫体的方法,通过使a)多异氰酸酯与b)含有至少两个对异氰酸酯基团具有活性的氢原子的化合物反应而制备,其特征在于含有至少两个对异氰酸酯基团具有活性的氢原子的化合物为以下物质的混合物:bi)相对于组分bi)、bii)、biii)和biv)的重量计25重量%至70重量%的含羟基天然油或脂肪、或含羟基天然油或脂肪与环氧烷的反应产物;bii)相对于组分bi)、bii)、biii)和biv)的重量计3重量%至30重量%的至少一种聚醚醇,其羟基数为100至800mg KOH/g,官能度为3至5,并且选自通过环氧烷与胺加成而制备的聚醚醇;biii)相对于组分bi)、bii)、biii)和biv)的重量计20重量%至50重量%的至少一种聚醚醇,其羟基数为10至80mg KOH/g,官能度为2至5,并且可通过环氧乙烷和环氧丙烷与H-官能化起始原料的加成而制备,其中环氧乙烷的比例为5-25重量%,基于聚醚醇的重量计,并且至少部分环氧乙烷加成在聚醚链的末端;biv)相对于组分bi)、bii)、biii)和biv)的重量计>0重量%至8重量%的至少一种聚醚醇,其官能度为2至4,羟基数为15至60mg KOH/g,并且环氧乙烷的含量>50重量%,基于聚醚醇的重量计。
Description
本发明涉及一种通过使多异氰酸酯与含有至少两个对异氰酸酯基团具有活性的氢原子的化合物反应而制备粘弹性柔性聚氨酯泡沫体的方法。
粘弹性柔性聚氨酯泡沫体近年来愈来愈重要。其用于——特别是——制备室内装潢、垫子或用于振动的缓冲,例如用于地毯的泡沫衬底中。
为了本发明的目的,泡沫体在根据DIN 53445的扭摆测试中于25℃的损耗因数正切值变化(tan delta)大于0.15、优选大于0.2时为粘弹性的。还优选的是,本发明的泡沫体在宽的温度范围内,即-20℃至+50℃,但至少-5℃至+30℃,显示出粘弹性行为。
泡沫体当根据DIN EN ISO 8307测量的回弹性小于30%、优选为5至25%、特别优选为8至22%时同样为粘弹性的。
特别优选的是,本发明的泡沫体既满足损耗因数的上述标准,又满足回弹性的上述标准。
具有上述阻尼系数的本发明的粘弹性泡沫体被称为“柔软的”泡沫体。
粘弹性优选地通过选择起始原料、特别是多元醇来设定。
一种可能的制备粘弹性泡沫体的方法是使用羟基数为20至100的优选地三官能化的聚醚醇和至少一种羟基数在160至250范围内的、链中存在大量环氧丙烷单元的优选地三官能化的聚醚醇的混合物。
这些泡沫体的缺点是,例如,特别是当甲苯二异氰酸酯(TDI)作为多异氰酸酯使用时,其高比例的闭合孔导致在加工过程中的问题和较差的机械性质。
此外,粘弹性可通过使用至少一种环氧乙烷含量高(优选地至少50重量%)的聚醚醇和至少一种与所述第一种聚醚醇不相容并且环氧丙烷含量高(优选地至少90重量%)的聚醚醇的混合物作为含有至少两个对异氰酸酯基团具有活性的氢原子的化合物而实现。
US 2004/0254256描述了粘弹性泡沫体,在其制备中,多元醇组分包含30至70重量份的在聚醚链中具有高比例的环氧乙烷单元的聚醚醇。EP 1 240 228描述了使用聚醚醇来制备粘弹性泡沫体,所述聚醚醇在聚醚链中的环氧乙烷的含量至少为50重量%并且羟基数在40至50的范围内。
DE19936481描述了吸音的、易于加工的模塑柔性PUR泡沫体,其损耗因数>0.2并且包含至少一种蓖麻油聚醚醇,所述蓖麻油聚醚醇通过使用例如碱金属氢氧化物的阴离子聚合或通过蓖麻油与环氧烷的阳离子聚合制备而来。可任选地加入纯净的蓖麻油,但其用量不多于10%。在此的一个缺点是,仅可加工小量的纯净蓖麻油。完全由于使用必须以额外的制备步骤由蓖麻油制备而来的蓖麻油衍生物,可再生原材料的比例显著增加。另一个缺点是,根据WO 04/20497,由基于可再生原材料(例如蓖麻油)的聚醚醇制备而来的柔性聚氨酯泡沫体在使用碱性催化剂时表现出极差的气味、散发和成雾性质。
DE 3316652描述了由具有减小噪音的性质的粘弹性泡沫体组成的模塑体,所述泡沫体基于极大比例的蓖麻油制备而来,材料密度至少为120kg/m3,并且为自粘的,因此可粘合在支持材料上。
