CN108350143A - 得自加聚-低聚酯的pur/pir硬质泡沫 - Google Patents

得自加聚-低聚酯的pur/pir硬质泡沫 Download PDF

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Publication number
CN108350143A
CN108350143A CN201680069002.3A CN201680069002A CN108350143A CN 108350143 A CN108350143 A CN 108350143A CN 201680069002 A CN201680069002 A CN 201680069002A CN 108350143 A CN108350143 A CN 108350143A
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CN
China
Prior art keywords
weight
pur
rigid foams
pir
component
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Pending
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CN201680069002.3A
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English (en)
Inventor
H.内夫茨格
T.哈根
K.洛伦茨
R.阿贝尔斯
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Covestro Deutschland AG
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Bayer MaterialScience AG
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Publication of CN108350143A publication Critical patent/CN108350143A/zh
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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
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4244—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups
    • C08G18/4261—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups prepared by oxyalkylation of polyesterpolyols
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Abstract

本发明的主题是制备PUR/PIR‑硬质泡沫的方法，其包括至少一种聚酯多元醇(a)与下述物质的反应：(b)至少一种含多异氰酸酯的组分，(c)至少一种发泡剂，(d)至少一种催化剂，(e)任选地至少一种阻燃剂和/或其他助剂和添加物，(f)任选地至少一种不同于聚酯多元醇(a)的具有至少两个异氰酸酯反应性基团的另外的化合物，所述聚酯多元醇(a)可通过下述反应得到：a.1.)至少一种环状羧酸酐；a.2.)至少一种分子量为62至450 Da的低分子量二醇；和a.3.)至少一种烯化氧；通过组分a.1.)和a.2.)的酯化，和随后借助于组分a.3.)将所产生的羧酸半酯烷氧基化；其中至少烷氧基化使用a.4.)至少一种胺催化剂来进行，在该胺催化剂中一个或多个氮原子是芳族环体系的一部分。本发明还涉及可根据本发明的方法获得的PUR/PIR‑硬质泡沫，以及包含根据本发明的PUR/PIR‑硬质泡沫和至少一个覆盖层的复合元件，所述覆盖层选自混凝土，木材，压板，铝，铜，钢，不锈钢，纸，无纺织物和塑料以及多层复合材料或其组合。本发明还涉及根据本发明的PUR/PIR‑硬质泡沫或根据本发明的复合元件用于隔热的用途。

Description

得自加聚-低聚酯的PUR/PIR硬质泡沫
聚氨酯-聚异氰脲酸酯(PUR/PIR)-硬质泡沫通常在发泡剂存在下通过多元醇组分与异氰酸酯组分的反应来制备。此外，还可添加添加剂，如泡沫稳定剂和阻燃剂。与其他硬质泡沫例如PUR硬质泡沫相比，PUR/PIR-硬质泡沫具有出色的热稳定性和改进的燃烧性能。这些改进的性能归因于异氰脲酸酯结构单元。
在现有技术中广泛使用短链聚酯多元醇作为这种PUR/PIR-硬质泡沫的多元醇组分。在这些短链聚酯多元醇的合成方面，原则上有两种可用的可能性：一方面，它们可以通过由低分子量多元醇，大都是二元醇，与低分子量多元羧酸，大都是二元羧酸，和/或与多元羧酸等价物，如酸酐或酯与一元醇的缩聚反应来制备。然而，另一方面还存在通过烯化氧与半酯的加聚反应来生产短链聚酯多元醇的可能性，所述半酯例如可以通过二醇在多元羧酸酐上的加成来获得。
