CN102470629B - 制造泡沫复合元件的方法 - Google Patents

制造泡沫复合元件的方法 Download PDF

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Publication number
CN102470629B
CN102470629B CN201080034543.5A CN201080034543A CN102470629B CN 102470629 B CN102470629 B CN 102470629B CN 201080034543 A CN201080034543 A CN 201080034543A CN 102470629 B CN102470629 B CN 102470629B
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China
Prior art keywords
adhesion promoter
cover layer
polyether polyol
polymer polyatomic
composite element
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CN201080034543.5A
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English (en)
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CN102470629A (zh
Inventor
J.范德布拉克
R.勒尔斯
P.哈斯
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Covestro Deutschland AG
Bayer Intellectual Property GmbH
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Bayer MaterialScience AG
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Priority claimed from EP09010091A external-priority patent/EP2286989A1/de
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Abstract

本发明涉及制造泡沫复合元件的方法，包括以下步骤：提供覆盖层，施加附着力促进剂，和将包含聚氨酯和/或聚异氰脲酸酯的泡沫层施加至附着力促进剂，特征在于附着力促进剂由至少一种选自以下的化合物组成：聚醚多元醇(B.1)、聚合物多元醇(B.2)、聚脲分散体(B.3)、聚酯多元醇(B.4)和PIPA多元醇(B.5)。本发明进一步涉及至少一种选自聚醚多元醇、聚合物多元醇和聚脲分散体的化合物作为附着力促进剂在泡沫复合元件制造中的用途，以及通过根据本发明的方法制造的泡沫复合元件。

Description

制造泡沫复合元件的方法
本发明涉及制造泡沫复合元件的方法，包括以下步骤：提供覆盖层，将附着力促进剂施加至覆盖层，和将包含聚氨酯和/或聚异氰脲酸酯的泡沫层施加至附着力促进剂，特征在于附着力促进剂由至少一种选自聚醚多元醇、聚合物多元醇、聚脲分散体、聚酯多元醇和PIPA多元醇的化合物组成。本发明进一步涉及至少一种选自聚醚多元醇、聚合物多元醇和聚脲分散体的化合物作为附着力促进剂在泡沫复合元件制造中的用途，并且涉及通过根据本发明的方法制造的泡沫复合元件。
