CN117677646A - 具有低脆性和有所改善的附着性的异氰酸酯-环氧树脂混合泡沫材料 - Google Patents
具有低脆性和有所改善的附着性的异氰酸酯-环氧树脂混合泡沫材料 Download PDFInfo
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- CN117677646A CN117677646A CN202280051112.2A CN202280051112A CN117677646A CN 117677646 A CN117677646 A CN 117677646A CN 202280051112 A CN202280051112 A CN 202280051112A CN 117677646 A CN117677646 A CN 117677646A
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- Prior art keywords
- isocyanate
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- acid
- compound
- epoxy
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- 239000012948 isocyanate Substances 0.000 claims abstract description 48
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- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 claims abstract description 14
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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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
-
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Abstract
本发明涉及一种制备异氰酸酯‑环氧树脂混合泡沫材料的方法,其中将聚异氰酸酯(a)与至少两个具有至少两个针对异氰酸酯有反应活性的氢的化合物(b)、至少一个具有至少两个环氧基的化合物(c)、至少一个加快该具有至少两个针对异氰酸酯有反应活性的氢的化合物(b)和该具有环氧基的化合物(c)与聚异氰酸酯(a)的反应的催化剂(d)、含有甲酸的化学和/或物理发泡剂(e)、以及视情况采用的助剂和添加剂(f)混合成反应混合物,其中,聚异氰酸酯(a)中的异氰酸酯基与该具有至少两个环氧基的化合物(c)中的环氧基的当量比为1.2:1至500:1,并且,将所述反应混合物反应成泡沫材料,其特征在于,所述具有至少两个针对异氰酸酯有反应活性的氢原子的化合物(b)具有至少一个羟基值为195至400且平均标称官能度为2至4的聚酯醇(b1),并且具有至少一个羟基值为40至80且平均标称官能度为2.6至6.5的聚醚多元醇(b2)。本发明还涉及一种依据这种方法获得的异氰酸酯‑环氧树脂混合泡沫材料,以及涉及包含本发明的异氰酸酯‑环氧树脂混合泡沫材料的夹层式元件。
Description
说明书
本发明涉及一种制备密度为15g/L至60g/L的异氰酸酯-环氧树脂混合泡沫材料的方法,其中将聚异氰酸酯(a)与至少两个具有至少两个针对异氰酸酯有反应活性的氢的化合物(b)、至少一个具有至少两个环氧基并且环氧当量为90g/eq至500g/eq的化合物(c)、至少一个加快所述具有至少两个针对异氰酸酯有反应活性的氢的化合物(b)和所述具有环氧基的化合物(c)与所述聚异氰酸酯(a)的反应的催化剂(d)、含有甲酸的化学和/或物理发泡剂(e)、以及视情况采用的助剂和添加剂(f)混合成反应混合物,其中,所述聚异氰酸酯(a)中的异氰酸酯基与所述具有至少两个环氧基的化合物(c)中的环氧基的当量比为1.2:1至500:1,并且,将所述反应混合物反应成泡沫材料,其特征在于,所述具有至少两个针对异氰酸酯有反应活性的氢原子的化合物(b)具有至少一个羟基值为195至400且平均标称官能度为2至4的聚酯醇(b1),并且具有至少一个羟基值为40至80且平均标称官能度为2.6至6.5的聚醚多元醇(b2)。本发明还涉及一种依据这种方法获得的异氰酸酯-环氧树脂混合泡沫材料,以及涉及包含本发明的异氰酸酯-环氧树脂混合泡沫材料的夹层式元件。
例如在US 3 793 236、US 4 129 695和US 3 242 108中描述过用异氰酸酯和聚环氧化物制备泡沫。此外已知的是,除异氰酸酯和聚环氧化物以外,也可使用多元醇。这例如记载于US 3 849 349中。此泡沫材料的优点在于其高耐燃性。
KR 102224864描述过一种针对液化气罐的绝缘材料,其用发泡混合物制备,包含6官能聚醚多元醇、8官能聚醚多元醇、3官能聚醚多元醇、芳香族聚酯多元醇、异氰酸酯、发泡剂和双酚基环氧化物。
WO2004085509揭示过含有充当物理发泡剂的正戊烷的异氰尿酸酯-环氧树脂泡沫材料。
US2013324626揭示过聚氨酯夹层式元件及其制备。
EP3059270揭示过基于异氰酸酯-环氧树脂的、具有高阻燃性的泡沫材料。通过将异氰酸酯、环氧化物、具备针对异氰酸酯有反应活性的基团的催化剂和发泡剂反应成泡沫材料,获得这类泡沫材料。
较新的现有技术描述过用聚异氰酸酯和聚环氧化物,通过含有部分三聚化的异氰尿酸酯基(=中间物)的中间阶段制备这类异氰酸酯-环氧树脂混合泡沫材料的优选方案,借助终止剂将其稳定化。在此情形下,通过将由聚异氰酸酯、聚环氧化物、催化剂和终止剂构成的反应混合物反应成储存稳定的粘性较高的中间物(“预三聚化”),并且通过添加发泡剂和自发地加快异氰酸酯/环氧化物反应的催化剂,将此粘度较高的中间物转化成最终的发泡的、不再能熔化的最终状态,获得耐高温的泡沫材料。EP3259295例如描述过这类异氰酸酯-环氧树脂混合泡沫材料。其中根据EP 3259295的揭示,即使在不采用终止剂的情况下也能制备环氧化物-异氰酸酯泡沫(EPIC泡沫),且其仍具备高阻燃性。
根据WO 2012/80185 A1和WO 2012/150201 A1,在将特定的发泡剂用于制备EPIC泡沫材料的情况下,能够显著改善如此制备的泡沫的品质。根据这些文献的原理,同样优选在存在用作终止剂的稳定剂的情况下,通过反应物的反应制备EPIC泡沫。