加聚反应的变体固有地具有许多优点。可提及的例如是，相对于缩聚反应大大缩短的反应持续时间，由于甚至放热的反应进程而显著更小的能量引入和尤其也实际上定量的反应收率，因为例如没有解离出降低收率的反应水。
因此，过去不乏尝试考虑这种加聚反应来制备短链聚酯多元醇。
DE3621039A1描述了该方法并阐述了，通过环状二羧酸酐与多元醇和/或二链烷醇胺以1：0.5至1.5，优选1：0.7至1.2的摩尔比，在50至150℃，优选90至130℃的温度下反应生成相应的二羧酸半酯-和/或-半酰胺，随后在80至150℃，优选90至130℃的温度下，用氧化乙烯和/或氧化丙烯，使用1：0.8至1.7，优选1：1.0至1.6的酸基团与烯化氧的当量比，烷氧基化羧基得到具有羟基的低聚酯，其具有200-600 mg KOH/g的OH值，其特征在于，所述烷氧基化反应使用氨、低级的C2-C6脂族二胺和哌嗪的丙氧基化产物（其中所有的NH官能团均已丙氧基化）作为催化剂来进行。
关于所使用的催化剂，DE3621039进一步说明（第3页，第56行），N-甲基咪唑作为出色的酯交换催化剂产生具有（不希望的）宽摩尔质量分布的产物，这是应该避免的。
因此，虽然在非根据该发明的比较例（比较例2b，第7页，第10行）中描述了这种用N-甲基咪唑催化的多元醇的制备，但它不反应生成PUR/PIR泡沫，因为根据DE 36 21 039的教导，其是一种具有扩大的摩尔质量分布和相应增加的粘度的产物，即必须被归为明显不适合于此目的的。然而，在本专利申请的研究工作中发现，使用DE 36 21 039中有利的催化剂，只有非常困难才能获得优选的低聚酯-OH值范围为100-280mg KOH/g，相当于200-560g/mol当量摩尔质量，因为氨的丙氧基化产物、低级的C2-C6脂族二胺的丙氧基化产物和哌嗪的丙氧基化产物随着OH值的减少而迅速失去它们的催化活性。
DE3315381同样描述了一种生产聚酯多元醇或聚醚-聚酯多元醇的方法，其特征在于，使多元醇，优选羟值为15-250 mg KOH/g的聚醚多元醇，与至少一种羧酸酐，优选邻苯二甲酸酐，在N-甲基咪唑、三亚乙基二胺、三苯基膦或由这些化合物中的至少两种构成的混合物的存在下酯化成羧酸半酯，然后用至少一种烯化氧，优选氧化乙烯，在作为催化剂的N-甲基咪唑存在下将其烷氧基化。
然而，应该指出的是，在DE 33 15 381中公开的方法适合于烯化氧/羧基的摩尔比为最大1.5:1，优选1:1（第8页，第27和28行）。然而，本发明的目的是如下拓宽现有技术，即提供这样的物质作为用于PUR/PIR-硬质泡沫的低聚酯组分，其二羧酸单元（Baustein）主要用二亚烷基二醇结构单元酯化，因此在中间产物的半酯结构上可加成多于1.5mol的烯化氧。DE 33 15 381中没有认识到用简单的咪唑催化或用咪唑衍生物催化也可用于将真正的二亚烷基二醇结构单元与半酯结构连接的可能性。此外，没有给出下述启示，即，这种聚酯多元醇或聚醚-聚酯多元醇可用作PUR/PIR-硬质泡沫中的多元醇组分。DE3315381仅以非常一般的方式提及了由这种产物制备聚氨酯（第3页，第4行），但没有提供相关的实施例，并且没有一般性地要求保护聚氨酯的制备或具体地要求保护PUR -PIR硬质泡沫的制备。
因此，本领域技术人员不能从DE 33 15 381和/或DE 36 21 039得出结论，可以使用一个或多个氮原子是芳族环体系的一部分的胺催化剂，例如在咪唑或咪唑衍生物的情况中，作为在制备本发明中所力求的具有低聚醚单元的酯结构的催化剂，特别是随后将它们用作PUR/PIR-硬质泡沫中的多元醇组分。
因此，本发明的目的在于，提供PUR/PIR-硬质泡沫，其多元醇组分可使用一个或多个氮原子是芳族环体系的一部分的胺催化剂，例如在咪唑或咪唑衍生物的情况中，由环状羧酸酐、低分子量二醇以及烯化氧得到，其中每摩尔羧酸酐使用优选多于1.5mol的烯化氧，由此可得到的低聚酯具有在100-280mg KOH/g范围的OH值。
另一目的在于，将上述聚酯组分加入到PUR/PIR-硬质泡沫中，从而获得具有有吸引力的性质的PUR-PIR硬质泡沫，其性能至少达到基于常规缩聚多元醇的类似PUR/PIR-硬质泡沫的水平。
在本发明意义上的PUR/PIR-硬质泡沫特别是这样的PUR/PIR泡沫，其根据DIN ENISO 845:2009-10的粗密度在15kg/m3至300kg/m3的范围，并且其根据DIN EN 826:2013的抗压强度在0.1MPa至5MPa的范围。
因此，本发明的主题是制备PUR/PIR-硬质泡沫的方法，该方法包括至少一种聚酯多元醇(a)与
(b) 至少一种含多异氰酸酯的组分，
(c) 至少一种发泡剂，
(d) 至少一种或多种催化剂，
(e) 任选地至少一种阻燃剂和/或其他助剂和添加物，
(f) 任选地至少一种不同于聚酯多元醇(a)的具有至少两个异氰酸酯反应性基团的另外的化合物的反应，
所述聚酯多元醇(a)可通过下述反应得到：
a.1.) 至少一种环状羧酸酐；
a.2.) 至少一种分子量为62至450 Da的低分子量二醇；和
a.3.) 至少一种烯化氧；
通过组分a.1.)和a.2.)的酯化，和随后借助于组分a.3.)将所产生的羧酸半酯烷氧基化）；
其中至少所述烷氧基化使用
a.4.) 至少一种胺催化剂来进行，在该胺催化剂中一个或多个氮原子是芳族环体系的一部分。
此外，可按照根据本发明的方法获得的PUR/PIR-硬质泡沫。
