CN1217347A - 基于异氰酸酯的开孔硬质泡沫体 - Google Patents
基于异氰酸酯的开孔硬质泡沫体 Download PDFInfo
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- CN1217347A CN1217347A CN98120638A CN98120638A CN1217347A CN 1217347 A CN1217347 A CN 1217347A CN 98120638 A CN98120638 A CN 98120638A CN 98120638 A CN98120638 A CN 98120638A CN 1217347 A CN1217347 A CN 1217347A
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- compound
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- hydrogen atom
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- acid
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- 239000012948 isocyanate Substances 0.000 title claims abstract description 20
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- 238000000034 method Methods 0.000 claims abstract description 28
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- 239000005056 polyisocyanate Substances 0.000 claims abstract description 23
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000654 additive Substances 0.000 claims abstract description 4
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Abstract
一种制备开孔硬质泡沫体的方法,通过反应下面组分:a)多异氰酸酯,与b)含有与异氰酸酯反应的氢原子的化合物,反应在以下组分存在下进行c)水,d)如果需要,作为物理发泡剂的有机化合物,e)催化剂,助剂和/或添加剂,其中所用的含有活泼氢原子的化合物含有具有下列结构的物质,式中各基团定义详见说明书。
Description
本发明涉及基于异氰酸酯的开孔硬质泡沫体,其特别适用于真空绝热设备中的芯材。本发明也提供用于生产此类硬质泡沫体的助剂及由这些开孔的硬质聚氨酯泡沫体制备的真空绝热设备。
作为绝热材料的基于异氰酸酯的硬质泡沫体的生产已公知许久,最重要的化学起始物质为多官能团异氰酸酯。由这些多异氰酸酯形成的化学结构可包括聚氨酯,聚脲,聚异氰酸酯,也包括其它异氰酸酯加成物如脲基甲酸酯,缩二脲,碳化二亚胺,噁唑烷酮,聚酰亚胺,聚酰胺等。这些结构类型由与异氰酸酯反应的物质,催化和反应条件控制。由多异氰酸酯与多醇反应得到的基于异氰酸酯的硬质泡沫体在工业上最为重要。这些硬质聚氨酯泡沫体的生产描述在如《塑料手册(Kunststoff-Handbuch)》,第Ⅶ卷,“聚氨酯”,第3版,由G.Oertel,编辑,Carl-Hanser-Verlag,Munich,Vienna,1993。
基于异氰酸酯的常规硬质泡沫体大部分具有闭孔,其中存在着低热传导性的泡孔气体。以前,通常称为R11的氯氟烃(CFCs)如三氯氟甲烷被用于此目的。对于氯氟烃,本文将通常使用R11。