这些异氰酸酯-环氧树脂混合泡沫材料,尤其在其利用二阶段方法制备的情况下,具有异氰酸酯-(NCO)基的反应不令人满意的缺点。然而,泡沫中的游离的(未反应的)异氰酸酯基(所谓的“残余NCO”)可能会导致非期望的老化过程,如附着问题和机械属性的劣化(例如脆化)。
根据EP3259294,通过使用碳二亚胺结构(<10wt%)改善NCO基的反应。在EP3259293中揭示过以单阶段方法,在不作后续退火的情况下,以异氰酸酯和聚环氧化物为基础制备这类异氰酸酯-环氧树脂混合泡沫材料。借助加快异氰酸酯-环氧化物反应的可置入的催化剂来制备泡沫。然而,这些泡沫材料的机械属性,特别是脆性和针对金属的附着性仍有待改善,在制造夹层式元件时尤其涉及这一点。
在用特别是金属覆盖层和由基于异氰酸酯的泡沫材料构成的泡沫材料制造复合式元件(往往也称作夹层式元件)时,可不连续地进行制造,或者例如在连续工作的双带式设备上连续地制造。其中,目前广泛采用在双带式设备上进行的连续制造。除了用于冷库绝缘的夹层式元件以外,用于构建各种楼宇的立面的元件也变得愈发重要。
有鉴于此,本发明的目的在于改善异氰酸酯-环氧树脂混合泡沫材料的机械属性,特别是脆性及其针对金属的附着性。本发明意外发现,通过组合式选择特定的聚异氰酸酯、发泡剂和使用高分子以及低分子多元醇,所能获得的泡沫材料的脆性和针对金属覆盖层的附着性远超按照现有技术基于异氰酸酯和环氧树脂制备的泡沫。
本发明用以达成上述目的的解决方案为一种密度为15g/L至60g/L的异氰酸酯-环氧树脂混合泡沫材料,可按照以下方法制备:其中将聚异氰酸酯(a)与至少两个具有至少两个针对异氰酸酯有反应活性的氢的化合物(b)、至少一个具有至少两个环氧基并且环氧当量为90g/eq至500g/eq的化合物(c)、至少一个加快所述具有至少两个针对异氰酸酯有反应活性的氢的化合物(b)和所述具有环氧基的化合物(c)与所述聚异氰酸酯(a)的反应的催化剂(d)、含有甲酸的化学和/或物理发泡剂(e)、以及视情况采用的助剂和添加剂(f)混合成反应混合物,其中,异氰酸酯基与环氧基的当量比为1.2:1至500:1,并且,将所述反应混合物反应成所述异氰酸酯-环氧树脂混合泡沫材料,其特征在于,所述具有至少两个针对异氰酸酯有反应活性的氢原子的化合物(b)具有至少一个羟基值为195至400且平均标称官能度为2至4的聚酯醇(b1),并且具有至少一个羟基值为40至80且平均标称官能度为2.6至6.5的聚醚多元醇(b2)。
本发明的另一标的为一种制备本发明的异氰酸酯-环氧树脂混合泡沫材料的方法,及其在用覆盖层与由异氰酸酯-环氧树脂混合泡沫材料构成的芯部制造复合式元件(所谓的夹层式元件)的过程中的应用。优选地,将诸如钢板、铝板或铜板的金属覆盖层用作覆盖层。
所述制造夹层式元件的方法可连续地或不连续地进行。例如在双带式设备的启动过程中,以及就利用不连续工作的压机制造的复合式元件而言,可采用不连续的工作方式。在使用双带式设备时为连续式应用。其中,在采用双带工艺时,例如以高压或低压技术制备反应混合物,并且通常利用往复式或固定式浇注耙(Gieβharken)将反应混合物施覆至下部覆盖层上。随后将上部覆盖层施覆至固化(ausreagierend)的反应混合物上。随后最终固化成泡沫材料,优选仍在双带式设备中进行。这类方法是已知的,对其的描述例如参阅Kunststoffhandbuch(塑料手册),第7卷,“Polyurethane(聚氨酯)”,Carl-Hanser-VerlagMünchen,第3版,1993,章节4.2.2、6.2.2和6.2.3。
可以将柔性或刚性的覆盖层,优选刚性的覆盖层,如石膏板、玻璃砖、铝箔、铝板、铜板或钢板,优选将铝箔、铝板或钢板,特别优选将钢板用作覆盖层。其中,覆盖层也可经过涂布,例如涂布有常见的漆。覆盖层可经过涂布,或未经涂布。可对覆盖层进行预处理,例如采用Corona处理、电弧处理、等离子处理,或者采用其他常见方法。
优选地,在双带工艺中以1m/min至60m/min、优选2m/min至50m/min、特别优选2.5m/min至30m/min并且特别是2.5m/min至20m/min的恒定速度输送覆盖层。其中,至少从施覆泡沫系统起,覆盖层便处于大体水平的位置中。
在将反应混合物施覆至下部覆盖层上前,在将反应混合物施覆至下部覆盖层上前,优选将所述覆盖层从卷筒展开,视情况对其进行压型,视情况对其进行加热,视情况对其进行预处理以增强可发泡性,并且可选地为其涂布增附剂。在连续式双带工艺中,优选在双带式设备中将反应混合物固化,并且最终裁切至期望的长度。
可将已知的有机的、脂肪族的、脂环族的、芳脂族的异氰酸酯,并且优选将芳香族的多元异氰酸酯用作聚异氰酸酯(a)。这类多官能异氰酸酯是已知的,或可按照已知方法制备。多官能异氰酸酯特别是也可用作混合物,使得组份(a)在此情形下含有不同的多官能异氰酸酯。针对每个分子,可视作聚异氰酸酯的多官能异氰酸酯具有两个(下文称作二异氰酸酯)或两个以上的异氰酸酯基。
具体而言特别是包括:亚烷基残基中包含4至12个碳原子的亚烷基二异氰酸酯,如1,12-十二烷二异氰酸酯、2-乙基四亚甲基-1,4-二异氰酸酯、2-甲基五亚甲基-1,5-二异氰酸酯、四亚甲基-1,4-二异氰酸酯、优选六亚甲基-1,6-二异氰酸酯;环脂族二异氰酸酯,如环己烷-1,3-二异氰酸酯和环己烷-1,4-二异氰酸酯以及这些异构体的任何混合物,1-异氰酸基-3,3,5-三甲基-5-异氰酸基甲基环己烷(IPDI),2,4-和2,6-六氢甲苯二异氰酸酯以及对应的异构体混合物,4,4'-、2,2’-和2,4'-二环己基甲烷二异氰酸酯以及对应的异构体混合物,并且优选为芳香族聚异氰酸酯,如2,4-和2,6-甲苯二异氰酸酯以及对应的异构体混合物,4,4'-、2,4'-和2,2'-二苯基甲烷二异氰酸酯以及对应的异构体混合物,4,4'-与2,4'-二苯基甲烷二异氰酸酯的混合物,多苯基多亚甲基多异氰酸酯,4,4'-、2,4'-和2,2'-二苯基甲烷二异氰酸酯与多苯基多亚甲基多异氰酸酯的混合物(粗MDI),以及粗MDI与甲苯二异氰酸酯的混合物。
尤其适用的是2,2’-、2,4'-和/或4,4'-二苯基甲烷二异氰酸酯(MDI),1,5-亚萘基二异氰酸酯(NDI),2,4-和/或2,6-甲苯二异氰酸酯(TDI),3,3'-二甲基二苯基二异氰酸酯,1,2-二苯基乙烷二异氰酸酯和/或对苯二异氰酸酯(PPDI),三亚甲基二异氰酸酯,四亚甲基二异氰酸酯,五亚甲基二异氰酸酯,六亚甲基二异氰酸酯,七亚甲基二异氰酸酯和/或八亚甲基二异氰酸酯,2-甲基-1,5-五亚甲基二异氰酸酯,2-乙基亚丁基-1,4-二异氰酸酯,五亚甲基-1,5-二异氰酸酯,亚丁基-1,4-二异氰酸酯,1-异氰酸基-3,3,5-三甲基-5-异氰酸基甲基环己烷(异佛尔酮二异氰酸酯,IPDI),1,4-和/或1,3-双(异氰酸基甲基)环己烷(HXDI),1,4-环己烷二异氰酸酯,1-甲基-2,4-和/或-2,6-环己烷二异氰酸酯,以及4,4’-、2,4'-和/或2,2'-二环己基甲烷二异氰酸酯。