此外复合元件，其包含本发明的PUR/PIR-硬质泡沫和至少一个覆盖层，所述覆盖层选自：混凝土、木材、压板、铝、铜、钢、不锈钢、纸、无纺织物和塑料以及多层复合材料或者它们的组合。
本发明还涉及根据本发明的PUR/PIR-硬质泡沫或本发明的复合元件用于隔热的用途。
下文中记载的参数可以优选按照在标题“实施例”下列出的测量方法来确定。在本发明中，术语“多元醇”同样用于聚酯多元醇(a)。
作为羧酸酐a.1.)，原则上可以考虑环状的脂族和芳族二羧酸酐，例如马来酸酐、衣康酸酐、柠康酸酐、琥珀酸酐、戊二酸酐、邻苯二甲酸酐和四氢邻苯二甲酸酐。优选使用马来酸酐和/或邻苯二甲酸酐和/或戊二酸酐，非常特别优选邻苯二甲酸酐或者至少85重量％由邻苯二甲酸酐组成的羧酸酐的混合物。此外可以考虑至少85重量％由环状羧酸酐和至多15重量％由一种或多种二羧酸组成的混合物，所述二羧酸例如是琥珀酸、戊二酸、己二酸、癸二酸、邻苯二甲酸、对苯二甲酸和间苯二甲酸，它们任选地也可以通过发酵途径获得。
此外可以使用至少85％由环状羧酸酐和至多15重量％由一种或多种一元羧酸的酸酐（例如乙酸酐或苯甲酸酐）组成的混合物。
作为可用于环状酸酐的开环的低分子量二醇a.2.)，原则上可以考虑分子量在62-450Da范围的所有二醇， 例如乙二醇、1,3-丙二醇、1,2-丙二醇、二甘醇、三甘醇、四甘醇、二丙二醇、三丙二醇、1,4-丁二醇、2-甲基-1,3-丙二醇、1,5-戊二醇、新戊二醇、1,6-己二醇和3-甲基-1,5-戊二醇，它们可以单独地或作为混合物来使用。
作为本申请范围内的低分子量二醇还包括与更高官能的醇和/或一元醇的混合物，所述更高官能的醇选自甘油、1,1,1-三羟甲基丙烷、季戊四醇，和一元醇例如2-乙基-1-己醇、丁基二甘醇、甲醇、乙醇、1-丙醇、2-丙醇、正丁醇、2-丁醇、2-甲基-1-丙醇、十二烷醇或苯酚(衍生物)，只要其比例不超过20重量％，基于所有所使用的二醇、更高官能的醇或一元醇计。
然而，优选使用乙二醇、二甘醇、三甘醇和四甘醇，非常特别优选二甘醇。
羧酸酐a.1.)和低分子量二醇a.2.)以摩尔比1:0.3至1.5，优选1:0.4至1.2，特别优选1:0.5至0.8:1来反应，生成相应的二羧酸半酯，这里已证明适合的温度范围为50-150℃，优选90-130℃。
由羧酸酐a.1.)和低分子量二醇a.2.)制备二羧酸半酯可以催化或无催化地进行；优选不使用催化剂。
作为烯化氧a.3.)，其用于借助于低分子量二醇由环状酸酐开环产生的主要包含半酯结构的中间产物的烷氧基化，优选使用1,2-或2,3-氧化丁烯、氧化乙烯和氧化丙烯，更优选氧化乙烯或氧化丙烯或这两种环氧化物的混合物。
它们可以连续添加到反应混合物中。嵌段加入环氧化物或环氧化物混合物同样是可行的，例如通过首先仅加入氧化丙烯或由氧化丙烯和氧化乙烯构成的富氧化丙烯的混合物，然后仅加入氧化乙烯或由氧化丙烯和氧化乙烯构成的富氧化乙烯的混合物。
基于计量加入的环氧化物的质量计，氧化乙烯的比例优选为90-100重量％，基于烯化氧a.3.)的总重量计，其非常特别优选为95至100重量％。
所述烷氧基化使用例如1:1.6至1:3.0，优选1:1.7至1:2.5的酸基团与烯化氧的当量比，在80-150℃，优选90℃-140℃的温度下进行。
在本发明的方法中优选使用≥1.5mola.3.)/mola.1.)。(a)优选具有100-280 mgKOH/g的OH值。
作为用于催化烷氧基化反应的胺a.4.)，可以考虑这样的胺催化剂，在该胺催化剂中一个或多个氮原子是芳族环体系的一部分。
然而，特别优选的是选自咪唑及其衍生物的芳族胺，特别是N-甲基咪唑。
也可以在借助于低分子量二醇使环状羧酸酐开环之前，将所述胺催化剂加入到反应混合物中。然而，它也可以在进行开环之后，但在开始添加烯化氧之前才加入。
合适的催化剂浓度优选在300至7000ppm，更优选500至5000ppm，特别优选800至3000ppm的范围，在每种情况下基于(a)至(f)的总重量计。
合适的聚酯(a)优选具有200-600mg KOH/g范围的羟值，以及1.3-3.5，更优选1.6-2.2，非常特别优选1.8-2.1的官能度。
作为含多异氰酸酯的组分(b)，原则上可以考虑脂族、脂环族、芳脂族、杂环的和特别是芳族的二-和/或多异氰酸酯，如其由W.Siefken记载在Justus Liebigs Annalen derChemie，562，第75至136页中，例如式Q(NCO)n的那些，其中n = 2至4，其中n是数均值，并且Q表示具有2至18、优选6至12个C-原子的脂族烃残基，具有4至20、优选5至11个C-原子的脂环族烃残基，具有平均6至27、优选6至23个C-原子的芳族烃残基，或者具有8至15、优选8至13个C-原子的芳脂族烃残基，例如DE-A 28 32 253的第10至11页中记载的那些多异氰酸酯。特别优选工业上容易获得的多异氰酸酯，例如2,4-和/或2,6-甲苯二异氰酸酯以及这些异构体的任意混合物（“TDI”），二苯基甲烷二异氰酸酯（“MDI”；“4,4'-和/或2,4'-和/或2,2'-异构体），多苯基-多亚甲基-多异氰酸酯环，如其通过苯胺-甲醛缩合，然后光气化和任选蒸馏浓缩多环组分来制备，和“改性多异氰酸酯”，其例如具有碳二亚胺基团、氨基甲酸酯基团、脲基甲酸酯基团、异氰脲酸酯基团、脲基团和/或缩二脲基团；特别是衍生自2,4-和/或2,6-甲苯二异氰酸酯和优选衍生自4,4'-和/或2,4'-二苯基甲烷二异氰酸酯的那些改性多异氰酸酯。非常特别优选的是多亚苯基-多亚甲基-多异氰酸酯的多异氰酸酯（“聚合-MDI”）。