对于连续制造基于聚氨酯硬质泡沫，即是说聚氨酯和聚异氰脲酸酯硬质泡沫的金属夹层元件，金属覆盖层对泡沫的附着力是重要的，特别是当泡沫为聚异氰脲酸酯泡沫时。在市场上已确立的是双组分聚氨酯附着力促进剂体系。原则上通过使用这类双组分附着力促进剂体系显著提高附着力，这对于最终组件的生产商而言意味着改进的产品。特别地，附着力失效的长期风险显著降低。
然而，在这种双组分附着力促进剂体系的加工期间可能出现附着力促进剂组分难以充分均匀。不充分均匀可能意味着在金属复合元件的长期粘结性能方面的高风险，因为在交变的温度情形中可能出现覆盖层对泡沫的附着力失效。此外，这意味着在生产阶段的开始时双组分附着力促进剂体系加工的相对高次品率。
为了避免由于两种附着力促进剂组分不充分均匀的粘结性能不足的风险，提供了单组分溶液。例如，EP1516720A1公开了聚氨酯附着力促进剂用于提高包含聚异氰脲酸酯泡沫和覆盖层的复合元件的层间附着力的用途，以及这样的复合元件本身和它们的制造方法。
EP1593438A2公开了用于制造夹层复合元件的设备和方法。所述设备至少由先后连接的用于覆盖层的两个进料设备、用于附着力促进剂的施加设备、用于芯层的施加设备、传送设备和偏转设备组成。用于附着力促进剂的施加设备至少由用于附着力促进剂的进料管、具有至少一个侧面出口开口的转盘加料器，和用于转盘加料器的驱动组成。可以使用例如基于聚氨酯，例如含NCO基团的预聚物的单组分体系作为附着力促进剂。另外可能的单组分体系基于聚氯丁二烯、环氧化物或聚乙酸乙烯酯。附着力促进剂也可由多组分体系，优选双组分体系组成。优选的双组分体系是聚氨酯体系。
一直以来的目的是提高泡沫复合元件中泡沫与覆盖层之间的附着力。因此，需要用于制造这种复合元件的替代性和改进的方法，所述方法特别允许泡沫复合元件中泡沫与覆盖层之间提高的附着力并且同时在泡沫/覆盖层界面区最多出现轻度的瑕疵。
本发明因此提供一种制造泡沫复合元件的方法，包括以下步骤：
A)提供覆盖层；
B)将附着力促进剂施加至覆盖层；和
C)将包含聚氨酯和/或聚异氰脲酸酯的泡沫层施加至多元醇化合物，
特征在于附着力促进剂由至少一种选自以下的化合物组成：聚醚多元醇(B.1)、聚合物多元醇(B.2)、聚脲分散体(B.3)、聚酯多元醇(B.4)和PIPA多元醇(B.5)。
发现通过使用聚醚多元醇(B.1)、聚合物多元醇(B.2)、聚脲分散体(B.3)、聚酯多元醇(B.4)和/或PIPA多元醇(B.5)作为附着力促进剂，与已知的体系相比，泡沫对覆盖层的附着力可以提高。因此根据本发明，除了由至少一种选自聚醚多元醇(B.1)、聚合物多元醇(B.2)、聚脲分散体(B.3)、聚酯多元醇(B.4)和PIPA多元醇(B.5)的化合物组成的根据本发明的附着力促进剂外，不使用另外的附着力促进剂。通过仅使用根据本发明的附着力促进剂，特别地可以避免在不充分混合的双组分附着力促进剂体系上要避免的问题。不充分混合的附着力促进剂体系将导致气泡形成或者复合材料中削弱点(Sollbruchstelle)。有利地，单独使用多元醇化合物也使得能够润湿覆盖层的整个表面。
根据本发明制造的泡沫复合元件特别适合作为绝热元件。
根据本发明的方法的步骤A)涉及提供覆盖层。这可以在连续制造设备中，例如通过从辊上解开卷起的覆盖层进行。覆盖层的性质目前没有进一步规定，可以优选使用在绝热领域中常规用于覆盖层的材料。覆盖层的厚度可以例如为≥200μm至≤5mm，优选≥300μm至≤2mm并且特别优选≥400μm至≤1mm。