然而,这些CFCs具有高的臭氧消耗能力(ODP)和高的温室效应(GWP)。为此,近年来CFCs已被ODP为零和非常低GWP的产物代替。在反应后作为泡孔气体保留在泡沫体中并具有ODP为0和GWP几乎为0的发泡剂中,烃是最重要的。然而,这些物质导致泡沫体的热传导性增加。
现有技术已有一系列减少热传导性的可能方法。
WO95/15356描述了一种制备硬质聚氨酯泡沫体的方法,该泡沫体具有封闭,非常小泡孔及含有IR吸收剂、特别是炭黑以减少热传导性。将这种固体作为IR吸收剂的缺陷,特别是,如它们通过沉降或阻塞过滤机,妨碍将多醇组分和异氰酸酯组分加工成聚氨酯。
GB-A-2286134公开了具有IR吸收中间层的硬质聚氨酯泡沫体。然而,这些层的***需要附加的步骤,该方法不能通过用聚氨酯常规、简单填充中空空间来提供绝热性。
克服这些缺陷的另一方法是抽空泡沫体的泡孔,以消除发泡气体。这种方法描述在R.De Vos,D.Dosbotham和J.Dechaght,1994,SPI“聚氨酯世界研讨会(Polyurethanes World Congress),Boston;W.Wacher,A.Christfreund,D.Randall,N.W.Keane,1996,SPI,“Polyurethanes EXPO’96,“,Las Vegas。这种与精细微孔结构结合的真空强绝热作用通常是公知的,其已在理论上被***地解释,如VDI-Warmeatlas,第6版,1991,KF1-KF19“superisolationen”。这种理论指明,该结构必需尽可能为精细微孔以减少真空的需要。
WO95/00580公开了微孔开孔的聚氨酯,其被用作真空绝热部件的芯。其中描述的材料由溶液或通过NCO封端的预聚物在水中的絮凝而制备。与常规的发泡相比,这种制备方法通常在技术上更复杂。
DE-A-4439328描述了具有聚氨酯短纤维芯的真空面板,该面板与一种粘合剂压制在一起。其缺陷是成型费用的增加和通常超过100kg/m3的高密度。
US-A-5478867描述了含作为芯的聚脲干凝胶的真空面板的制备方法。然而,这些干凝胶的制备是非常费时费钱的。
EP-A-662494描述了用于真空面板的开孔、硬质聚氨酯泡沫体,其中泡沫体包括能与作为泡孔扩张剂的异氰酸酯反应的脲化合物。然而,这些脲衍生物仅有限地影响泡孔的扩张,因此这些泡沫体对真空面板仅是有限的适用。
EP-A-188806描述了用于真空面板的硬质聚氨酯泡沫体,该泡沫体的制备是使用二价金属的粉状羧酸盐。然而,在液体聚氨酯成形组分中使用这些固体,在加工中将导致上述问题。
US-A-4444821描述了包括作为芯的玻璃纤维的真空面板。EP-A-434225和US-A-4726974描述了具有硅石填料的真空面板。这些方法也不能带来通过使用聚氨酯的优点。
本发明的一个目的是提供基于异氰酸酯的开孔、微孔的硬质泡沫体,其适用于真空面板的芯材。
我们已发现,该目的可通过多异氰酸酯与含活泼氢原子且具有结构Ⅰ的化合物进行反应来实现
其中
m=0-15
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r=0-1
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x=1-5
y=1-4或1-3的混合物,其中r+n≠0
z=0-3
zi=0.1-3
R1为多元醇去除OH后的残余脂族结构,所述多元醇优选乙二醇,二乙二醇,三乙二醇,1,2-丙二醇和二丙二醇,1,4-丁二醇,1,6-己二醇,新戊二醇,1,3-丁二醇,三羟甲基丙烷,三羟甲基乙烷,丙三醇,季戊四醇,这些物质在酯化时也可混合使用,R1也可为相应结构的混合物,
R2为多元羧酸去除COOH后的残基,所述多元羧酸例如是己二酸,对苯二酸,邻苯二甲酸,
R3为如R1的醇残基。
相应地,本发明提供一种制备基于异氰酸酯的开孔硬质泡沫体的方法,该泡沫体适用于真空绝热设备的芯材,通过反应下列组分而得:
a)多异氰酸酯,与