作为发泡剂(c)，在本发明范围内可以考虑物理和化学发泡剂。在此，将化学发泡剂理解为是指通过与异氰酸酯的反应形成气态化合物的那些化合物。相反，将物理发泡剂理解为是指在25℃下以液体或气体形式存在、使用并且不与异氰酸酯发生任何化学反应的那些化合物。
将物理发泡剂理解为是指溶解或乳化在聚氨酯生产的原料中并且在通常的反应条件下，优选在25℃以上蒸发的化合物。本发明的聚氨酯泡沫通常在生产过程中变热，从室温开始增加至最高约180℃。所述物理发泡剂例如是烃，例如环戊烷、异戊烷和正戊烷、丁烷和丙烷，卤代烃和其它化合物，例如全氟烷烃如全氟己烷，全氟烯烃如1,1,1,2,3,4,5,5,5-九氟-4-(三氟甲基)戊-2-烯、1,1,1,3,4,4,5,5,5-九氟-2-(三氟甲基)戊-2-烯或顺-1,1,1,4,4,4-六氟-2-丁烯，氟氯烯烃如反-1-氯-3,3,3-三氟丙烯，以及醚、酯、酮和/或缩醛。
化学发泡剂例如是水和羧酸，其通过与异氰酸酯的反应释放二氧化碳，形成脲和酰胺。
作为发泡剂组分(c)，优选使用烃和/或水和/或至少一种羧酸。更优选的烃是在25℃为气态的烃，最优选的是正戊烷、环戊烷、异戊烷和/或所述异构体的混合物。这些可以与水和/或羧酸组合使用。在替代实施方案中，(c)是水和/或至少一种羧酸。
发泡剂组分(c)优选以0.1至30重量％，优选0.5至20重量％，特别优选0.7至10重量％的量来使用，基于组分(a)至(f)的总重量计。
作为用于制备本发明PUR/PIR-硬质泡沫的催化剂(d)，可以使用例如已知的形成聚氨酯或聚异氰脲酸酯的催化剂，例如有机锡化合物，如二乙酸锡、二辛酸锡、二月桂酸二丁基锡和/或强碱性的胺如 2,2,2-二氮杂双环辛烷、三乙胺、三亚乙基二胺、五甲基二亚乙基三胺、N,N-二甲基环己胺或双(N,N-二甲基氨基乙基)醚、N,N-二甲基苄胺和N-甲基咪唑，以及用于催化PIR反应的催化剂，例如乙酸钾、乙酸钠、N-[(2-羟基-5-壬基苯基)甲基]-N-甲基氨基乙酸钠、2,4,6-三[(3-二甲基氨基)丙基]六氢三嗪、2-乙基己酸钾和脂族季铵盐，例如新戊酸四甲基铵，及其混合物。
催化剂(d)优选以0.05至3重量％，优选0.06至2重量％的量来使用，基于所有组分(a)至(f)的总重量计。
上述组分的反应任选在阻燃剂和/或其它助剂和添加物(e)的存在下进行。
作为阻燃剂通常可以使用由现有技术已知的阻燃剂。合适的阻燃剂例如是溴化的醚（例如Ixol® B251），溴化的醇如二溴新戊醇、三溴新戊醇和PHT-4-二醇，以及氯化的磷酸酯例如三-(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。除了已经提到的卤素取代的磷酸酯之外，也可以使用无机阻燃剂，如红磷、含红磷的制剂、氧化铝水合物、三氧化锑、多磷酸铵和硫酸钙，或氰脲酸衍生物，例如三聚氰胺，或由至少两种阻燃剂例如聚磷酸铵和三聚氰胺的混合物，以及任选的淀粉用于根据本发明制备的PUR/PIR-硬质泡沫的阻燃处理。作为另外的液体无卤阻燃剂可以使用乙基膦酸二乙酯（DEEP）、磷酸三乙酯（TEP）、二甲基丙基膦酸酯（DMPP）、二苯基枯基磷酸酯（DPK）等。
在本发明范围内，基于组分(a)至(f)的总重量计，阻燃剂优选以0至30重量％，特别优选0.3至20重量％，特别是0.5至15重量％的量来使用。
其他助剂和添加物优选是填料，泡孔调节剂，泡沫稳定剂，表面活性化合物和/或抗氧化、热或微生物降解或老化的稳定剂。作为泡沫稳定剂是指在泡沫形成时促进形成规则泡孔结构的物质。作为示例可列举以下稳定剂：含硅氧烷的泡沫稳定剂，如硅氧烷-氧化烯-混合聚合物和其它有机聚硅氧烷，此外下述物质的烷氧基化产物：脂肪醇，羰基合成醇，脂肪胺，烷基酚，二烷基酚，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，以及此外由甲醛和烷基酚、甲醛和二烷基酚、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构成的缩合产物的烷氧基化产物。关于上述提及的以及关于其它起始材料的进一步说明可以在技术文献中获悉，例如Kunststoffhandbuch卷VII,Polyurethane, Carl Hanser Verlag 慕尼黑, 维也纳, 1., 2.和3.版, 1966, 1983和1993。
可以任选使用的其它化合物是具有至少两个异氰酸酯反应性基团的化合物(f)，即具有至少两个异氰酸酯基团反应性氢原子，可以使用在下文中一般性地描述并且不同于化合物(a)的化合物。