往往也使用改性聚异氰酸酯,即通过聚异氰酸酯的化学反应获得的产物,且其每个分子具有至少两个反应性的异氰酸酯基。特别是提及含有酯、脲、缩二脲、脲基甲酸酯、碳二亚胺、异氰脲酸酯、脲二酮、氨基甲酸酯和/或氨基甲酸乙酯基团的聚异氰酸酯,通常也与未反应的多异氰酸酯一起。
特别优选地,所述组份(a)的聚异氰酸酯含有2,2‘-MDI或2,4‘-MDI或4,4‘-MDI(也称作单体二苯基甲烷或MMDI)或低聚MDI,其由MDI的高核同系物构成,这些同系物具有3个芳香核和至少为3的官能度,或者含有由前述二苯基甲烷异氰酸酯中的两个或三个构成的混合物,或者含有在制备MDI时产生的粗MDI,或者优选地含有由MDI的至少一个低聚物与前述低分子量MDI衍生物2,2‘-MDI、2,4‘-MDI或4,4‘-MDI(也称作聚合MDI)中的至少一者构成的混合物。通常通过对粗MDI进行蒸馏获得MDI的异构体和同系物。
优选地,除了两核MDI以外,聚合MDI还含有MDI的一个数个官能度大于2、特别是为3或4或5的多核缩合产物。聚合MDI是已知的,并且通常被称作多苯基多亚甲基多异氰酸酯。
含有聚合MDI的聚异氰酸酯的平均官能度可在约2.2至约4、特别是2.4至3.8、尤其是2.6至3.0的范围内变化。具有不同官能度的基于MDI的多官能异氰酸酯的这种混合物特别是粗MDI,其为MDI制备过程中的中间产物。
多官能异氰酸酯,或者数个基于MDI的多官能异氰酸酯是已知的,例如BASFPolyurethanes GmbH销售的M20或者/>M50。
相对于组份(a)的总重量而言,组份(a)含有优选至少70wt%、特别优选90wt%、特别是100wt%的一或数个异氰酸酯,其选自由2,2‘-MDI、2,4‘-MDI、4,4‘-MDI和MDI低聚物构成的群组。其中,相对于组份(a)的总重量而言,低聚MDI的含量优选为至少20wt%,特别优选大于30wt%乃至小于80wt%。
可以将任意的常用于聚氨酯制备的有机化合物用作具有至少两个针对异氰酸酯有反应活性的氢原子的化合物(b)。本发明的化合物(b)包括至少一个聚酯醇(b1)和至少一个聚醚多元醇(b2),所述至少一个聚酯醇的羟基值为195mg KOH/g至400mg KOH/g,优选为200mg KOH/g至300mg KOH/g,平均标称官能度为2至4,所述至少一个聚醚多元醇的羟基值为40mg KOH/g至80mg KOH/g,优选为50mg KOH/g至70mg KOH/g,平均标称官能度为2.6至6.5,优选为3至4.5。其中,在本发明的范围内,平均标称官能度是指起始化合物的平均官能度。在多元醇(b)、特别是聚醚多元醇(b2)的制备过程中因制备中的副反应而发生的官能度降低不被纳入考量。
组份(b)还可含有扩链剂和/或交联剂(b3),以及其他在聚氨酯化学中常见的、不归属于化合物(b1)至(b3)的定义范围的、包含至少两个针对异氰酸酯有反应活性的氢原子的化合物。这类其他包含针对异氰酸酯有反应活性的氢原子的化合物是已知的,对其的描述例如参阅Kunststoffhandbuch(塑料手册),第7卷,“Polyurethane(聚氨酯)”,Carl-Hanser-Verlag München,第3版,1993,章节3.1或6.1.1。
优选地,在组份(b)中,除组份(b1)和(b2)以外,相对于组份(b)的总重量而言,含有小于20wt%的、特别优选小于10wt%的其他包含至少两个能够与异氰酸酯基反应的氢原子的化合物,特别是不含此种化合物。
聚酯醇(b1)在聚酯醇(b1)与聚醚醇(b2)的总重量中所占的重量比优选为40wt%至80wt%,特别优选为50wt%至75wt%,并且特别是为60wt%至70wt%。
优选用芳香族二羧酸,或者用由芳香族和脂肪族二羧酸构成的混合物,特别优选仅用芳香族二羧酸和多元醇来制备适用的聚酯多元醇(b1)。作为游离二羧酸的替代,也可使用对应的二羧酸衍生物,例如具有1至4个碳原子的醇的二羧酸酯或者二羧酸酐。
优选以混合物形式或者单独地将邻苯二甲酸、邻苯二甲酸酐、对苯二甲酸和/或间苯二甲酸用作芳香族二羧酸或芳香族二羧酸衍生物,特别优选使用邻苯二甲酸、邻苯二甲酸酐、对苯二甲酸或者由这些酸中的至少2个构成的混合物。特别优选使用对苯二甲酸或者对苯二甲酸二甲酯,尤其是对苯二甲酸。脂肪族二羧酸可与少量的芳香族二羧酸混合使用。脂肪族二羧酸的示例为琥珀酸、戊二酸、己二酸、辛二酸、壬二酸、癸二酸、癸烷二羧酸、马来酸和富马酸。优选地,相对于酸组份和醇组份的总重量而言,所述至少二官能的芳香酸的比例为至少20wt%。
多元醇的示例为:乙二醇、二乙二醇、1,2-或1,3-丙二醇、二丙二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、1,10-癸二醇、甘油、三羟甲基丙烷和季戊四醇,或其烷氧基化物。优选使用二乙二醇、二丙二醇、丙二醇、甘油、三羟甲基丙烷,或其烷氧基化物,或者由所述多元醇中的至少两个构成的混合物。
在本发明的一个特定实施方式中,也将一种聚醚醇用作多元醇,其为甘油和/或三羟甲基丙烷与环氧乙烷和/或环氧丙烷(优选与环氧乙烷)的反应产物,其中,该聚醚醇的OH值处于500mg KOH/g至750mg KOH/g的范围内。由此改善组份(b1)的储存稳定性。
为了制备聚酯多元醇(b1),除了芳香族二羧酸或其衍生物以及多元醇以外,优选也使用至少一个脂肪酸或脂肪酸衍生物,优选使用脂肪酸。
所述脂肪酸可以含有羟基。所述脂肪酸还可含有双键。
在本发明的一个实施方式中,所述脂肪酸优选不含羟基。
优选地,相对于组份(b1)的重量而言,组份(b1)的平均脂肪酸含量大于1wt%、优选大于2.5wt%、优选大于4wt%、并且特别优选大于5wt%。优选地,相对于组份(b3)的总重量而言,组份(b1)的平均脂肪酸含量小于30wt%、优选小于20wt%。
优选地,所述脂肪酸或者脂肪酸衍生物是基于可再生原材料的脂肪酸或者脂肪酸衍生物,选自由以下构成的组:蓖麻油、多羟基脂肪酸、蓖麻油酸、羟基改性油、葡萄籽油、黑页蒿子油、南瓜籽油、琉璃苣籽油、大豆油、小麦籽油、菜籽油、葵花籽油、花生油、杏核油、开心果油、杏仁油、橄榄油、澳洲坚果油、鳄梨油、沙棘油、芝麻油、大麻油、榛子油、月见草油、野玫瑰油、红花油、核桃油、基于肉豆蔻油酸的羟基改性脂肪酸和脂肪酸酯、棕榈油酸、油酸、异油酸、岩芹酸、鳕烯酸、芥酸、神经酸、亚油酸、亚麻酸、十八碳四烯酸、花生四烯酸、花生五烯酸、二十二碳五烯酸和二十二碳六烯酸。
特别优选将油酸用作脂肪酸。