在步骤B)中，将根据本发明的附着力促进剂施加至提供的覆盖层。可以使用常规技术例如喷涂或辊涂进行施加。根据本发明的附着力促进剂由至少一种选自以下的化合物组成：聚醚多元醇(B.1)、聚合物多元醇(B.2)、聚脲分散体(B.3)、聚酯多元醇(B.4)和PIPA多元醇(B.5)。优选地，根据本发明的附着力促进剂由至少一种选自聚醚多元醇(B.1)和聚合物多元醇(B.2)的化合物组成。最优选地，使用例如B.1:B.2比例=3:1－1:3的聚醚多元醇(B.1)和聚合物多元醇(B.2)的混合物作为附着力促进剂。
优选地，根据本发明的附着力促进剂具有1－8，特别优选2－4，最特别优选2－3的羟基官能度。
优选地，根据本发明的附着力促进剂具有15－500，特别优选20－200，最特别优选20－60的羟值。
优选地，根据DIN53015在25℃温度下测量，根据本发明的附着力促进剂具有200－30,000mPa.s，特别优选200－20,000mPa.s，最特别优选200－10,000mPa.s的粘度。
使用通过已知方法制备的聚醚多元醇(B.1)作为附着力促进剂。这例如通过用碱金属氢氧化物例如氢氧化钠或钾，或者用碱金属醇盐例如甲醇钠、甲醇钠或钾或者异丙醇钾作为催化剂，并且加入至少一种包含连接在其中的2－8个活性氢原子，优选2－3个活性氢原子的起始物分子阴离子聚合制备聚氧亚烷基多元醇，或者通过用路易斯酸例如五氯化锑、三氟化硼醚化物等或膨润土作为催化剂由一种或多种在亚烷基部分具有2－4个碳原子的环氧烷的阳离子聚合进行。在本发明范围内，聚醚多元醇B.1不含填料。
根据本发明合适的环氧烷是例如环氧乙烷、1,2-环氧丙烷、四氢呋喃、1,3-环氧丙烷、1,2-和2,3-环氧丁烷，并且优选环氧乙烷和1,2-环氧丙烷。环氧烷可以分开地，交替地先后或者以混合物形式使用。
作为起始物分子，优选使用选自以下的化合物：水，有机二羧酸例如丁二酸、己二酸、邻苯二甲酸和对苯二甲酸，在烷基部分中具有1－4个碳原子的脂族和芳族，任选地N-单-、N,N-和N,N'-二烷基取代的二胺，例如任选地单-和二-亚烷基取代的乙二胺，二亚乙基三胺，三亚乙基四胺，1,2-亚丙胺，1,3-和1,4-亚丁基二胺，1,2-、1,3-、1,4-、1,5-和1,6-六亚甲基二胺，亚苯基二胺，2,3-、3,4-、2,4-和2,6-亚甲苯基二胺以及4,4'-、2,4'-和2,2'-二氨基二苯基甲烷，链烷醇胺例如乙醇胺、N-甲基-和N-乙基-乙醇胺，二链烷醇胺例如二乙醇胺、N-甲基-和N-乙基-二乙醇胺，和三链烷醇胺，例如三乙醇胺，和氨。优选使用多元醇，特别是二至八元的醇和/或亚烷基二醇，例如乙二醇、1,2-和1,3-丙二醇、二甘醇、二丙二醇、1,4-丁二醇、1,6-己二醇、甘油、三羟甲基丙烷、季戊四醇、山梨醇和蔗糖，和至少两种多元醇的混合物。
作为聚醚多元醇，也可以使用可以通过环氧烷和另外的单体(例如酐、二氧化碳)加成到起始物分子上制备的共聚物，例如聚醚碳酸酯多元醇。通过环氧烷和二氧化碳阳离子加成到H-官能起始物分子上制备聚醚碳酸酯多元醇描述于例如Inoue等人,CopolymerizationofCarbonDioxideandEpoxidewithOrganometallicCompounds;DieMakromolekulareChemie130,210-220,1969中。
聚醚多元醇优选为聚氧丙烯和聚氧丙烯-聚氧乙烯多元醇。聚醚多元醇优选具有2－8的官能度，并且特别优选20－500的羟值。