DE 3710731描述了具有隔音和防噪音性质的柔性泡沫体,其材料密度为80-250kg/m3,可包含蓖麻油作为组分,并优选地通过RIM(反应注射成型)法制备。这些模塑泡沫体的损耗因数至少为0.4。由于在≤80的NOC指数下加工反应混合物,所以其具有粘合性表面。
DE3708961描述了具有低回弹性的模塑泡沫体,其包含蓖麻油,并且表现出——在无第二增粘剂的情况下——对经涂布的和未经涂布的金属表面的粘合性。
DE-A-19924803描述了具有胶乳状行为的模塑泡沫体。由于>0.15的损耗因数和<30%的回弹性,所述泡沫体还可称为粘弹性的。其缺点为所述模塑泡沫体具有极粘的表面。
DE19634392描述了用至少50重量%的蓖麻油与含有活性羟基基团的增链剂和/或交联剂来制备发泡聚氨酯模塑体。这些模塑体具有极高的劲度和压缩强度,因此不适于柔性泡沫体的常规用途。
出于生态学原因,市场越来越需要含有可再生原材料的泡沫体。在聚氨酯的制备中,可再生原材料还可为石油化学制备的起始原料的替代品。所述泡沫体通常用含有羟基基团的天然材料或用通过环氧烷与这些化合物的加成而制备的多元醇来制备。
WO 2007/085548示出了可如何在可再生原材料、优选蓖麻油的基础上制备出损耗因数>0.15或回弹性<30%的粘弹性泡沫体。所述泡沫体优选地在宽的温度范围显示出粘弹性行为。其缺点为泡沫体只能通过块状泡沫体方法(slabstock foam process)而获得。所述起始原料的总体活性不足以制备模塑泡沫体。
WO 2008/003567描述了一种用蓖麻油和聚醚链中环氧乙烷含量不同的聚醚醇来制备粘弹性块状泡沫体的方法。在该方法中,使用了较大量的环氧乙烷含量低的聚醚醇和环氧乙烷含量高的聚醚醇。这可导致多元醇组分中的相容性问题,直到分开。
因此,本发明的目的是用可再生原材料来提供具有粘弹性和基本上无粘性表面的优选地柔性聚氨酯泡沫体。所述泡沫体应该能够作为柔性模塑泡沫体和作为柔性块状泡沫体而制备。多元醇组分中的可再生原材料的比例应该高;泡沫体重量的至少25重量%应该优选地包含可再生原材料。
本发明因此提供了一种制备粘弹性柔性聚氨酯泡沫体的方法,通过使下述物质反应而进行
a)多异氰酸酯与
b)含有至少两个对异氰酸酯基团具有活性的氢原子的化合物,其中以下物质的混合物
bi)基于组分bi)、bii)、biii)和biv)的重量计,25重量%至70重量%的含羟基天然油或脂肪、或含羟基天然油或脂肪与环氧烷的反应产物,
bii)基于组分bi)、bii)、biii)和biv)的重量计,3重量%至30重量%的至少一种聚醚醇,所述聚醚醇的羟基数为100至800mgKOH/g,官能度为3至5,并且选自通过环氧烷与胺的加成而制备的聚醚醇,
biii)基于组分bi)、bii)、biii)和biv)的重量计,20重量%至50重量%的至少一种聚醚醇,所述聚醚醇的羟基数为10至80mgKOH/g,官能度为2至5,并且可通过环氧乙烷和环氧丙烷与H官能化起始(starter)物质的加成而制备,其中环氧乙烷的比例为5-25重量%,基于聚醚醇的重量计,并且至少部分环氧乙烷加成在聚醚链的末端,
biv)基于组分bi)、bii)、biii)和biv)的重量计,>0重量%至8重量%的至少一种聚醚醇,所述聚醚醇的官能度为2至4,羟基数为15至60mg KOH/g,并且环氧乙烷的含量>50重量%,基于聚醚醇的重量计,
作为含有至少两个对异氰酸酯基团具有活性的氢原子的化合物。
本发明还提供通过该方法制备的粘弹性柔性聚氨酯泡沫体。