为了制备聚酯多元醇(b1),可在无催化剂的情况下,或者优选在存在酯化催化剂的情况下,优选在诸如氮气的惰性气体氛围中,在150℃至280℃、优选180℃至260℃下的熔体中,视情况而定在减压条件下,将脂肪族和芳香族聚羧酸和/或衍生物与多元醇缩聚至期望的酸值,其有利地小于10,优选小于2。根据一个优选实施方式,在上述温度下,在常压下且随后在小于500mbar、优选为40mbar至400mbar的压力下,将所述酯化混合物缩聚至400至195、优选350至200的羟基值。例如将金属、金属氧化物或金属盐形式的铁、镉、钴、铅、锌、锑、镁、钛和锡催化剂用作酯化催化剂。但也可在液相中,在存在稀释剂和/或夹带剂(例如苯、甲苯、二甲苯或氯苯)的情况下进行缩聚,以对缩合水进行共沸蒸馏。
为了制备聚酯多元醇(b1),优选将聚羧酸和/或衍生物与多元醇以1:1至2.3,优选1:1.05至2.2,并且特别优选1:1.1至2.1的摩尔比缩聚。
优选地,所述聚酯多元醇(b1)的数均官能度大于等于2、优选大于2、特别优选大于2.2并且特别是大于2.3,这使得如此制备的聚氨酯具有较高的交联密度,进而有助于改善聚氨酯泡沫的机械属性。特别优选地,所述聚酯多元醇(b1)的数均官能度小于4、特别是小于3。
一般而言,获得的聚酯多元醇(b1)具有250g/mol至1200g/mol、优选300g/mol至1000g/mol、特别是400g/mol至700g/mol的数均分子量。
通常通过将环氧烷附加至H官能起始物质上来制备聚醚醇(b2)。此方法众所周知,并且常用于制备此类产物。
可将醇或胺用作起始物质。可将诸如乙二胺的脂肪胺用作胺。在本发明的另一实施方式中,可使用芳香胺,特别是甲苯二胺(TDA)或者由二苯基甲烷二胺与多亚苯基多亚甲基多胺构成的混合物。在本发明的一个特别优选的实施方式中,所述组份b)含有基于脂肪胺、特别是乙二胺的聚醚醇。
因此,为了制备聚醚醇(b1),优选将多官能醇用作H官能起始物质。
除了胺以外,也可将醇用作起始分子。示例为二醇,如乙二醇或丙二醇,甘油,三羟甲基丙烷,季戊四醇,以及糖醇,如蔗糖或山梨醇,形式例如为不同醇的混合物。特别是将诸如蔗糖或山梨醇的固态起始物质与诸如二醇或甘油的液态起始物质混合。其中,选择数均官能度作为起始物质的起始官能度。
在一个特别优选的实施方式中,将仅通过一个胺起始的聚醚用作聚醚(b2)。
优选将环氧乙烷、环氧丙烷或者由这些化合物构成的混合物用作环氧烷。特别优选使用纯环氧丙烷或者由环氧乙烷与环氧丙烷构成的混合物,其中,在接近反应末尾时添加环氧乙烷,从而获得具有初级羟基的环氧乙烷端基。在此情形下,使用相对于环氧丙烷和环氧乙烷的总重量而言比例优选为至少50wt%、特别优选为至少70wt%、特别是为至少80wt%的环氧丙烷。
优选在有催化剂存在的情况下将环氧化物附加至起始物质上。在多数情况下将碱性化合物用作催化剂,其中,碱金属或碱土金属的氧化物以及特别是氢氧化物在技术上最为重要。在多数情况下将氢氧化钾用作催化剂。
在本发明的一个实施方式中,将胺用作用于制备聚醚醇(b2)的催化剂。其中,优选采用具有至少一个三级氨基的胺,咪唑,胍,或其衍生物。优选地,这些胺类催化剂具有至少一个能够与环氧烷反应的基团,例如初级或二级胺基,或者特别优选具有羟基。
所述含有环氧基的组份c)是任意的具有至少两个环氧基的有机化合物,如脂肪族、脂环族、芳香族和/或杂环化合物,其中,所述含有环氧基的组份c)的环氧当量为90g/eq至500g/eq。适合充当组份c)的优选的环氧化物具有每个分子2至4个、优选2个环氧基,并且具有优选95g/eq至400g/eq、特别优选140g/eq至220g/eq的环氧当量。
适合的聚环氧化物例如为多元酚的聚缩水甘油醚,这些多元酚例如是邻苯二酚,间苯二酚,对苯二酚,4,4'-二羟基二苯基丙烷(双酚A),4,4'-二羟基-3,3'-二甲基二苯基甲烷,4,4'-二羟基二苯基甲烷(双酚F),4,4'-二羟基二苯基环己烷,4,4'-二羟基-3,3'-二甲基二苯基丙烷,4,4'-二羟基联苯,4,4'-二羟基二苯砜(双酚S),三-(4-羟基苯基)-甲烷,前述二酚的氯化产物和溴化产物,酚醛清漆(即一元或多元酚和/或甲酚与醛、特别是甲醛在酸性催化剂存在的情况下以小于1:1的当量比反应生成的产物),通过将2摩尔芳香族氧基羧酸的钠盐与一摩尔二卤代烷或二卤代二烷基酯酯化获得的二酚(参阅英国专利案1017 612),或者通过将酚与含有至少两个卤素原子的长链卤代烷烃缩合获得的多酚(参阅GB-PS1 024 288)。还提及的是:基于芳香胺和环氧氯丙烷的聚环氧化合物,例如N-二-(2,3-环氧丙基)-苯胺,N,N'-二甲基-N,N'-二环氧丙基-4,4'-二氨基二苯基甲烷,N,N-二环氧丙基-4-氨基-苯基缩水甘油醚(参阅GB-PS 772 830和816 923)。
此外可采用:芳香族、脂肪族和脂环族多元羧酸的缩水甘油酯,例如邻苯二甲酸二缩水甘油酯,间苯二甲酸二缩水甘油酯,对苯二甲酸二缩水甘油酯,己二酸二缩水甘油酯,以及1摩尔芳香族或脂环族二羧酸酐与1/2摩尔二醇或1/n摩尔包含n个羟基的多元醇的反应产物的缩水甘油酯,或者六氢邻苯二甲酸二缩水甘油酯,其可视情况被甲基取代。
也可使用多元醇的缩水甘油酯,例如1,4-丁二醇的缩水甘油酯(DY-D,Huntsman),1,4-丁烯二醇的缩水甘油酯,甘油的缩水甘油酯,三羟甲基丙烷的缩水甘油酯(DY-T/CH,Huntsman),季戊四醇的缩水甘油酯,以及聚乙二醇的缩水甘油酯。此外还可采用异氰脲酸三缩水甘油酯,N,N'-二环氧基丙氧基酰胺,多元硫醇的聚缩水甘油基硫醚,如双巯基甲基苯,二缩水甘油基三亚甲基三砜,基于乙内酰脲的聚缩水甘油醚。
最后,也可使用多不饱和化合物的环氧化产物,如植物油及其转化产物。也可使用二烯烃和聚烯烃的环氧化产物,如丁二烯,乙烯基环己烷,1,5-环辛二烯,1,5,9-环十二碳三烯,含有尚可环氧化的双键的聚合物和共聚物,例如基于聚丁二烯,聚异戊二烯,丁二烯-苯乙烯共聚物,二乙烯基苯,二环戊二烯,不饱和聚酯,还可使用烯烃的环氧化产物,其可通过Diels-Alder加成获得且随后通过采用过化合物的环氧化转化成聚环氧化物,或者含有通过桥原子或桥原子团连接的两个环戊烯环或环己烯环的化合物。
此外也可使用不饱和单环氧化物的聚合物,例如甲基丙烯酸缩水甘油酯或烯丙基缩水甘油醚的聚合物。
根据本发明,优选将以下聚环氧化合物或其混合物用作组份(c):