b)含有可与异氰酸酯反应的氢原子的化合物,反应在以下组分存在下进行
c)水,
d)如果需要,作为物理发泡剂的有机化合物,
e)催化剂,助剂和/或添加剂,其中所用的含有活泼氢原子的化合物含有具有下列结构的物质:
其中
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x=1-5
y=1-4或1-3的混合物,其中r+n≠0
z=0-3
zi=0.1-3
R1为多元醇去除OH后的残余脂族结构,所述多元醇优选乙二醇,二乙二醇,三乙二醇,1,2-丙二醇和二丙二醇,1,4-丁二醇,1,6-己二醇,新戊二醇,1,3-丁二醇,三羟甲基丙烷,三羟甲基乙烷,丙三醇,季戊四醇,这些物质在酯化时也可混合使用,R1也可为相应结构的混合物,
R2为多元羧酸去除COOH后的残基,所述多元羧酸例如是己二酸,对苯二酸,邻苯二甲酸,
R3为如R1的醇残基。
本发明也提供通过该方法制备的基于异氰酸酯的开孔、微孔硬质泡沫体,及由其制备的真空面板。
本发明含活泼氢原子的结构式Ⅰ的化合物优选为脂肪酸与多官能团醇的含羟基酯化产物。在此可使用饱和或不饱和酸,其中优选使用不饱和化合物。基于与其它聚氨酯形成组分的良好的混溶性,优选使用蓖麻油酸和/或蓖麻油和/或浮油脂肪酸与多官能团醇的反应产物。所使用的多官能团醇,特别是那些具有2~6个碳原子,优选3~6个碳原子,更优选3~5个碳原子的。其例子为乙二醇,丙二醇,二乙二醇,二丙二醇,丙三醇,丁二醇。含活性氢的结构式Ⅰ化合物的羟值优选>160mgKOH/g。
本发明使用的含活泼氢原子化合物的用量,基于组分b)-e)的全部用量,具体为0.1-80wt%,优选5-50wt%,更优选10-20wt%。
对于其它形成组分,下面将进行详细说明:a)合适的有机多异氰酸酯为脂族、环脂族、芳脂族和优选的芳族多官能团异氰酸酯,它们都是已知的。
特别优选2,4-和2,6-甲苯二异氰酸酯和相应的异构体混合物,二苯基甲烷4,4′-、2,4′-和2,2′-二异氰酸酯和相应的异构体混合物,二苯基甲烷4,4′-和2,4′-二异氰酸酯、多苯基多亚甲基多异氰酸酯的混合物,二苯基甲烷4,4′-、2,4′-和2,2′-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。
也通常使用改性的多官能团异氰酸酯,如通过有机二异氰酸酯和/或多异氰酸酯的化学反应获得的产物。
可提及的例子为含酯、脲、缩二脲、脲基甲酸酯、碳化二亚胺、异氰脲酸酯、脲二酮和/或脲烷基团的多异氰酸酯。该改性的多异氰酸酯可互相混合使用或与其它非改性的多异氰酸酯混合使用。
现已发现,特别适用的有机多异氰酸酯为二苯基甲烷二异氰酸酯异构体混合物或具有二苯基甲烷二异氰酸酯异构体含量为33~55wt%的粗MDI。b)作为含至少两个对异氰酸酯活性的氢原子且可与本发明的结构式Ⅰ的含活性氢化合物一起使用的化合物,为分子上具有两个或更多选自OH基团、SH基团、NH基团、NH2基团和CH酸性基团如β二酮基团的反应基团的化合物。
优先使用那些具有官能度2~8、优选2~6,分子量300~8000、优选400~4000的化合物。已知可用的化合物为,如多醚多胺和/或优选的多醇,选自聚醚多醇,聚酯多醇,聚硫醚多醇,聚酯酰胺,含羟基聚缩醛和含羟基脂族聚碳酸酯或至少两种上述多醇的混合物。优选使用聚酯多醇和/或聚醚多醇。这些多羟基化合物的羟值通常为100~850,优选200~600。
适合的聚酯多醇可由具有2~12个碳原子的有机二羧酸、优选具有4~6个碳原子的脂族二羧酸与具有2~12个碳原子、优选2~6个碳原子的多元醇,优选二元醇制备。合适的二羧酸例子为: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,富马酸,邻苯二甲酸,间苯二甲酸和对苯二甲酸。这些二羧酸可单独或混合使用。也可使用相应的二羧酸衍生物来替代这些二羧酸,该衍生物如具有1~4个碳原子醇的二羧酸酯或二羧酸酐。二元和多元醇、特别是二醇的例子为: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,丙三醇和三羟甲基丙烷。