聚醚多元醇(B.1)可以单独地或者以与另外的聚醚多元醇的混合物形式，或者以与另外的附着力促进剂B.2－B.5的混合物形式使用。优选地，使用聚醚多元醇(B.1)与聚合物多元醇(B.2)和/或聚脲分散体(B.3)的混合物作为附着力促进剂。
优选地，根据DIN53015在25℃温度下测量，聚醚多元醇具有200－30,000mPa.s，特别优选200－20,000mPa.s，最特别优选200－10,000mPa.s的粘度。
根据本发明，还使用聚合物多元醇(B.2)作为附着力促进剂。聚合物多元醇通常也被称为接枝多元醇。这些聚合物多元醇常规地通过合适的烯属单体例如苯乙烯、丙烯腈、丙烯酸酯和/或丙烯酰胺在充当接枝基底的聚醚醇(“载体聚醚醇”)中自由基聚合制备。通常通过自由基从生长的聚合物链转移到聚醚多元醇形成侧链。除了接枝共聚物外，聚合物多元醇主要包含分散在未改变的聚醚醇中的烯烃均聚物。
在优选实施方案中，丙烯腈、苯乙烯，特别是比例为1:1－3:1的苯乙烯和丙烯腈作为单体以及任选地在另外的单体、大分子单体、缓和剂(Moderator)的存在下，并且使用自由基引发剂，大多数为偶氮或过氧化合物，在作为连续相的聚醚醇或聚酯醇中制备。
作为载体聚醚醇，通常考虑通过环氧烷，优选环氧乙烷和/或环氧丙烷的阴离子、阳离子或中性聚合(DMC)制备的具有2－8，优选2－3的羟基官能度，20－100mgKOH/g，优选25－70mgKOH/g的羟值的化合物。
大分子单体，也称为稳定剂，是具有至多2000g/mol数均分子量的线型或支化多元醇，其包含至少一个末端反应性烯属不饱和基团。通过与酐(马来酸酐、富马酸)，丙烯酸酯和甲基丙烯酸酯衍生物以及异氰酸酯衍生物，例如3-异丙烯基-1,1-二甲基苄基异氰酸酯、甲基丙烯酸异氰酸根合乙酯反应，可以将乙烯属不饱和基团引入已经存在的多元醇。
在自由基聚合期间，将大分子单体一并引入共聚物链。因此，形成具有聚醚嵌段和聚丙烯腈-苯乙烯嵌段的嵌段共聚物，其充当连续相与分散相之间的界面的相相容剂并且抑制聚合物多元醇颗粒团聚。基于用于制备聚合物多元醇的单体的总重量，大分子单体的份额通常为1－15重量%。
缓和剂，也称为链转移剂，通常用于制备聚合物多元醇(B.2)。缓和剂减少通过生长的自由基链转移导致的所形成的共聚物的分子量，结果是聚合物分子之间的交联减少，这影响了聚合物多元醇的粘度和分散稳定性以及过滤性。基于用于制备聚合物多元醇的单体的总重量，缓和剂的份额通常为0.5－25重量%。常规用于制备聚合物多元醇的缓和剂是醇，例如1-丁醇、2-丁醇、异丙醇、乙醇、甲醇，环己烷，甲苯，硫醇例如乙硫醇、1-庚硫醇、2-辛硫醇、1-十二烷硫醇、硫代苯酚、巯基乙酸2-乙基己酯、巯基乙酸甲酯、环己基硫醇和烯醇醚化合物，吗啉类化合物和α-(苯甲酰氧基)苯乙烯。
为了引发自由基聚合，常规地使用过氧化物或偶氮化合物，例如过氧化二苯甲酰、过氧化月桂酰、过氧-2-乙基己酸叔戊酯、二叔丁基过氧化物、过氧碳酸二异丙酯、过氧-2-乙基己基叔丁酯、过新戊酸叔丁酯、过新癸酸叔丁酯、过苯甲酸叔丁酯、过巴豆酸叔丁酯、过异丁酸叔丁酯、过氧-1-甲基丙酸叔丁酯、过氧-2-乙基戊酸叔丁酯、过氧辛酸叔丁酯和过邻苯二甲酸二叔丁酯，2,2'-偶氮双(2,4-二甲基戊腈)、2,2'-偶氮双异丁腈(AIBN)、2,2'-偶氮双异丁酸二甲酯、2,2'-偶氮双(2-甲基丁腈)(AMBN)、1,1'-偶氮双(1-环己甲腈)。基于用于制备聚合物多元醇的单体的总重量，引发剂的份额常规地为0.1－6重量%。
由于单体的反应速率和引发剂的半衰期，因此制备聚合物多元醇的自由基聚合常规地在70－150℃的温度和至多20巴的压力下进行。用于制备聚合物多元醇的优选的反应条件是80－140℃的温度、大气压至15巴的压力。