作为含羟基天然油或脂肪bi),可特别是蓖麻油、多羟基脂肪酸、蓖麻油酸、羟基改性油(例如葡萄籽油)、黑枯茗油(black cumin oil)、南瓜籽油、琉璃苣子油(borage seed oil)、大豆油、小麦胚芽油、油菜籽油、向日葵油、花生油、杏仁油、乳香黄连木油、杏仁油、橄榄油、澳洲坚果油(macadamia nut oil)、鳄梨油、沙枣油、芝麻油、大麻油(hemp oil)、榛子油、月见草油、野玫瑰油(wild rose oil)、大麻油(hemp oil)、红花油、核桃油,基于肉豆蔻脑酸、棕榈油酸、油酸、11-十八碳烯酸、岩芹酸、顺9-二十碳烯酸(gadoleic acid)、芥酸、神经酸、亚油酸、α-和γ-亚麻酸、十八碳四烯酸(stearidonic acid)、花生四烯酸、二十碳五烯酸、鰶鱼酸和二十二碳六烯酸(cervonic acid)的羟基改性的脂肪酸和脂肪酸酯。优选使用蓖麻油和氢化蓖麻油,特别是蓖麻油。
天然油和脂肪可通过与环氧烷的加成反应而改性。在此,环氧烷优选地以使加成产物的羟基数为20至150mg KOH/g的量加成。与环氧烷的加成反应可优选地用DMC催化剂来进行。
化合物bi)的官能度优选地为2至4。当没有环氧烷加成时,组分bi)的羟基数优选地在20至200mg KOH/g、特别优选地在100至200mgKOH/g的范围内。
组分bi)的用量优选地为30重量%至60重量%,特别优选40重量%至50重量%,基于组分bi)、bii)、biii)和biv)的重量计。
用于制备组分bii)的胺通常为二胺。这些可为脂族胺(例如乙二胺、丙二胺)或芳香胺(例如甲苯二胺(TDA))。使用TDA时,特别优选使用邻位异构体,也称为连位TDA。
聚醚醇bii)可为纯的丙氧基化物。也可同时使用环氧乙烷,特别是在使用芳香胺时。所用环氧乙烷的量优选地在2重量%至15重量%的范围内,基于聚醚醇计。
组分bii)的羟基数优选地在150至500mg KOH/g的范围内。
组分bii)的用量优选地为5至25重量%,特别优选5至15重量%,基于组分bi)、bii)、biii)和biv)的重量计。
组分biii)的羟基数优选地为15至60mgKOH/g,特别优选地为25至45mgKOH/g。
组分biii)的官能度优选地为2至5,更优选地为2至4并且特别优选地为2至3。
组分biii)的用量优选地为25重量%至40重量%,基于组分bi)、bii)、biii)和biv)的重量计。
在本发明的一个优选的实施方案中,组分biii)包含基于组分biii)的重量计至少80重量%的聚醚醇,该聚醚醇中的环氧乙烷的含量为10重量%至25重量%,基于聚醚醇的重量计。优选将至少一半环氧乙烷加成在该链的末端。在一个特别优选的实施方案中,将全部量的环氧乙烷加成在该链的末端。
组分biii)优选地包含聚醚醇,所述聚醚醇的伯羟基基团含量至少为50%,基于羟基基团的总数计。
组分biv)的用量优选地为1重量%至8重量%,特别优选3重量%至5重量%,各自基于组分bi)、bii)、biii)和biv)的重量计。
组分b)优选地仅由组分bi)、bii)、biii)和biv)组成。然而,组分b)也可包含其它组分。
这些其他组分可为不同于bi)、bii)、biii)和biv)的聚醚醇。
此外,组分b)还可包含增链剂和交联剂。其为分子量为62至400g/mol的优选地H官能化的化合物,特别是2至3官能的醇、胺或氨基醇。它们以特别是0重量%至25重量%、优选2重量%至12重量%的量存在,基于组分b)的重量计。
原则上可使用所有已知的分子中含有至少两个异氰酸酯基团的化合物作为多异氰酸酯a)。优选使用二异氰酸酯。优选地将二苯基甲烷二异氰酸酯(MDI)和/或甲苯二异氰酸酯(TDI)——优选MDI——用于本发明方法。
当使用MDI时,可使用纯的4,4’异构体、纯的2,4’异构体以及可还包含最高达5重量%的2,2’异构体的上述两种异构体的任意混合物。时常用改性的异氰酸酯代替纯的异氰酸酯或与纯的异氰酸酯掺混,因为固体形式的纯MDI是难以加工的。这类改性的异氰酸酯可例如通过将基团引入多异氰酸酯来形成。这类基团的实例有氨基甲酸酯、脲基甲酸酯、碳二亚胺、脲酮亚胺(uretonimine)、异氰脲酸酯、脲和缩二脲基团。