为制备聚酯多醇,有机如芳族及优选脂族多羧酸和/或衍生物和多元醇可在下面条件下进行缩聚:不存在催化剂或优选使用酯化催化剂,优选在惰性气体如氮气、一氧化碳、氦气、氩气等气氛中,在150~250℃、优选180~220℃的熔融温度下,在常压或减压下,缩聚进行至所需的酸值,该酸值有利地为小于10、优选小于2。
为制备聚酯多醇,有机多羧酸和/或衍生物与多元醇以摩尔比率1∶1~1.8、优选1∶1.05~1.2进行缩聚。
所获得的聚酯多醇优选具有官能度为2~4、优选2~3,分子量为300~3000、优选350~2000、更优选400~600。
然而,所使用的多醇特别优选聚醚多醇,其由公知方法如由一种或多种亚烷基上具有2~4个碳原子的烯化氧,使用碱金属氢氧化物如氢氧化钠或氢氧化钾或碱金属烷氧化物如甲醇钠、乙醇钠或钾或异丙醇钾作为催化剂,加入至少一种以键合形式含2~8、优选2~6可反应的氢原子的引发剂通过阴离子聚合制备,或使用路易斯酸如五氯化锑、醚合三氟化硼或漂白土作为催化剂通过阳离子聚合制备。
合适的烯化氧为四氢呋喃,1,3-环氧丙烷,1,2-或2,3-环氧丁烷,氧化苯乙烯和优选的环氧乙烷和1,2-环氧丙烷。这些烯化氧可单独、交替或混合使用。合适的引发剂的例子为水,有机二羧酸如琥珀酸、己二酸、邻苯二甲酸和对苯二甲酸,在烷基上具有1~4个碳原子的脂族和芳族、非烷基化、N-单烷基化,N,N-和N,N′-二烷基化二胺,例如非烷基化、单烷基化和二烷基化乙二胺、二亚乙基三胺、三亚乙基四胺、1,3-丙二胺、1,3-或1,4-丁二胺、1,2-、1,3-、1,4,1,5-和1,6-六亚甲基二胺。
其它合适的引发剂分子为:烷醇胺如乙醇胺、N-甲基乙醇胺和N-乙基乙醇胺、二烷醇胺如二乙醇胺,N-甲基二乙醇胺和N-乙基二乙醇胺,以及三烷醇胺如三乙醇胺,还有氨。优选使用多元,特别是二元、三元和/或更高元醇如乙二醇,1,2-和1,3-丙二醇,二乙二醇,二丙二醇,1,4-丁二醇,1,6-己二醇,丙三醇,三羟甲基丙烷,季戊四醇和蔗糖。
聚醚多醇,优选聚氧丙烯基多醇和聚氧丙烯基-聚氧乙烯基多醇优选具有官能度2~6、更优选2~4,分子量为300~8000、优选400~1500、特别优选420~1100,合适的聚氧四亚甲基二醇的分子量为高至约3500。
合适的聚醚多醇还可以是聚合物改性的聚醚多醇,优选接枝聚醚多醇,具体为基于苯乙烯和/或丙烯腈的那些,其制备是通过丙烯腈、苯乙烯或优选的丙烯腈与苯乙烯的混合物以重量比率90∶10~10∶90、优选70∶30~30∶70,在上述聚醚多醇存在下进行原位聚合,使用德国专利1111394,1222669(US3304273,3383351,3523093),1152536(GB1040452)和1152537(GB987618)方法,以及含有作为分散相通常为1~50wt%、优选2~25wt%例如含键合的叔氨基和/或蜜胺的聚脲、聚酰肼、聚氨酯的聚醚多醇分散液,它们例如描述在EP-B-011752(US4304708),US-A-4374209和DE-A-3231497中。
同聚酯多醇一样,聚醚多醇可单独或混合使用。它们也可与接枝聚醚多醇或聚酯多醇或与含羟基聚酯酰胺、聚缩醛、聚碳酸酯和/或聚醚多胺一起混合。
合适的含羟基聚缩醛例如为能由二醇如二乙二醇、三乙二醇、4,4′-二羟基乙氧基二苯基二甲基甲烷或己二醇和甲醛制备的化合物。合适的聚缩醛也可由环状缩醛通过聚合制备。
合适的含羟基聚碳酸酯为那些所公知的类型,例如可通过二醇如1,3-丙二醇、1,4-丁二醇和/或1,6-己二醇、二乙二醇、三乙二醇或四乙二醇与碳酸二芳基酯如碳酸二苯基酯或光气反应制备。
聚酯酰胺包括如主要是线性缩聚物,其由饱和和/或不饱和多元羧酸或其酐与多官能团饱和和/或不饱和氨基醇或多官能团醇与氨基醇和/或多胺的混合物制得。