多元酚的聚缩水甘油醚,特别是双酚A的聚缩水甘油醚(GY250,Huntsman;/>0162,Bakelite AG;/>Resin 162,Hexion SpecialtyChemicals GmbH;Eurepox 710,Brenntag GmbH;/>GY250,Hunstman,D.E.R.TM332,The Dow Chemical Company;/>A 18-00,LEUNA-Harze GmbH)或者双酚F的聚缩水甘油醚(4,4'-二羟基-二苯基-甲烷,/>GY281,Huntsman;/>F 16-01,LEUNA-Harze GmbH;/>F 17-00,LEUNA-Harze GmbH),基于芳香胺的聚环氧化合物,特别是双(N-环氧丙基)苯胺,N,N'-二甲基-N,N'-二环氧丙基-4,4'-二氨基二苯甲烷和N,N-二环氧丙基-4-氨基苯基缩水甘油醚;脂环族二羧酸的聚缩水甘油酯,特别是六氢邻苯二甲酸二缩水甘油酯,以及n摩尔六氢邻苯二甲酸酐与1摩尔具有n个羟基(n=2-6的整数)的多元醇的反应产物的聚环氧化物,特别是3摩尔六氢邻苯二甲酸酐与一摩尔1,1,1-三羟甲基丙烷的反应产物的聚环氧化物;3,4-环氧环己基甲烷-3,4-环氧环己烷羧酸酯。
特别优选采用双酚A和双酚F的聚缩水甘油醚以及酚醛清漆的聚缩水甘油醚,或者由这些化合物中的两个或两个以上构成的混合物,尤其是双酚F的聚缩水甘油醚。
在特殊的情形下,液态聚环氧化物或者低粘度的二环氧化物,如双-(N-环氧丙基)-苯胺或乙烯基环己烷二环氧化物会使已呈液态的聚环氧化物的粘度进一步下降,或者将固态聚环氧化物转化成液态混合物。
使用一定量的组份(c),使得异氰酸酯基与环氧基的当量比为1.2:1至500:1,优选3:1至65:1,特别是3:1至30:1,特别优选为3:1至15:1。根据本发明,相对于所述具有至少两个环氧基的化合物(c)与所述具有至少两个针对异氰酸酯有反应活性的氢的化合物(b)的总重量而言,所述具有至少两个环氧基的化合物(c)的重量比例优选为35wt%至80wt%,特别优选为40wt%至70wt%,并且特别是为45wt%至60wt%。
催化剂(d)大幅加快所述具有至少两个针对异氰酸酯有反应活性的氢的化合物(b)以及所述具有环氧基的化合物(b)与所述聚异氰酸酯的反应。
催化剂(d)优选具有至少一个可置入的(einbaubar)催化剂。可置入的催化剂(d1)具有至少一个,优选1至8个并且特别优选1至2个针对异氰酸酯有反应活性的基团,如初级胺基、二级胺基、羟基或者脲基。其中,在本发明中,不将具有至少一个三级胺基的可置入的催化剂视作具有至少两个针对异氰酸酯有反应活性的氢的化合物(b),而是将其视作催化剂(d)。其中区分酰胺与胺基,在本发明的范围内,不将初级酰胺和二级酰胺称作初级胺基或二级胺基。优选地,所述可置入的胺催化剂优选具有初级胺基、二级胺基和/或羟基。根据本发明,除针对异氰酸酯有反应活性的基团以外,所述可置入的胺催化剂具有三级胺基。优选地,所述可置入的胺催化剂的三级胺基带有至少两个脂肪族烃残基,每个残基优选包含1至10个碳原子,每个残基特别优选包含1至6个碳原子。特别优选地,所述三级胺基带有两个残基,其相互独立地选自甲基残基、乙基残基以及另一有机残基。可使用的可置入的催化剂的示例例如为双二甲基氨基丙基脲,双(N,N-二甲基氨基乙氧基乙基)氨基甲酸酯,二甲基氨基丙基脲,N,N,N-三甲基-N-羟乙基双(氨基丙醚),N,N,N-三甲基-N-羟乙基双(氨基乙醚),二乙基乙醇胺,双(N,N-二甲基-3-氨基丙基)胺,二甲氨基丙胺,3-二-甲基氨基丙基-N,N-二甲基丙烷-1,3-二胺,二甲基-2-(2-氨基乙氧基乙醇)和(1,3-双(二甲基氨基)-丙烷-2-醇),N,N-双-(3-二甲基氨基-丙基)-N-异丙醇胺,双-(二甲基氨基丙基)-2-羟乙基-胺,N,N,N-三甲基-N-(3氨基丙基)-双(氨基-乙醚),3-二甲基氨基异丙基-二异丙醇胺,或者上述的混合物。
除了所述可置入的胺催化剂以外,可以使用其他常见的已知被用于聚氨酯制备的胺催化剂(d2)。其中例如包括脒,如2,3-二甲基-3,4,5,6-四氢嘧啶,三级胺,如三乙胺,三丁胺,三亚乙基二胺,二甲基环己胺,二甲基辛胺,N,N-二甲基苄胺,N-甲基-、N-乙基-、N-环己基吗啉,N,N,N',N'-四甲基亚乙基二胺,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-(N,N-二甲基氨基乙基)-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,以及优选1,4-二氮杂-双环-(2.2,2)-辛烷。此外,五甲基-二亚乙基三胺,N-甲基-N'-二甲基氨基乙基-哌嗪,N,N-二乙基乙醇胺以及硅吗啉,三氯化硼-叔胺加合物以及N-[3-(二甲基-氨基)丙基]甲酰胺例如也适用。
如果除了可置入的催化剂以外还使用其他催化剂,则这些催化剂优选含有三氯化硼-叔胺加合物、N,N-二甲基苄胺和/或硼-三氯(N,N-二甲基辛胺。
相对于组份(a)、(b)、(c)和(d)的总重量而言,用作催化剂或催化剂组合的催化剂(d)的浓度优选为0.001wt%至8wt%,特别优选为0.6wt%至6wt%,进一步优选为1.5wt%至5wt%,并且热别是为2.1至5wt%。其中,相对于催化剂(d)的总重量而言,具有针对异氰酸酯有反应活性的基团的催化剂的比例为至少5wt%,特别优选为至少8wt%,并且特别是为8至25wt%。
用于制备本发明的泡沫材料的化学和/或物理发泡剂(e)含有甲酸,视情况而定采用与其他发泡剂混合的形式。除了甲酸以及可能的水以外,可将氧化膦(Phospholinoxid)用作化学发泡剂。这些化学发泡剂与异氰酸酯基反应形成二氧化碳,就甲酸而言形成二氧化碳和一氧化碳。这些发泡剂通过与异氰酸酯基的化学反应释放气体,故被称作化学发泡剂。除此以外,也可使用物理发泡剂,如低沸点的烃。具有针对聚异氰酸酯a)的惰性并且在大气压力下的沸点低于100℃、优选低于50℃,进而能够在放热加聚反应的影响下蒸发的液体尤其适用。这类优选使用的液体的示例为烷烃,如庚烷,己烷,正戊烷和异戊烷,优选正戊烷和异戊烷的技术混合物,正丁烷和异丁烷和丙烷,环烷烃,如环戊烷和/或环己烷,烯,如呋喃,二甲醚和二乙醚,酮,如丙酮和甲基乙基酮,羧酸烷基酯,如甲酸甲酯、草酸二甲酯和乙酸乙酯,卤代烃,如二氯甲烷,二氯一氟甲烷,二氟甲烷,三氟甲烷,二氟乙烷,四氟乙烷,氯二氟乙烷,1,1-二氯-2,2,2-三氟乙烷,2,2-二氯-2-氟乙烷,五氟丙烷,七氟丙烷和六氟丁烯。也可以使用这些低沸点液体彼此的混合物,以及/或者与其他取代或未取代的烃的混合物。此外,有机羧酸,例如甲酸、乙酸、草酸、蓖麻油酸和含有羧基的化合物也适用。优选地,所述物理发泡剂可溶于组份(b)。
优选地,将小于2wt%、特别优选小于1wt%、进一步优选小于0.5wt%的卤化烃用作发泡剂(e),特别是不将卤化烃用作发泡剂。其中,这些重量比例均是相对于组份(a)至(f)的总重量而言。优选将水、甲酸-水混合物或者甲酸用作化学发泡剂,特别优选的化学发泡剂为甲酸-水混合物或者甲酸。优选将戊烷异构体或戊烷异构体的混合物用作物理发泡剂。