作为具有至少两个异氰酸酯反应性基团的化合物特别可以使用在分子中带有两个或更多个选自OH基团、SH基团、NH基团、NH2基团和CH-酸性基团（例如β-二酮基团）的那些。尤其使用具有2至8个OH基团的化合物用于制备根据本发明方法可优选获得的PUR/PIR-硬质泡沫。优选使用不同于化合物(a)的聚醚多元醇和/或聚酯多元醇。对于制备PUR/PIR-硬质泡沫，所使用的聚醚多元醇和/或聚酯多元醇的羟值为优选25-850mg KOH/g，特别优选25-480mg KOH/g，摩尔质量为优选大于230克/mol。组分(f)优选包含根据已知方法，例如通过环氧化物的阴离子聚合或者通过环氧化物的阳离子聚合来制备的聚醚多元醇，所述阴离子聚合通过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，芳族胺例如N-甲基咪唑催化，加入至少一种键合包含2至8个反应性氢原子的起始分子，所述阳离子聚合通过路易斯酸如五氯化锑，氟化硼-醚合物等或漂白土催化，加入至少一种2至8个制备的起始剂分子。此外，聚醚多元醇的制备可以借助于双金属氰化物催化来进行，其中这里完全连续的方式也是可行的。
适用于此的烯化氧例如是1,2-和2,3-氧化丁烯，氧化乙烯，1,2-氧化丙烯和氧化苯乙烯。特别合适的烯化氧是在亚烷基残基中具有2至4个碳原子的那些，特别是氧化乙烯，和1,2-氧化丙烯或1,2-氧化丁烯。烯化氧可以单独地、相继嵌段地、交替嵌段地或作为混合物计量加入。作为起始剂分子可以考虑例如脂族多元醇以及脂族和/或芳族胺和多胺，例如1,3-丙二醇，1,2-丙二醇，乙二醇，二乙二醇，二丙二醇，1,2-丁二醇，1,3-丁二醇，1,4-丁二醇，己二醇，戊二醇，3-甲基-1,5-戊二醇，1,12-十二烷二醇，水，甘油，三羟甲基丙烷，三乙醇胺，季戊四醇，山梨糖醇，蔗糖，氢醌，邻苯二酚，间苯二酚，双酚F，双酚A，1,3,5-三羟基苯，得自甲醛和酚或三聚氰胺或尿素的含羟甲基的缩合物，以及曼尼希碱。也可以使用基于氢化淀粉水解产物的高官能度起始剂化合物。这些例如记载在EP-A 1 525 244中。含氨基的起始剂化合物的例子是氨，乙醇胺，二乙醇胺，异丙醇胺，二异丙醇胺，乙二胺，六亚甲基二胺，苯胺，甲苯胺的异构体，二氨基甲苯的异构体，二氨基二苯基甲烷的异构体，以及在苯胺与甲醛缩合成二氨基二苯基甲烷时产生的多环（höherkernig）产物。当然也可以使用各种起始剂化合物的混合物。
组分(f)还可以任选地包含聚酯多元醇、增链剂和/或交联剂。作为增链剂和/或交联剂尤其可以使用二官能或三官能的胺和醇，特别是摩尔质量小于400g/mol，优选60-300g/mol的二醇和/或三醇。
为制备PUR/PIR硬质泡沫，使多异氰酸酯(b)和组分(a)和任选的(f)以这样的量反应，以至于该制剂的异氰酸酯特征数> 100，通常为110-600，优选150-500，特别优选180至450。
在此，将异氰酸酯特征数理解为是指由实际使用的异氰酸酯基团的物质的量[mol]和为完全转化所有异氰酸酯反应性基团化学计量所需的异氰酸酯基团的物质的量[mol]的商乘以100。因为为转化1mol异氰酸酯反应性基团需要1mol异氰酸酯基团，因此适用：
特征数=（异氰酸酯基团的摩尔数/异氰酸酯反应性基团的摩尔数）×100。
借助于已知的方法，可以不连续地或连续地制备PUR/PIR-硬质泡沫。本领域技术人员尤其已知块状泡沫的制备（连续和不连续），其用于单组分体系（不连续）和绝缘模塑泡沫（不连续）中。这里描述的发明涉及所有的方法。优选的方法是用于生产包含PUR/PIR-硬质泡沫芯和一个或多个覆盖层的复合元件的连续双带法，其中可使用柔性和/或刚性材料作为覆盖层。覆盖层材料例如是混凝土，木材，压板，铝，铜，钢，不锈钢，纸，无纺织物，特别是矿物无纺织物，和塑料以及多层复合材料。优选的塑料是丙烯腈-丁二烯-苯乙烯共聚物，聚乙烯，聚苯乙烯，聚氯乙烯和聚丙烯。在此，覆盖层的种类原则上不受限制；可以是模制品，建筑业的结构元件，管道，房屋部件等。
本发明尤其涉及金属复合元件的制造。金属复合元件是由至少两个覆盖层和一个位于其间的芯层组成的夹心复合元件。特别地，金属泡沫复合元件至少由两个由金属制成的覆盖层和一个由聚氨酯/聚异氰脲酸酯（PUR/PIR）-硬质泡沫制成的芯层组成。这种金属泡沫复合元件是由现有技术充分已知的，并且也被称为金属复合元件。在芯层和覆盖层之间可以设置其他层。例如，覆盖层可以被涂覆，例如用漆。
这种金属复合元件的应用的例子是用于工业建筑物建造和冷库建造以及用于卡车车身建造、厅门或运输集装箱的平面的或具有线纹的（linierte）壁元件以及成型屋顶元件。
所述金属复合元件的制造可以连续或不连续地进行。例如由DE 1 609 668 A或DE1 247 612 A已知用于连续制造的设备。包含PUR-和优选PUR/PIR-硬质泡沫的根据本发明的PUR/PIR-硬质泡沫优选具有大于90％，特别优选大于95％的闭孔率，根据DIN EN ISO4590：2003通过压力变化（比重瓶）测定。
根据本发明的PUR/PIR-硬质泡沫优选具有25 g/m3 - 300 g/m3，特别优选28 g/m3- 50 g/m3的粗密度。
根据本发明的PUR/PIR-硬质泡沫特别用于隔热，例如制冷设备、容器或建筑物的隔热，例如以绝缘管、夹心元件、绝缘片的形式或作为制冷设备中的绝缘层。
以下参照实施例说明本发明。
实施例
将参考下面的实施例更详细地解释本发明。使用以下分析方法：
羟值:OH值的测定根据DIN 53240（1971年12月）的规程进行。
酸值:根据DIN EN ISO 2114（2002年6月）
导热系数:根据DIN 52616:1977-11；在20 K的温差和10℃的泡沫中点温度（Schaumstoffmittentemperatur）下。
固化时间:固化时间（“凝胶点tG”）通过将木棒***反应的混合物中并又从取出来确定。它表征了混合物开始固化的时间点。该时间点作为tG给出，在该点在木棒和反应的混合物之间首次可以拉出丝。时间测量从混合泡沫组分开始。