合适的聚醚多胺可由上述的聚醚多醇通过公知的方法进行制备。可提及的例子为聚氧亚烷基多醇的氰烷基化,随后将形成的腈进行氢化(US3267050),或在氢气和催化剂存在下,使用胺或氨对聚氧亚烷基多醇进行部分或完全胺化(DE1215373)。
开孔的硬质聚氨酯泡沫体可使用或不使用扩链剂和/或交联剂进行制备。然而,加入扩链剂、交联剂或视需要的它们的混合物,对改善生成聚氨酯的机械性能如硬度是有益的。所使用的扩链剂和/或交联剂为分子量小于400、优选60~300的二醇和/或三醇。合适的扩链剂/交联剂为具有2~14、优选4~10个碳原子的脂族、环脂族和/或芳脂族二醇,如乙二醇,1,3-丙二醇,1,10-癸二醇,邻、间、对二羟基环己烷,二乙二醇,二丙二醇和优选的1,4-丁二醇,1,6-己二醇和双(2-羟乙基)氢醌,三醇如1,2,4-或1,3,5-三羟基环己烷,丙三醇和三羟甲基丙烷,以及低分子量含羟基的基于环氧乙烷和/或1,2-环氧丙烷的聚烯化氧,作为引发剂的上述二醇和/或三醇。
如果扩链剂、交联剂或其混合物被用来生产基于异氰酸酯的硬质泡沫体,它们有益的用量基于多醇组分(b)的重量为至多20wt%,优选2~8wt%。c)对于发泡剂,优选使用通过与异氰酸酯基团反应消除二氧化碳的水。水的具体含量基于所有氢活性化合物的总量,为0.1~4wt%,优选0.3~3wt%,更优选为0.5~2wt%。过高水含量可导致泡沫体的脆性和热传导性的增加。
除水之外,还可使用物理发泡剂d)。具体地说,使用低沸点烃,低级单官能团醇,缩醛或部分卤化烃如HCFCs。优选为至多12个碳原子的低沸环状和无环饱和烃,它们可单独或混合使用,特别是戊烷,可使用戊烷异构体的混合物或纯异构体。该烃的用量,基于全部氢活性化合物的重量,为1~30重量份,优选16~22重量份,更优选6~12重量份。
而且,使用全氟化合物作为共发泡剂是有益的。具体地使用全氟链烷烃,优选全氟正戊烷,全氟正己烷,全氟正庚烷,全氟正辛烷。该全氟化合物可单独或混合使用。它们的用量,基于组分b)~e)的总和,为0.1~6重量份。
因为全氟化合物不溶于多醇组分中,因此它们通常在该组分中进行乳化。乳化剂优选使用(甲基)丙烯酸酯,特别是那些具有含氟侧链的如氟化烷基酯。e)本发明用于制备泡沫体所使用的催化剂,具体地说是那些加速含活泼氢原子的组分(b)与多异氰酸酯(a)反应的化合物。为此,优选叔胺,锑和铋化合物,碱金属和碱土金属羧酸盐,季铵盐,s-羟基三嗪和三(二烷基氨基甲基)苯酚。
特别优选下面分子式的三级氨基醇
R1R2NR3OH,
其中R1和R2为具有1-15个碳原子的脂族或环脂族基团,或R1和R2一起形成一个环上具有3-15个碳原子和氮原子的单环脂族环,R3为具有1-15个碳原子的脂族链。
R1,R2和R3的碳链或环还可含有杂原子如硫或特别是氧原子。
优选地,R1和R2与氮原子一起形成哌啶,吡咯烷,咪唑或吗啉结构,吡咯烷/哌啶类型或双环化合物的生物碱,如氮杂降冰片烷。
可提及的例子为Air Products销售的化合物为在泡沫体中形成异氰脲酸酯结构,使用常规催化剂,例如金属羧酸盐如乙酸钾和其它物质,如描述在《塑料手册》,第Ⅶ卷,聚氨酯,第3版(1993),第108页。
所使用的催化剂的用量,基于100重量份的组分b),c),d)和e),优选为0.1-10重量份。
其它的助剂和添加剂为如表面活性物质,泡沫稳定剂,泡孔调节剂,阻燃剂,填料和水解抑制剂。
对于上述和其它的起始物质的更详细情况可参照专门文献,如H.J.Saunders和K.C.Frisch的专著《高聚物(High Polymers)》,第ⅩⅥ卷,聚氨酯第1和2部分,Interscience Publishers(1962和1964)或者《塑料手册》第Ⅶ卷,聚氨酯,Carl Hanser Verlag,Munich,Vienna,第1、2和3版(1966,1983和1993)。
为制备基于异氰酸酯的本发明硬质泡沫体,多异氰酸酯与含有可与异氰酸酯反应的氢原子的化合物,及视需要部分地与其本身进行反应。通常组分b)~e)在反应之前结合以形成多醇组分。
在最简单情况下,多醇组分可与多异氰酸酯通过搅拌进行混合。然而,通常在机器中发泡。在此,组分在混合头进行混合,然后导入到模具中。