其中,所述化学发泡剂可以单独使用,即不添加物理发泡剂,或者可以与物理发泡剂一起使用。优选单独使用所述化学发泡剂。如果将化学发泡剂与物理发泡剂一起使用,则优选将纯水、甲酸-水混合物或者纯甲酸与戊烷异构体或戊烷异构体的混合物一起使用。在一个特别优选的实施方式中,甲酸是唯一的发泡剂。
可使用的助剂和添加剂(e)例如为填料,如石英粉、白垩、微晶白云岩、氧化铝、碳化硅、石墨或者刚玉;颜料,如二氧化钛、氧化铁或者诸如酞菁颜料的有机颜料;增塑剂,如邻苯二甲酸二辛酯、磷酸三丁酯或磷酸三苯酯;可置入的增容剂,如甲基丙烯酸、β-羟基丙酯、马来酸酯和富马酸酯;增强阻燃性的物质,如红磷或者氧化镁;可溶性染料,或者增强材料,如玻璃纤维或者玻璃织物。同样适用的是碳纤维或碳纤维织物,以及其他有机聚合物纤维,例如芳纶纤维或者LC聚合物纤维(LC=“Liquid Crystal(液晶)”)。还可将诸如铝、铜、铁和/或钢的金属填料用作填料。金属填料特别是以颗粒形式和/或粉末形式使用。
其他需要视情况一起使用的助剂和添加剂(e)为可聚合的烯属不饱和单体,其用量相对于组份a)、b)和c)的总重量而言为至多100wt%,优选为至多50wt%,特别是为至多30wt%。
可聚合的烯属不饱和单体添加剂的典型示例是那些不具有针对NCO基团有反应活性的氢原子的单体,如二异丁烯,苯乙烯,C1-C4-烷基苯乙烯,如α-甲基苯乙烯,α-丁基苯乙烯,氯乙烯,乙酸乙烯酯,诸如双-(4-马来酰亚胺基-苯基)-甲烷的马来酰亚胺衍生物,丙烯酸-C1-C8-烷基酯,如丙烯酸甲酯,丙烯酸丁酯或丙烯酸辛酯,对应的甲基丙烯酸酯,丙烯腈或者邻苯二甲酸二烯丙酯,以及包含针对NCO基团有反应活性的氢原子的烯属不饱和单体,例如甲基丙烯酸羟乙酯,甲基丙烯酸羟丙酯和甲基丙烯酸氨基乙酯。在本发明的范围内,不将包含针对NCO基团有反应活性的氢原子的烯属不饱和单体视作化合物(b)。
也可使用这类烯属不饱和单体的任意混合物。在使用烯属不饱和单体的前提下,优选使用苯乙烯和/或(甲基)-丙烯酸-C1-C4-烷基酯。在使用烯属不饱和单体的情况下,可使用传统的聚合引发剂,如过氧化苯甲酰,但一般情况下并不需要。
此外,助剂和添加剂e)还可包含已知的聚醚硅氧烷类型的泡沫材料稳定剂,脱模剂,例如聚酰胺蜡和/或硬脂酸衍生物和/或天然蜡,如巴西棕榈蜡。
助剂和添加剂e)既可以在实施本发明的方法前便加入起始材料a)和b)中,也可以之后再混入。
为了实施本发明的方法,可以将起始材料a)、b)和c)相互混合。视情况将其他助剂和添加剂e)、催化剂c)和发泡剂(d)加入反应混合物,对整体进行充分混合,并且将具备发泡能力的混合物注入开放或者闭合的模具。作为替代方案,可以采用双组分方法,其中将含有聚异氰酸酯(a)的异氰酸酯组份(B)与含有化合物(b)和(c)的有对异氰酸酯的反应性的组份(A)相互混合。将其他组分(d)至(f)添加至这两个组份中的一者中,优选添加至该有对异氰酸酯的反应性的组份(A)中。
在使用聚氨酯加工中已知的多组分混合头的情况下,所述方法具有灵活性高的特征。通过改变组份(a)、(b)和(c)的混合比,能够以相同的起始材料实现不同的泡沫材料品质。此外,不同的组份a)和不同的组份b)也可以不同的比例直接移入混合头。助剂和添加剂e)、催化剂c)和发泡剂d)可单独地或成批地移入混合头。也可将助剂和添加剂e)与催化剂c)一起投加,并且单独投加发泡剂d)。通过改变发泡剂的量,能够制造出具有不同表观密度范围的泡沫。
优选地,以单步骤将所述组份混合(所谓的“one-shot”方法)。特别优选地,以无预三聚步骤的方式实施所述反应。所述制备方法可连续地或不连续地进行。
优选地,所述组份(a)的化合物的异氰酸酯基与所述组份(b)的针对异氰酸酯有反应活性的基团的比例大于1.8:1,特别优选为1.8至4.0比1,进一步优选为2.0至3.0比1,并且特别是为2.0至2.5比1。
视使用的组份而定,发泡操作一般在2s至4min的晾置时间(Liegezeit)后开始,并且通常在2min至8min后结束。泡沫是均匀的并且呈细孔状。
本发明的异氰酸酯-环氧树脂混合泡沫材料的密度优选为15g/L至60g/L、特别优选为20至40,并且特别是为25至35。
优选在15℃至90℃的温度下,特别优选在20℃至60℃的温度下,并且特别是在20℃至45℃的温度下将起始组份混合。可通过高压或低压配料机将反应混合物注入闭合的支撑模具(Stützwerkzeuge)。按照此工艺制造例如不连续的夹层式元件。
无需对本发明的泡沫材料进行后续温度处理。在一个优选实施方式中,不对所述泡沫材料进行退火。
在使用闭合模具来制备本发明的泡沫材料(模具发泡)的情况下,为了实现最优的属性,优选对模具进行过填充。过填充是指填入一定量的具备发泡能力的混合物,使得其在开放模具中在完全发泡后将会占据比模具内容积更大的体积。
优选地,在连续工作的双带式设备上制造本发明的硬质泡沫材料。在采用双带工艺的情况下,优选通过高压机械投加多元醇组份和异氰酸酯组份,并在混合头中将其混合。预先通过独立的泵将催化剂和/或发泡剂投加至所述多元醇混合物中。将反应混合物连续地施覆至下部覆盖层上。包含反应混合物的下部覆盖层与上部覆盖层进入双带式设备,反应混合物在该双带式设备中发泡和固化。在离开双带式设备后,将连续式带状物裁切至期望的尺寸。这样便能制造出包含金属覆盖层的夹层式元件,或者具有柔性覆盖层的绝缘元件。
本发明的泡沫材料具有低导热性和极佳的机械属性,如高抗压强度、高压缩弹性模量和低脆性。此外,本发明的泡沫材料具有阻燃性,并且在燃烧时仅产生少量的热和烟雾。所述泡沫材料的介电损耗低,防潮性、耐磨性以及模具中的可加工性优越。因此,本发明的泡沫塑料非常适合充当针对空腔的填充泡沫,充当用于电绝缘的填充泡沫,充当夹层式构造的芯部,用于制造针对各种内部和外部应用的构造材料,用于制造针对车辆、船舶、飞机和火箭制造的构造材料,用于制造飞机内部和外部构件,用于制造各种类型的绝缘材料,用于制造绝缘板、管道和容器绝缘物,用于制造吸音材料,应用在发动机舱中,用于制造砂轮,以及用于制造高温绝缘物和阻燃绝缘物。特别优选用作夹层式元件的芯部泡沫材料,其中,借此获得的夹层式元件的缩孔数目极小,并且在泡沫层与覆盖层之间的附着性优越。本发明的另一标的为一种夹层式元件,包含本发明的异氰酸酯-环氧树脂混合泡沫材料。
下面结合实例对本发明进行阐释:
实施例
为了制备实验室泡沫,根据表1(以重量份数计),在异氰酸酯指数给定的情况下,按照以下顺序添加A组份的原料。将环氧树脂、多元醇以及水混合。随后添加催化剂混合物并搅拌。最后将化学发泡剂以及物理发泡剂添加至组份。