无粘性时间（Klebfreizeit）:在达到固化时间后不久，用木棍以短的时间间隔测试泡沫表面。从混合开始起，当木棍从泡沫表面毫无困难地脱离而没有任何粘附的产品时达到无粘性时间。
粗密度:根据DIN EN ISO 845:2009-10确定粗密度。
尺寸稳定性:尺寸稳定性通过在室温下测定从至少12小时前制备的泡沫块切下具有至少100 cm3 体积并且不包含压实的边缘区域（Randzoneverdichtung）的长方体形样品体的精确尺寸来确定。将如此得到的样品体在升高的温度（例如100℃）下储存给定的时间（例如24小时），并且在冷却30分钟至室温后重新测定其尺寸。以各自原始尺寸的百分比给出尺寸的相对变化。
粘附性:在实验室中通过在铺了纸的边长为20 cm x 20 cm的向上开口的木制模具中制备泡沫并在5分钟和24小时之后用手将纸从泡沫上剥下来定性确定泡沫粘附性。根据下述标度定性评估粘附性能：非常好= 1，好= 2，中等= 3，差= 4，无粘附= 5。
以类似的方式在双输送带上生产的泡沫样品上进行粘附性测试，其中在此=放入尺寸为50 cm * 90 cm的金属片并过度发泡。
粘度:动态粘度值使用Anton Paar公司的流变仪MCR 51根据DIN 53019：2008-09用测量锥CP 50-1，直径50mm，角度1°，在25、100、200和500 s-1的剪切速率下测定。本发明的和非本发明的多元醇表现出不依赖于剪切速率的粘度值。
燃烧性能:BVD测试按照由Vereinigung kantonaler Feuerversicherungen在1988年发布的用于确定建筑材料可燃性水平的瑞士基本测试，其补充为1990年，1994年，1995年和2005年（可从Vereinigung kantonaler Feuerversicherungen, Bundesstr. 20, 3011伯尔尼，瑞士获得）。
抗压强度/压缩弹性模量: 根据DIN EN 826:2013在压缩实验中测定。
压痕深度:通过如下来测定：在边长为20 cm x 20 cm的向上开口的木制模具（参见粘附性）中制备的尚未完全反应完的泡沫上，在1.5分钟后，从混合泡沫组分起测量，放上在具有直径2cm的圆形接触表面（Auflagefläche）的6kg重物，然后在2.5和5分钟的时间之后确定压痕深度（mm），同样从混合泡沫成分起测量。泡沫的层厚度为约15cm。
横向拉伸强度:根据EN 1607，在垂直于覆盖层的拉伸试验中测定。
使用的原料
聚酯S240P: Covestro Deutschland AG公司的通过缩合制备的聚酯多元醇，基于邻苯二甲酸酐和二甘醇，羟值为240±15mg KOH/g，酸值最大值为1.80mg KOH/g并且在25℃下测量的粘度为12000±2500mPas。
Desmophen 2382 Covestro Deutschland AG公司的聚酯多元醇，OH值为大约240 mgKOH/g，通过缩聚制备。
Desmophen® V657: Covestro Deutschland AG公司的反应性三官能聚醚多元醇，用于生产聚氨酯产品，羟值为255±15 mg KOH/g，酸值最大值 0.350mg KOH/g，并且在25℃下测量的粘度为265±20mPas。
Desmophen® T460: Covestro Deutschland AG公司的胺基多官能聚醚多元醇，用于生产聚氨酯产品，羟值为415±20mg KOH/g，并且在25℃下测量的粘度为8000±1500mPas。
Desmophen® L2830: Covestro Deutschland AG公司的具有主要为伯羟基的双官能聚醚多元醇，羟值为26-30mg KOH/g，25℃下的粘度为790-930mPa·s
Levagard PP: 三氯异丙基磷酸酯；Lanxess公司的阻燃剂
TEP:磷酸三乙酯，Lanxess公司的阻燃剂
添加剂1132:Covestro Deutschland AG公司，包含邻苯二甲酸酐和二甘醇的反应产物，酸值约97mg KOH/g。
B8443：Tegostab B8443, Evonik公司的稳定剂
添加剂19IF00 A: Covestro Deutschland AG公司的用于生产PUR/PIR-硬质泡沫的作为共发泡剂起作用的组分，羟值为1440±50mgKOH/g，胺值为290±15mgKOH/g，酸值为142±9mgKOH/g和在25℃下的粘度为390±70 mPa•s。
Desmorapid 1792: Covestro Deutschland AG公司的发泡剂; 用于生产聚氨酯硬质泡沫产品。Desmorapid®1792催化聚异氰脲酸酯反应。
Activator 726-B: N,N-二甲基环己胺。Covestro Deutschland AG公司的用于生产聚氨酯的催化剂。
正戊烷: Julius Hoesch公司的正戊烷。
Desmodur® 44V70L: 二苯基甲烷-4,4'-二异氰酸酯（MDI）与异构体和更高官能度的同系物的液体混合物，NCO含量在30.5-32.0重量％NCO范围，并且在25℃下的粘度在610-750mPas 的范围，来自Covestro Deutschland AG公司。