本发明的泡沫体通常具有开孔率为50~100%。其密度优选为30~100kg/m3,特别优选50~65kg/m3。本发明的泡沫体优选用于填充其随后抽空的中空空间,如冷冻机的壁和/或门,存储容器,车辆结构,长距离加热管或夹层元件,特别用于真空绝热设备的芯材。
为此,将该泡沫体的芯材用薄膜封紧,形成密闭,然后抽空。所使用的薄膜优选为多层薄膜。
该薄膜通常通过熔接进行密封,同整个薄膜一样,熔接缝必需是不渗透的。
真空绝热元件中的压力通常为0.001~10mbar。为了束缚最后的残留的痕量气体,最好使用公知的真空吸气剂。
使用本发明的方法可制备具有开孔率高至100%的硬质聚氨酯泡沫体。由本发明制备的硬质泡沫体生产的真空保温元件具有良好的机械特性以及明显低于现有产品的热传导性。
本发明通过下面实施例进行阐述。实施例1~13所使用的形成组分:多醇1:
聚醚多醇,羟值470mg KOH/g,分子量470,官能度3.9,由乙二胺与环氧丙烷反应而得。多醇2:
聚醚多醇,羟值490mg KOH/g,分子量490,官能度4.3,由蔗糖,丙三醇和水的混合物与环氧丙烷反应而得。多醇3:
聚醚多醇,羟值555mg KOH/g,分子量1800,官能度3.0,由三羟甲基丙烷与环氧丙烷反应而得。多醇4:
聚酯醇,由丙三醇与蓖麻油而得,羟值500mg KOH/g。多醇5:
聚酯醇,由单乙二醇与浮油脂肪酸而得,羟值161mg KOH/g。多醇6:
聚酯醇,由三羟甲基丙烷与浮油脂肪酸而得,羟值293mg KOH/g。多醇7:
聚酯醇,由丙三醇与浮油脂肪酸而得,羟值310mg KOH/g。多醇8:
聚酯醇,由丙三醇与蓖麻油而得,羟值357mg KOH/g。多醇9:
聚酯醇,由己二酸/邻苯二甲酸酐/油酸/三羟甲基丙烷而得,羟值385mg KOH/g,分子量530。多醇10:
聚醚多醇,羟值35mg KOH/g,分子量3980,官能度2.5,由丙三醇与环氧乙烷和环氧丙烷反应而得。多醇11:
聚醚多醇,羟值400mg KOH/g,分子量420,官能度3.0,由丙三醇与环氧丙烷反应而得。Lupranat M 20A:
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,NCO含量为31.5wt%。Lupranat M50:
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,NCO含量为31.0wt%。Tegostab B8919:泡孔扩张剂(Goldschmidt)Ortegol 501:泡孔扩张剂(Goldschmidt)Tegostab B8863Z:泡沫稳定剂(Goldschmidt)Tegostab B8870:泡沫稳定剂(Goldschmidt)Tegostab B8461:泡沫稳定剂(Goldschmidt)Tegostab B8409:泡沫稳定剂(Goldschmidt)FC 430:氟化烷基酯(3M Deutschland GmbH)Dabco AN 20:催化剂(Air Products)Lupragen N 301:催化剂(BASF AG)Lupragen VP 9104:催化剂(BASF AG)UAX 6164:泡孔扩张剂(OSI)
在表1~4中指明的多醇和异氰酸酯组分进行混合,然后在尺寸400×700×90mm的开口模具中自由发泡。
从泡沫体块料上锯下尺寸190/190/20mm的样品,将其包裹在密闭的薄膜中,在抽真空至最终的压力为0.05mbar之后,通过熔接进行封闭。
使用”Hesto-Lambda-Control-A-50”仪器测定热传导性。
依据ASTM D 2856-87,方法B测定开孔率。
表1:
多醇组分 | 实施例1(C) | 实施例2 | 实施例3 |
多醇1 | 20 | 20 | 20 |
多醇2 | 30 | 20 | 40 |
多醇3 | 50 | 50 | 30 |
多醇4 | 10 | 10 | |