优选地，聚合物多元醇(B.2)具有1－45重量%，特别优选5－30重量%，最特别优选15－25重量%的填料含量。
优选地，根据DIN53015在25℃温度下测量，聚合物多元醇具有200－30,000mPa.s，特别优选200－20,000mPa.s，最特别优选200－10,000mPa.s的粘度。
优选地，聚合物多元醇具有≥50mol%至≤100mol%的伯羟基含量。
聚合物多元醇组分可以例如通过环氧丙烷和环氧乙烷加成到作为起始物分子的甘油上制备。环氧丙烷的份额可以有利地为≥80重量%至≤95重量%，并且环氧乙烷的量可以有利地为≥5重量%至≤20重量%。聚合物多元醇中伯羟基的份额也可以特别优选为≥60mol%至≤80mol%。
根据本发明，也使用聚脲分散体(B.3)作为附着力促进剂。本发明范围内的聚脲分散体是含填料的聚醚多元醇，填料是二和/或多异氰酸酯与二胺和/或肼的反应产物。优选地，聚脲分散体通过二胺和/或肼与二和/或多异氰酸酯在根据组分B.1的聚醚多元醇的存在下获得(PHD分散体)。
根据组分B.3的聚脲分散体(PHD分散体)例如通过二和/或多异氰酸酯或者异氰酸酯混合物与二胺和/或肼在根据组分B.1的聚醚多元醇中现场聚合制备。优选地，PHD分散体通过75－85重量%2,4-甲苯二异氰酸酯(2,4-TDI)和15－25重量%2,6-甲苯二异氰酸酯(2,6-TDI)的异氰酸酯混合物与二胺和/或肼在根据组分B.1的聚醚多元醇，优选通过三官能起始物(例如甘油和/或三羟甲基丙烷)烷氧基化制备的聚醚多元醇中反应制备。用于制备PHD分散体的方法描述于例如US4,089,835和US4,260,530中。
聚脲分散体优选具有1－45重量%，特别优选5－30重量%，最特别优选10－25重量%的填料含量。
使用聚酯多元醇(B.4)作为附着力促进剂。聚酯多元醇(B.4)特别由具有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，和多元醇，优选具有2－12个碳原子，优选2－6个碳原子的链烷二醇，具有3－6个碳原子的二亚烷基二醇和/或链烷三醇制备。根据本发明使用的二羧酸优选选自丁二酸、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。二羧酸可以单独地或者以混合物使用。代替二羧酸，还可以使用相应的羧酸衍生物，例如具有1－4个碳原子的醇的二羧酸酯或者二羧酸酐。作为二和多元醇，特别是链烷二醇和二亚烷基二醇，根据本发明可以使用选自乙二醇、二甘醇、1,2-和1,3-丙二醇、二丙二醇、1,4-丁二醇、1,5-戊二醇和1,6-己二醇的化合物。
也可以使用得自内酯例如ε-己内酯，或羟基羧酸例如ω-羟基己酸的聚酯多元醇。
为了制备聚酯多元醇，可以不使用催化剂或者优选地在酯化催化剂存在下，有利地在惰性气体例如氮气、氦气、氩气等气氛中在熔体中在150－250℃，优选180－220℃温度下，任选地在减压下使有机的，例如芳族和优选脂族二羧酸和/或它们的衍生物以及多元醇和/或亚烷基二醇聚合至希望的酸值，其有利地小于10，优选小于2。
根据优选实施方案，使酯化混合物在上述温度下在常压下缩聚至80－30，优选40－30的酸值并且然后在小于500毫巴，优选50－150毫巴的压力下缩聚。作为酯交换催化剂，考虑例如金属、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。然而，缩聚也可以在液相中在稀释剂和/或夹带剂，例如苯、甲苯、二甲苯或氯苯的存在下进行，用于共沸蒸馏出缩合水。