NMI: BASF公司的N-甲基咪唑
N-甲基二乙醇胺: Aldrich公司
Desmorapid DB: N,N-二甲基苄基胺，催化剂（Lanxess AG）。
Desmophen® 4051 B: 基于胺的四官能聚醚多元醇，用于生产聚氨酯产品，具有450-490mg KOH/g的羟值和在25℃下测量的4950-5850mPas的粘度（Covestro DeutschlandAG）。
EO: Ineos公司的氧化乙烯
PO: Lyondell公司的氧化丙烯
Irganox 1076: 3-(3,5-二叔丁基-4-羟基苯基)丙酸十八烷基酯（Ciba SpecialtyChemicals（现为BASF）），抗氧化剂。
A.) 通过加聚反应制备聚酯多元醇
制备规程实施例A-1.：
将273.6 g二甘醇（DEG）和1.8 g N-甲基咪唑（NMI）预先加入到2升实验室高压釜中。加热至50℃后，加入580.3g邻苯二甲酸酐。在关闭填充管接件之后，通过5次用3.0巴绝对压力的氮气填充设备并随后释放过压至大气压力来除去氧气。在200U/min.的搅拌器转速（十字条搅拌器（Kreuzbalkenrührer））下，将高压釜的内容物加热至120℃。在接近加热阶段结束时，压力（绝对压力）为2.8巴。将搅拌器转速提高到800U/min.，然后在5.95h的时间内以恒定的计量加入速度将346.1g氧化乙烯计量加入到高压釜的顶部空间中。在计量加入阶段快结束时，反应器压力达到的最大值为5.0巴（绝对压力）。在4.1小时的后反应时间后，最终压力达到3.9巴（绝对压力）。然后将产物在120℃在真空中加热1.0小时。冷却至80℃后，加入0.630g Irganox® 1076。该产物的OH值为250mg KOH/g，并且在25℃下的粘度为9805mPas。
表1示出了根据本发明的多元醇A1、A2、A11、A13和A14的配方。
A3V、A4V、A5V、A6V、A7V和A12V不是根据本发明的，因为为制备而使用的催化剂不含作为芳环体系的一部分的氮原子。A8V、A9V和A10V不是根据本发明的，因为为制备而使用的酸基团与烯化氧的当量比不在1：1.6至1：3.0的范围内。
B.) 制备PUR/PIR-硬质泡沫
通过向各自的多元醇添加阻燃剂、泡沫稳定剂、催化剂、水和发泡剂，以实验室规模制备PUR/PIR-硬质泡沫。
将如此得到的异氰酸酯反应性组合物与异氰酸酯混合并注入模具中。使用搅拌器，在4200U/min.和23℃原料温度下制备混合物本身。表2中汇总了精确配方，包括相应的物理研究的结果。
表 2: 以实验室规模制备PUR/PIR泡沫及其性能。
实施例: B-1V标准 B-2 B-3
多元醇侧:
聚酯S240P [重量份] 63.8
多元醇 A-1 [重量份] 53.8 53.8
Desmophen V657 [重量份] 5.0
Desmophen T460 [重量份] 5.0 5.0
Desmophen L2830 [重量份] 10.0 10.0
Levagard PP [重量份] 20.0 25.0 25.0
TEP [重量份] 5.0
添加剂1132 [重量份] 2.2 2.2 2.2
B8443 [重量份] 4.0 4.0 4.0
添加水以前的粘度 [mPas]，25℃ 1400 1650 1650
水 [重量份] 1 1
添加剂19IF00A [重量份] 1.5 1.5
Desmorapid 1792 [重量份] 4.0 3.8 2.7
Activator 726-B [重量份] 0.5
戊烷 [重量份] 15.1 12.9 11.8
异氰酸酯侧:
Desmodur 44V70L [重量份] 203 241 216
制备和性能:
指数 350 331 331
固化时间 [s] 46 48 47
无粘性时间 [s] 59 62 82
粗密度 [kg/m³] 38.9 38.2 40.2
在5 min/24h后的粘附性 2/2 2/2 1-2/2
压痕深度, 2.5/5 min [mm] 7.0/8.0 4.0/4.5 10.0/11.0
在100℃下24 h后的尺寸稳定性: 长、宽和厚度 (%, 最大) -0.1/0/-0.2 -0.6/-0.3/-0.1 0.2/0.4/-0.2
BVD (等级) 5 5 5
BVD (火焰高度的平均值) [mm] 133 130 120
因此，表2表明，所设定的目的已经实现。
根据本发明的实施例B-2和B-3达到了工业标准B-1V的BVD燃烧等级，而其它重要的特征参数例如粗密度、尺寸稳定性和粘附性能至少保持不变或甚至稍微改善。
表 3: 在双输送带装置上制备PUR/PIR泡沫及其性能。泡沫厚度设定为105mm，作为覆盖层使用厚度为50μm的铝箔。
实施例 B-4V参照 B-5 B-6 B-7
多元醇侧:
Desmophen 2382 [重量份] 63.8
多元醇 A-1 [重量份] 53.8 53.8 53.8
Desmophen V657 [重量份] 5.0
Desmophen T460 [重量份] 5.0 5.0 5.0
Desmophen L2830 [重量份] 10.0 10.0 10.0
Levagard PP [重量份] 20.0 25.0 25.0 25.0
TEP [重量份] 5.0
添加剂1132 [重量份] 2.2 2.2 2.2 2.2
B8443 [重量份] 4.0 4.0 4.0 4.0