B8919 | 3 | 3 | 3 |
B8863Z | 1 | 1 | 1 |
FC 430 | 1 | 1 | |
Dabco AN 20 | 5 | 5 | 5 |
水 | 0.5 | 2.3 | 0.5 |
环戊烷 | 7 | 7 | |
全氟己烷 | 4 | 4 | |
多异氰酸酯组分 | |||
M 20 A | 144 | 145 | 147 |
密度(g/l) | 55.3 | 54.7 | 55.0 |
开孔率(%) | 83 | 100 | 100 |
TC(mW/mK)0.1mbar | 13 | 7.5 | 7.0 |
(C)=比较例
所指的量均为重量份
表2:
多醇组分 | 实施例4 | 实施例5 | 实施例6 | 实施例7 |
多醇1 | 15 | 15 | 15 | 10 |
多醇2 | 17.5 | 22.5 | 20 | 10 |
多醇3 | 41 | 36 | 40 | 43 |
多醇7 | 5 | 14 | ||
多醇5 | 5 | |||
多醇6 | ||||
B 8919 | 3 | 3 | 3 | 4.5 |
B 8863Z | 1 | 1 | 1 | 1.4 |
FC 430 | 1 | 1 | 1 | |
Dabco AN 20 | 5 | 5 | 5 | 2.8 |
水 | 0.5 | 0.5 | 0.5 | 2.2 |
环戊烷 | 7 | 7 | 7 | |
全氟己烷 | 4 | 4 | 4 | |
多异氰酸酯组分 | ||||
M 20 A | 117 | 116 | 149 | 180 |
密度(g/l) | 55 | 52 | 53 | 55 |
开孔率(%) | 95 | 71 | 73 | 96 |
TC(mW/m*K)0.1mbar | 7.5 | 14 | 13 | 6.9 |
表3:
多醇组分 | 实施例8 | 实施例9 | 实施例10 | 实施例11 |
多醇1 | 10 | 10 | 10 | 10 |
多醇2 | 10 | 10 | 10 | 10 |
多醇3 | 43 | 43 | 43 | 43 |
多醇8 | 12 | 12 | 12 | 12 |
多醇11 | 20 | 20 | 20 | 20 |
Ortegol 501 | 3.6 | 3.6 | ||
B 8919 | 3.6 | 3.6 | ||
B 8870 | 1 | 0.8 | 1.4 | |
B 8863Z | 1.4 | |||
Dabco AN 20 | 3 | 3 | 3 | 3 |
水 | 2.5 | 2.3 | 2.3 | 2.3 |
多异氰酸酯组分 | ||||
M 20 A | 190 | 190 | 190 | 190 |
密度(g/l) | 59 | 58 | 59 | 60 |
开孔率(%) | 96 | 96 | 95 | 96 |
TC(mW/m*K)0.1mbar | 7.8 | 7.5 | 8.1 | 7.3 |
表4:
多醇组分 | 实施例12 | 实施例13 |
多醇9 | 26 | 26 |
多醇10 | 32 | 32 |
二丙二醇 | 17 | 17 |
B 8461 | 1.3 | 1.3 |
B 8409 | 1.3 | 1.3 |
B 8919 | 2 | |
UAX 6164 | 2 | |
水 | 0.4 | 0.4 |
Lupragen VP9104 | 5.1 | 5.1 |
Lupragen N 301 | 0.3 | 0.3 |
环戊烷 | 18 | 18 |
多异氰酸酯组分 | ||
M 50 A | 320 | 320 |
密度(g/l) | 64 | 61 |
开孔率(%) | 95.6 | 92.4 |
TC(mW/m*K) | 6.9 | 8.1 |
Claims (14)
1.一种制备开孔硬质泡沫体的方法,通过反应下面组分进行:
a)多异氰酸酯,与
b)含有可与异氰酸酯反应的氢原子的化合物,反应在以下组分存在下进行
c)水,
d)如果需要,作为物理发泡剂的有机化合物,