使用实验室搅拌器(Vollrath搅拌器),以1850rpm的搅拌速度和3秒的搅拌时间,将A组份与给定量的异氰酸酯组份在烧杯中充分混合,并且在此烧杯中发泡。在这个所谓的烧杯试验中,测定起始时间、固化时间和上升时间、表观密度,以及视情况而定测定脆性。为了测定其他属性,制造重量为150g的2.5L桶。
为了制备泡沫材料,使用以下原料:
聚酯醇1:聚酯基于对苯二甲酸,二乙二醇,油酸,和基于甘油和环氧乙烷的Polytherol,OH值为242mg KOH/g
聚酯醇2:聚酯基于己二酸,间苯二甲酸,1,4-丁二醇和单乙二醇,OH值为55mgKOH/g。
聚醚醇:基于环氧乙烷和环氧丙烷的乙二胺起始的聚醚多元醇,OH值为60mg KOH/g。
TEP:磷酸三乙酯
TCPP:三(2-氯异丙基)磷酸酯
环氧化物1:Leuna,A 18-00,基于双酚A的低分子环氧树脂,LEUNA-HarzeGmbH(洛伊纳/德国)的市售产品,依据DIN 16945的环氧当量为178g/eq-185g/eq,依据DIN53015的在25℃下的粘度为8000mPas至10000mPas。
稳定剂:硅氧烷稳定剂B 8498,聚醚聚硅氧烷,Evonik(德国埃森)的市售产品。
甲酸:85wt%甲酸水溶液
催化剂:由二乙基甲苯二胺、N,N,N'-三甲基-氨基乙基乙醇胺、三亚乙基二胺与双(2-二甲基氨基乙基)甲胺构成的催化剂混合物
添加剂1:由水、二丙二醇与甘油构成的混合物,OH值为425mg/KOHg
异氰酸酯:聚合亚甲基二苯基二异氰酸酯(PMDI),25℃下的粘度约为500mPa*s。
在小量试验(烧杯试验)中测定表观密度:
在烧杯试验中,通过分离杯缘上方的泡沫,随后对连同剩余泡沫在内的烧杯进行称重,测定泡沫的表观密度。此质量减去空烧杯的质量(在发泡前测得)后除以烧杯容积(0.735L),便得到表观密度。
机器试样:
按照双带工艺制造100mm厚的夹层式元件。借助催化剂混合物将液体表观密度调节至33±1g/L。
在机器泡沫材料上实施以下测量:
测定硬质泡沫的脆性:
依据ASTM C421(08)2014测定实验室泡沫的脆性。为此,首先将二十四个经室内干燥的检定立方体(19mm)置入用橡木制成的立方体盒子(190×197×197mm)中。使用细齿锯将泡沫切割成十二个小立方体(2.5mm)。用精密天平对这些试样体进行称重(M1),并将其与检定立方体置入试验装置。盒子刚性地安装在中心处,使得可旋转轴体的轴线垂直于盒子的面。盒子以每分钟60±2转的速度进行600±3次旋转。在定义的试验阶段后,将十二个泡沫块小心地从盒子取出。为试样清除掉灰尘和颗粒残余,随后重新为试样称重(M2)。按照以下方程计算出质量损失:
质量损失(%)=[(M1-M2)/M1]*100
M1=原始质量M2=最终质量
抗拉强度
依据DIN EN ISO 14509-1/EN 1607进行抗拉强度试验
导热性:
在发泡后,在标准气候下将泡沫立方体存放24小时。随后从泡沫立方体的中心切割出试样体(即顶侧和底侧被移除),其尺寸为200×200×30mm。随后在10℃的平均温度下使用热流测量板设备Hesto A50测定导热性。
测定抗压强度:
依据DIN 53421/DIN EN ISO 604测定抗压强度。
小型燃烧试验(Euro Class E):
依据EN-ISO 11925-2实施燃烧试验,数据对应火焰高度(单位:cm)。
从表1可以看出,在根据本发明将OH值为195mg KOH/g至400mg KOH/g且官能度为2至4的聚酯与OH值为40mg KOH/g至80mg KOH/g且官能度为2.6至6.5的聚醚组合的情况下,在密度相同且指数相似的情况下,获得的泡沫材料的抗拉强度有所改善且导热性有所减小。
实例2
根据在实例1中描述的发泡方法,以改变聚酯醇1的量的方式制备泡沫。为了测定脆性,按照上述方法制造密度为35±1g/L的2.5L桶。在表2中给出了起始物质的精确组成以及机械值和脆性测量的结果。
表2:
泡沫配方中的组份和物理特性参数。
表2中的实例显示,通过使用聚酯醇和聚醚醇能够显著降低脆性。在环氧化物的质量比例为11wt%的情况下,泡沫的质量损失最小且脆性最低。减少环氧化物组份使脆性降低,但同时也使抗压强度降低。在A组份中包含41份环氧化物和30份聚酯醇的情况下,理想地实现高抗压强度和有所减小的脆性。
Claims (14)
1.一种制备密度为15g/L至60g/L的异氰酸酯-环氧树脂混合泡沫材料的方法,其中将
a)聚异氰酸酯与
b)至少两个具有至少两个针对异氰酸酯有反应活性的氢的化合物,
c)至少一个具有至少两个环氧基并且环氧当量为90g/eq至500g/eq的化合物,
d)至少一个加快所述具有至少两个针对异氰酸酯有反应活性的氢的化合物(b)和所述具有环氧基的化合物(c)与所述聚异氰酸酯(a)的反应的催化剂
e)含有甲酸的化学和/或物理发泡剂,以及
f)视情况采用的助剂和添加剂
混合成反应混合物,其中,所述聚异氰酸酯(a)中的异氰酸酯基与所述具有至少两个环氧基的化合物(c)中的环氧基的当量比为1.2:1至500:1,并且,将所述反应混合物反应成所述异氰酸酯-环氧树脂混合泡沫材料,其特征在于,所述具有至少两个针对异氰酸酯有反应活性的氢原子的化合物(b)具有至少一个羟基值为195KOH/g至400mg KOH/g且平均标称官能度为2至4的聚酯醇(b1),并且具有至少一个羟基值为40mg KOH/g至80mg KOH/g且平均标称官能度为2.6至6.5的聚醚多元醇(b2)。
2.根据权利要求1所述的方法,其特征在于,所述聚酯多元醇(b1)可通过将至少二官能的酸组份与至少二官能的醇组份缩合来制备,以及,所述酸组份包括至少二官能的芳香酸或者芳香族二羧酸的衍生物。
3.根据权利要求2所述的方法,其特征在于,相对于所述酸组份和所述醇组份的总重量而言,所述至少二官能的芳香酸的比例为至少20wt%。
4.根据权利要求1至3中任一项所述的方法,其特征在于,所述聚醚醇(b2)包括至少一个胺起始的聚醚多元醇。
5.根据权利要求1至4中任一项所述的方法,其特征在于,所述聚酯醇(b1)在聚酯醇(b1)与聚醚醇(b2)的总重量中所占的重量比例为40wt%至80wt%。
6.根据权利要求1至5中任一项所述的方法,其特征在于,相对于所述具有至少两个环氧基的化合物(c)与所述具有至少两个针对异氰酸酯有反应活性的氢的化合物(b)的总重量而言,所述具有至少两个环氧基的化合物(c)的重量比例为35wt%至80wt%。
7.根据权利要求1至6中任一项所述的方法,其特征在于,所述异氰酸酯a)具有由至少一个MDI低聚物与低分子MDI衍生物2,2‘-MDI、2,4‘-MDI或4,4‘-MDI中的至少一者构成的混合物。