水 [重量份] 1.0 1.0 1.0
添加剂19IF00A [重量份] 1.5 1.5
Desmorapid 1792 [重量份] 5.0 5.2
Activator 726-B [重量份] 0.5 0.5
戊烷 [重量份] 16.6 14.7 13.9 14.8
异氰酸酯侧:
Desmodur 44V70L [重量份] 210 250 221 240
制备和性能:
指数 [ ] 354 334 335 361
固化时间 [s] 31 30 32 31
粗密度 [kg/m³] 39 38.9 39.4 39.5
BVD (等级) 5 5 5 5
BVD (火焰高度的平均值) [mm] 146 123 120 130
导热系数, 10℃,0值 [mW/(m*K)] 21.86 20.57 21.36 22.0
抗压强度/压缩-E-模量 [MPa][MPa] 0.1263.48 0.1453.98 0.2076.24 0.2498.51
横向拉伸强度 [MPa] 0.109 0.122 0.120 0.143
在100℃下的尺寸稳定性长、宽和厚度 [%] 1.8 -0.5/-0.3/0.8 -0.1/-0.6/1.3 -0.6/0.2/0.9
粘附性，金属片，新鲜/24h 2/3 2/4 2/3+ 2/4
带温度 [° C] 60 60 60 60
因此，表3也表明，已能达成所设定的目的。
特别地，根据本发明的实施例B-5、B-6和B-7达到了工业标准B-4V的BVD燃烧等级，但是，火焰高度显著降低。其它重要的特征参数，例如导热系数、抗压强度、尺寸稳定性和粘附性能保持至少不变或甚至略有改善。

Claims (15)

1.制备PUR/PIR-硬质泡沫的方法，其包括至少一种聚酯多元醇(a)与下述物质的反应：
(b) 至少一种含多异氰酸酯的组分，
(c) 至少一种发泡剂，
(d) 至少一种催化剂，
(e) 任选地至少一种阻燃剂和/或其他助剂和添加物，
(f) 任选地至少一种不同于聚酯多元醇(a)的具有至少两个异氰酸酯反应性基团的另外的化合物，
所述聚酯多元醇(a)可通过下述反应得到：
a.1.) 至少一种环状羧酸酐；
a.2.) 至少一种分子量为62至450 Da的低分子量二醇；和
a.3.) 至少一种烯化氧；
通过组分a.1.)和a.2.)的酯化，和随后借助于组分a.3.)将所产生的羧酸半酯烷氧基化；
其中至少所述烷氧基化使用
a.4.) 至少一种胺催化剂来进行，在该胺催化剂中一个或多个氮原子是芳族环体系的一部分。
2.根据权利要求1所述的方法，其特征在于，每mol a.1.)使用≥1.5mol 的a.3.)，并且(a)具有100-280 mg KOH/g的OH值。
3.根据权利要求1或2所述的方法，其特征在于，a.3.)与a.1.)的当量比为1.6:1至3:1。
4.根据前述权利要求中任一项所述的方法，其特征在于，a.4.)选自咪唑及其衍生物，优选为N-甲基咪唑。
5.根据前述权利要求中任一项所述的方法，其特征在于，a.3.)选自氧化乙烯、氧化丙烯或其混合物。
6.根据前述权利要求中任一项所述的方法，其特征在于，a.1.)选自马来酸酐、衣康酸酐、柠康酸酐、琥珀酸酐、戊二酸酐、邻苯二甲酸酐和四氢邻苯二甲酸酐或其混合物。
7.根据前述权利要求中任一项的方法，其特征在于，a.2.)选自乙二醇、二甘醇、三甘醇、四甘醇或其混合物。
8.根据前述权利要求中任一项所述的方法，其特征在于，(b)选自2,4-；2,6-甲苯二异氰酸酯; 4,4'-；2,4'-二苯基甲烷二异氰酸酯，上述的衍生物和它们的混合物。
9.根据前述权利要求中任一项所述的方法，其特征在于，(c)选自正戊烷、环戊烷、异戊烷、水、羧酸或其混合物。
10.根据前述权利要求中任一项所述的方法，其特征在于，(e)选自至少一种阻燃剂，填料，泡孔调节剂，泡沫稳定剂，表面活性化合物，抗氧化、热或微生物降解或老化的稳定剂或其混合物。
11.根据前述权利要求中任一项所述的方法，其特征在于，(f)选自至少一种聚醚多元醇，不同于(a)的聚酯多元醇及其混合物。
12.根据前述权利要求中任一项所述的方法，其特征在于，
以10至24重量％，优选12至22重量％的量包含(a);
以43至89重量％，优选48至83重量％的量包含(b);
以0.1-30重量％，优选0.5-20重量％的量包含(c);
以0.05至3重量％，优选为0.06至2重量％的量包含(d);
以0.5至12重量％，优选3至9重量％的量包含(e);
以0.1至9重量％，优选为1.4至7.5重量％的量包含(f);
其中组分(a)至(f)为100重量％。
13.PUR/PIR-硬质泡沫，其可根据权利要求1至12中任一项所述的方法获得。
14.复合元件，其包含根据权利要求13所述的PUR/PIR-硬质泡沫和至少一个覆盖层，所述覆盖层选自混凝土，木材，压板，铝，铜，钢，不锈钢，纸，无纺织物和塑料以及多层复合材料或其组合。
15.根据权利要求13所述的PUR/PIR-硬质泡沫或根据权利要求14所述的复合元件用于隔热的用途。
CN201680069002.3A 2015-11-26 2016-11-23 得自加聚-低聚酯的pur/pir硬质泡沫 Pending CN108350143A (zh)

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