e)催化剂,助剂和/或添加剂,
m=0-15
n=0-1
o=0-15
p=0-1
q=0-15
r=0-1
s=0-15
t=0-1
u=0-10
v=0-15
x=1-5
y=1-4或1-3的混合物,其中r+n≠0
z=0-3
zi=0.1-3
R1为多元醇去除OH后的残余脂族结构,所述多元醇优选乙二醇,二乙二醇,三乙二醇,1,2-丙二醇和二丙二醇,1,4-丁二醇,1,6-己二醇,新戊二醇,1,3-丁二醇,三羟甲基丙烷,三羟甲基乙烷,丙三醇,季戊四醇,这些物质在酯化时也可混合使用,R1也可为相应结构的混合物,
R2为多元羧酸去除COOH后的残基,所述多元羧酸例如是己二酸,对苯二甲酸,邻苯二甲酸,
R3为如R1的醇残基。
2.权利要求1的方法,其中,含活泼氢原子且具有结构Ⅰ的化合物为天然物与多元醇的酯化产物。
3.权利要求1的方法,其中,含活泼氢原子且具有结构Ⅰ的化合物占能与异氰酸酯反应的全部化合物b)的0.1~80wt%。
4.权利要求1的方法,其中,含活泼氢原子且具有结构Ⅰ的化合物占能与异氰酸酯反应的全部化合物b)的5~50wt%。
5.权利要求1的方法,其中,含活泼氢原子且具有结构Ⅰ的化合物占能与异氰酸酯反应的全部化合物b)的10~20wt%。
6.权利要求1的方法,其中,含有可与异氰酸酯反应的氢原子的化合物为结构Ⅰ化合物与官能度大于1.5且羟值为10~600mg KOH/g的多醇的混合物。
7.权利要求1的方法,其中,含有可与异氰酸酯反应的氢原子的化合物为结构Ⅰ化合物与一种反应产物的混合物,该反应产物由三羟甲基丙烷与烯化氧而得。
8.权利要求1的方法,其中,多异氰酸酯a)中至少10%的异氰酸酯基团进行反应,形成异氰脲酸酯基团。
9.权利要求1的方法,其中链烷烃用作物理发泡剂。
10.权利要求1的方法,其中全氟化合物用作物理发泡剂。
11.权利要求1的方法,其中全氟化合物的用量基于100重量份的组分b)~e)为0.1~6重量份。
12.权利要求1的方法,其中链烷烃与全氟化合物的混合物用作物理发泡剂。
13.一种可由权利要求1的方法制备的基于异氰酸酯的开孔硬质泡沫体。
14.权利要求13的泡沫体用作真空保温元件的芯材的用途。
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DE19742013A DE19742013A1 (de) | 1997-09-24 | 1997-09-24 | Offenzellige Hartschaumstoffe auf Isocyanatbasis |
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EP (1) | EP0905159A1 (zh) |
JP (1) | JPH11158244A (zh) |
KR (1) | KR19990030103A (zh) |
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- 1998-09-24 KR KR1019980039711A patent/KR19990030103A/ko not_active Application Discontinuation
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JPH11158244A (ja) | 1999-06-15 |
DE19742013A1 (de) | 1999-03-25 |
KR19990030103A (ko) | 1999-04-26 |
CA2245009A1 (en) | 1999-03-24 |
US5880168A (en) | 1999-03-09 |
CN1150239C (zh) | 2004-05-19 |
EP0905159A1 (de) | 1999-03-31 |
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