特别优选用氨基甲酸酯基团改性的异氰酸酯,其通常通过使异氰酸酯与低于化学计量的量的H官能化化合物反应而制备。这类化合物还时常称为NCO预聚物。这些预聚物的NCO含量优选地为20重量%至30重量%,特别是24重量%至29重量。用于制备所述预聚物的H官能化化合物通常为多官能的醇,优选聚醚醇。在本发明的一个实施方案中,蓖麻油也可用于制备所述预聚物。不认为其是组分bi)的部分。
同样特别优选含有碳二亚胺或脲酮亚胺的多异氰酸酯,其可通过异氰酸酯与其本身的靶向催化反应而形成。
在本发明的另一个实施方案中,二苯基甲烷二异氰酸酯和多亚苯基多亚甲基多异氰酸酯的混合物——也称为粗MDI——作为多异氰酸酯a)使用。
本发明的柔性聚氨酯泡沫体通常在发泡剂、催化剂和助剂和/或添加剂的存在下制备。
作为发泡剂,优选使用水。所用水的量取决于泡沫体的所需密度,并且优选地在1重量%至5重量%的范围内,基于组分b)的重量计。
代替水或与水一起,还可使用物理作用发泡剂。其优选地为这样的液体,所述液体对聚氨酯形成组分呈惰性的,沸点小于100℃——优选地小于50℃,特别是在50至30℃范围内——,并且在放热的加聚反应影响下汽化。这类液体的实例为烃类(例如正戊烷、异戊烷和/或环戊烷)、醚类、酮类、卤化烃类,只要其没有耗尽臭氧的能力。此外,对聚氨酯的形成组分呈惰性的气体——例如氮气或稀有气体(noble gas),但特别是二氧化碳——可作为物理发泡剂而使用。液体物理作用发泡剂的量通常为1至20重量份、优选2至15重量份,基于100重量份的含有至少两个对异氰酸酯具有活性的氢原子的化合物计。所用发泡剂的量取决于泡沫体的所需密度。
为进行该反应,通常采用常规的聚氨酯催化剂。其为例如叔胺(例如三亚乙基二胺)、金属盐(例如锡化合物)以及这些化合物的任意混合物。
所用助剂和/或添加剂有,例如,阻燃剂、表面活性物质、稳定剂、泡孔调节剂、抑制真菌和抑制细菌物质、抗静电剂、染料、颜料和填充剂。为了赋予特殊性质而需要时,将这些材料加入至泡沫体体系。
所用组分的更多细节可见于,例如,Kunststoff-Handbuch,卷VIIPolyurethane,Carl Hanser Verlag,Munich,Vienna,第一至第三版,1966,1983和1993。
通常使所用含有至少两个对异氰酸酯基团具有活性的氢原子的化合物组b)、发泡剂、催化剂和任意助剂和/或添加剂混合而形成多元醇组分,并以该形式与多异氰酸酯a)反应。
为制备本发明的柔性聚氨酯泡沫体,通常使起始化合物于0至100℃——优选15至60℃——的温度下以下述比例反应:相对于每个NCO基团存在0.5至2、优选0.6至1.3并且特别是0.7至1个活性氢原子,并且,当用水作为发泡剂时,水的两个氢原子被包括在活性氢原子的总数的计算中。
本发明的柔性聚氨酯泡沫体优选地通过一步法、通过将多元醇组分和异氰酸酯组分混合而制备,其中所述多元醇组分包含——如上所述——含有至少两个对异氰酸酯具有活性的氢原子的化合物、任选地催化剂、发泡剂以及助剂和/或添加剂,并且所述异氰酸酯组分包含多异氰酸酯以及任选地催化剂、物理发泡剂以及助剂和/或添加剂。这两种组分被充分混合,并通常被发泡为模塑泡沫体。此处,在所述多元醇组分中没有相容性问题且没有分开现象发生。
如上所述,本发明的泡沫体为粘弹性泡沫体。上文已描述了这些泡沫体的性质。本发明的泡沫体同样具有上述这些特征。
本发明的泡沫体用于特别是绝缘和阻尼元件,特别是用于交通工具结构,用于室内装潢家具或者用于坐或躺的家具,用于矫形外科领域和/或医疗领域的垫子或软垫,或用于鞋底或内底。其它用途为汽车的安全部件、用于存放物体的表面、家具领域和汽车构造中的扶手和类似部件。
本发明通过以下实施例示例说明。
多元醇1:甘油起始的聚氧丙烯-聚氧乙烯多元醇,羟基数=26mgKOH/g,环氧乙烷含量=21重量%,基于多元醇计,作为末端嵌段
多元醇2:甘油起始的聚氧丙烯-聚氧乙烯多元醇,羟基数=42mgKOH/g,环氧乙烷含量=72重量%,基于多元醇计,其中基于多元醇计5重量%作为末端嵌段而存在
多元醇3:乙二胺起始的聚氧丙烯多元醇,羟基数=470mg KOH/g
TegostabB 4113:硅酮稳定剂,Evonik