为了制备聚酯多元醇，有利地使有机二羧酸和/或它们的衍生物以及多元醇以1:1-1.8，优选1:1.05-1.2的摩尔比缩聚。所得的聚酯多元醇优选具有2－4，特别为2－3的官能度，和20－140，优选20－40的羟值。
优选地，根据DIN53015在25℃温度下测量，聚酯多元醇具有200－30,000mPa.s，特别优选200－20,000mPa.s，最特别优选200－10,000mPa.s的粘度。
也使用PIPA多元醇(B.5)作为附着力促进剂。这些是通过链烷醇胺和二异氰酸酯在根据B.1的聚醚多元醇中反应得到的含氨基甲酸酯基团的分散体。根据组分B.5的含填料的聚醚多元醇优选为PIPA(多异氰酸酯与链烷醇胺加聚)改性的聚醚多元醇，所述聚醚多元醇具有2.5－4的官能度和500－18,000的分子量。
附着力促进剂的层厚可以为例如≥10μm至≤500μm，优选≥20μm至≤200μm并且特别优选≥25μm至≤100μm。
使用组分B.1、B.2、B.3、B.4和/或B.5作为附着力促进剂允许在生产泡沫复合元件时中断，不会因此产生较大量的次品。尽管基于2-组分体系的常规附着力促进剂在短时间后反应掉，但作为附着力促进剂的组分B.1、B.2、B.3、B.4和/或B.5本身不反应或者不与本身反应。有利地，如果在生产过程中出现问题，则可以因此停止生产泡沫复合元件，不需要废弃大量材料。
在步骤C)中，将包含聚氨酯和/或聚异氰脲酸酯的泡沫层施加至附着力促进剂(组分B.1、B.2、B.3、B.4和/或B.5)的层。这也可以在连续生产设备中进行。该层可以例如以≥2cm至≤28cm、≥3cm至≤26cm并且优选≥4cm至≤24cm的厚度存在。可以在施加前即刻才使反应组分在混合头中混合并且将导致泡沫的反应混合物立即施加至附着力促进剂的层。使用包含聚异氰脲酸酯或者主要包含聚异氰脲酸酯的泡沫特别有利，因为即使具有减少的阻燃剂含量，它们也具有好的阻燃性能。
常规的脂族、脂环族和特别是芳族多异氰酸酯用于制备泡沫层。优选使用甲苯二异氰酸酯(TDI)、二苯基甲烷二异氰酸酯(MDI)，和特别是二苯基甲烷二异氰酸酯和聚亚苯基聚亚甲基多异氰酸酯(粗制MDI)的混合物。具有至少两个对异氰酸酯基团具反应性的氢原子的合适化合物通常是在分子中带有两个或更多个选自OH基、SH基、NH基、NH2基和CH-酸性基团例如β-二酮基的反应性基团的那些。优选使用聚醚醇和/或聚酯醇，优选聚醚醇。使用的聚醚醇和/或聚酯醇的羟值优选为25－800mgKOH/g，摩尔质量通常大于400g/mol。
泡沫层，通常也应被理解为是指泡沫层的泡沫，可以具有≥85%至≤100%，优选≥90%至≤100%的闭孔含量，其可以根据DINISO4590测量。此外，根据ASTM3576-77，泡沫层可以具有≥10μm至≤600μm，优选≥50μm至≤400μm的平均孔径。
当然，在根据本发明的方法中在步骤C)后可以再一次将如步骤B)中的附着力促进剂层施加至泡沫层并且然后施加另外的如步骤A)所述的覆盖层。然后获得两侧带有覆盖层的泡沫复合元件。所述方法可以例如在常规双皮带装置中进行。
在本发明方法的一个实施方案中，覆盖层的材料包括铝、钢、沥青、纸、矿物非织造物、包含有机纤维的非织造物、塑料板、塑料膜和/或木板。特别优选覆盖层是铝金属或钢。覆盖层，特别是铝或钢可以被涂覆。根据本发明使用的附着力促进剂特别在聚异氰脲酸酯泡沫与铝覆盖层或钢覆盖层之间产生特别好的附着力。
在根据本发明的方法的另一个实施方案中，附着力促进剂以≥20g/m2至≤50g/m2的量施加至覆盖层。这说明与已知方法相比所需的附着力促进剂的量减少。施加至覆盖层的附着力促进剂的量也可以为≥25g/m2至≤35g/m2。总的来说，因此获得材料节省(更少的附着力促进剂)。