8.根据权利要求7所述的方法,其特征在于,相对于所述组份(a)的总重量而言,低聚MDI的含量大于30wt%乃至小于80wt%。
9.根据权利要求1至8中任一项所述的方法,其特征在于,所述具有至少两个环氧基的化合物(c)选自由双酚A、双酚F或酚醛清漆的聚缩水甘油醚或其混合物构成的群组。
10.根据权利要求1至9中任一项所述的方法,其特征在于,所述加快异氰酸酯/环氧化物反应的催化剂(d)具有至少一个催化剂(d1),其具有至少一个针对异氰酸酯有反应活性的氢原子。
11.根据权利要求1至10中任一项所述的方法,其特征在于,所述组份(a)的化合物的异氰酸酯基与所述组份(b)的针对异氰酸酯有反应活性的基团的比例大于1.8:1。
12.根据权利要求1至11中任一项所述的方法,其特征在于,将所述反应混合物施覆至下部覆盖层上,并且按照双带工艺连续地制造复合式元件。
13.一种异氰酸酯-环氧树脂混合泡沫材料,可根据权利要求1至12中任一项所述获得。
14.一种夹层式元件,包含根据权利要求13所述的异氰酸酯-环氧树脂混合泡沫材料。
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EP21187200 | 2021-07-22 | ||
PCT/EP2022/069757 WO2023001686A1 (de) | 2021-07-22 | 2022-07-14 | Isocyanat-epoxy-hybridschaumstoffe mit geringer sprödigkeit und verbesserter haftung |
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KR (1) | KR20240036654A (zh) |
CN (1) | CN117677646A (zh) |
BR (1) | BR112024001164A2 (zh) |
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GB816923A (en) | 1954-12-06 | 1959-07-22 | Bayer Ag | Process for the production of basic n,n-diepoxides |
DE1011618B (de) | 1954-12-06 | 1957-07-04 | Bayer Ag | Verfahren zur Herstellung basischer Diepoxydharze |
US3242108A (en) | 1961-04-04 | 1966-03-22 | Union Carbide Corp | Compositions for producing polyurethane resins and resinous foams and products prepared therefrom |
DE1222076C2 (de) | 1962-02-03 | 1976-01-15 | Bayer Ag, 5090 Leverkusen | Verfahren zur herstellung von diepoxiden |
CH448513A (de) | 1963-11-14 | 1967-12-15 | Bayer Ag | Verfahren zur Herstellung von geformten Gebilden auf Basis von Epoxydharzen |
US3793236A (en) | 1971-02-12 | 1974-02-19 | Mitsubishi Chem Ind | Oxazolidone-modified isocyanurate resins |
US3849349A (en) | 1971-05-12 | 1974-11-19 | K Frisch | Polyisocyanurate foam and process for producing the same |
US4129695A (en) | 1974-11-20 | 1978-12-12 | Rhone-Poulenc Industries | Process for preparing foams from polyisocyanates and polyepoxides |
WO2004085509A1 (en) | 2003-03-24 | 2004-10-07 | Solvay (Société Anonyme) | Process for the manufacture of foams composed of polyurethane or of modified polyurethane |
RU2578713C9 (ru) | 2010-12-15 | 2016-11-20 | Байер Интеллектуэль Проперти Гмбх | Устойчивые к высоким температурам пеноматериалы |
CN103619927A (zh) | 2011-05-02 | 2014-03-05 | 拜耳知识产权有限责任公司 | 具有低导热性的耐高温泡沫材料 |
US20130324626A1 (en) | 2012-05-30 | 2013-12-05 | Basf Se | Producing rigid polyurethane foams |
EP3059270A1 (de) | 2015-02-20 | 2016-08-24 | Basf Se | Temperaturbeständige Schaumstoffe auf Isocyanatbasis mit hoher Flammwidrigkeit |
WO2016131878A1 (de) | 2015-02-20 | 2016-08-25 | Covestro Deutschland Ag | Hochtemperaturbeständige schaumstoffe |
EP3259295B1 (de) | 2015-02-20 | 2019-12-18 | Covestro Deutschland AG | Hochtemperaturbeständige schaumstoffe mit hoher flammwidrigkeit |
KR102224864B1 (ko) | 2018-10-05 | 2021-03-08 | 한국조선해양 주식회사 | 발포 조성물과 이의 발포체를 포함하는 단열재, 액화가스 저장탱크 및 선박 |
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