LupragenN 201:二氮杂二环辛烷,33%浓度的双丙甘醇溶液,BASF SE
通过混合表中所示的多元醇、催化剂和添加剂来制备均匀的多元醇组分。所示量以重量%计。
使所述多元醇组分与基于MDI的异氰酸酯组分以所示指数充分混合;然后将该混合物引入至金属模具,该模具的体积为14.5升,尺寸为40*40*10cm,并且一侧被斜切,已将该模具加热至55℃,其中,关闭盖子8至10分钟之后,混合物固化得到柔性泡沫体。在实施例1中,手动地混合多元醇组分和MDI组分。在实施例2至4中,借助购自Elastogran Maschinenbau GmbH的高压Puromat PU SV 20/3机械混合所述多元醇组分和MDI组分。
来自Elastogran GmbH的基于二苯基甲烷二异氰酸酯和多亚苯基多亚甲基多异氰酸酯的混合物的Iso 145/8作为异氰酸酯组分被使用。NCO含量为32.8%。
所示的性质根据以下标准确定:
粘性的评估是通过从模具中移除之后立即将手放在新制的泡沫体表面来测试表面是否是粘性的来进行的。
Claims (15)
1.一种制备粘弹性柔性聚氨酯泡沫体的方法,通过使下述物质反应而进行
a)多异氰酸酯与
b)含有至少两个对异氰酸酯基团具有活性的氢原子的化合物,其中以下物质的混合物
bi)基于组分bi)、bii)、biii)和biv)的重量计25重量%至70重量%的蓖麻油,
bii)基于组分bi)、bii)、biii)和biv)的重量计5重量%至25重量%的至少一种聚醚醇,所述聚醚醇的羟基数为100至800mgKOH/g,官能度为3至5,并且选自通过环氧烷加成于胺上而制备的聚醚醇,
biii)基于组分bi)、bii)、biii)和biv)的重量计20重量%至50重量%的至少一种聚醚醇,所述聚醚醇的羟基数为10至80mgKOH/g,官能度为2至5,并且可通过环氧乙烷和环氧丙烷与H-官能化起始物质的加成而制备,其中环氧乙烷的比例为5-25重量%,基于聚醚醇的重量计,并且至少部分环氧乙烷加成在聚醚链的末端,
biv)基于组分bi)、bii)、biii)和biv)的重量计>0重量%至8重量%的至少一种聚醚醇,所述聚醚醇的官能度为2至4,羟基数为15至60mg KOH/g,并且环氧乙烷的含量>50重量%,基于聚醚醇的重量计,
作为含有至少两个对异氰酸酯基团具有活性的氢原子的化合物。
2.权利要求1的方法,其中组分bi)的用量为30重量%至60重量%,基于组分bi)、bii)、biii)和biv)的重量计。
3.权利要求1的方法,其中组分bii)的羟基数在150至500mgKOH/g的范围内。
4.权利要求1的方法,其中组分bii)的用量为5至15重量%,基于组分bi)、bii)、biii)和biv)的重量计。
5.权利要求1的方法,其中组分biii)的羟基数为15至60mgKOH/g。
6.权利要求1的方法,其中组分biii)的用量为25至40重量%,基于组分bi)、bii)、biii)和biv)的重量计。
7.权利要求1的方法,其中组分biv)的用量为1重量%至8重量%,基于组分bi)、bii)、biii)和biv)的重量计。
8.权利要求1的方法,其中组分biv)的环氧乙烷含量>70重量%,基于聚醚醇的重量计。
9.权利要求1的方法,其中二苯基甲烷二异氰酸酯作为多异氰酸酯a)使用。
10.权利要求1的方法,其中二苯基甲烷二异氰酸酯和多亚苯基多亚甲基多异氰酸酯的混合物作为多异氰酸酯a)使用。
11.权利要求1的方法,其中含有异氰酸酯基团和氨基甲酸酯基团的、二苯基甲烷二异氰酸酯和含有对异氰酸酯基团具有活性的氢原子的化合物的反应产物作为多异氰酸酯a)使用。
12.权利要求11的方法,其中蓖麻油作为含有对异氰酸酯基团具有活性的氢原子的化合物使用。
13.权利要求1的方法,其中反应在发泡剂的存在下进行。
14.权利要求13的方法,其中水作为发泡剂使用。
15.可根据权利要求1至14之一制备的柔性聚氨酯泡沫体。
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