在根据本发明的方法的另一个实施方案中，在施加附着力促进剂和用于制备泡沫层的反应混合物后，将覆盖层加热至≥20℃至≤70℃，特别优选≥40℃至≤60℃的温度。通过加热覆盖层加快附着力促进剂与其它层的反应，总的获得更牢固的粘结。在施加附着力促进剂前，也可以特别优选将覆盖层加热至≥45℃至≤55℃的温度。
在根据本发明的方法的另一个实施方案中，泡沫层可由多异氰酸酯和至少一种选自包含聚酯多元醇和聚醚多元醇的反应混合物的化合物反应获得，反应开始前反应混合物中异氰酸酯基团与对异氰酸酯具反应性的基团(例如羟基)的摩尔比为≥1:1至≤5:1。该情形通常由指数(Kennzahl)表示。所述指数给出了实际使用的异氰酸酯量与化学计算量，即计算的异氰酸酯基团(NCO)量的百分比：
指数=[(使用的异氰酸酯的量):(计算的异氰酸酯的量)]×100(I)。
换句话说，该反应混合物的指数为100－500。指数也可以为≥150至≤350或≥200至≤300。伴随着该指数，主要获得聚异氰脲酸酯泡沫，如已经提及的那样其在较少量的阻燃剂就已足够并且由于根据本发明的方法，因此仍然可以牢固粘结于覆盖层，特别是铝覆盖层。该聚异氰脲酸酯泡沫优选为硬质泡沫，基于其在10%压缩下的压缩强度或者≥100kPa至≤300kPa定义。压缩强度或耐压缩性可以根据DIN53421/DINENISO604测量。其也可以为≥150kPa至≤250kPa或≥180kPa至≤280kPa。
在根据本发明的方法中（在其中泡沫层可由至少一种多异氰酸酯以及至少包含聚酯多元醇和任选的聚醚多元醇的反应混合物反应获得，具有≥150至≤350，特别优选≥200至≤300的指数），优选使用优选B.1与B.2和/或B.3的比例为3:1－1:3的聚醚多元醇(B.1)与聚合物多元醇(B.2)和/或聚脲分散体(B.3)的混合物作为附着力促进剂，所述附着力促进剂混合物的固含量优选为10－30重量%。
在根据本发明的方法的另一个实施方案中，泡沫层的表观密度为≥25g/l至≤48g/l，特别优选≥35g/l至≤45g/l。其可以根据标准ISO845测量。表观密度也可以最特别优选为≥37g/l至≤42g/l，仍然更优选≥39g/l至≤40g/l。与其无关的是，泡沫层，通常也应被理解为是指泡沫层的泡沫，另外也可以具有≥85%至≤100%，优选≥90%至≤100%的闭孔含量，其可以根据DINISO4590测量。此外，根据ASTM3576-77，泡沫层可以另外具有≥10μm至≤600μm，优选≥50μm至≤400μm的平均孔径。
本发明进一步涉及至少一种选自聚醚多元醇(B.1)、聚合物多元醇(B.2)和聚脲分散体(B.3)的化合物作为附着力促进剂在泡沫复合元件制造中的用途。用作附着力促进剂的聚醚多元醇(B.1)、聚合物多元醇(B.2)和聚脲分散体(B.3)的细节已经在上面描述，因此可以将它们全部引入作为参考。
本发明进一步提供一种通过根据本发明的方法得到的泡沫复合元件，其中覆盖层与泡沫层之间的附着力为≥0.20N/mm2至≤1.00N/mm2，特别优选≥0.20N/mm2至≤0.50N/mm2，最特别优选≥0.20N/mm2至≤0.30N/mm2。特别地，泡沫层可以是聚异氰脲酸酯泡沫层。附着力有利地根据DIN53292测量。在实际使用中，对于足够的附着力，0.20N/mm2的下限被认为特别有利。
本发明因此还提供一种包含以下层的泡沫复合元件
(α)覆盖层，
(β)由至少一种选自聚醚多元醇(B.1)、聚合物多元醇(B.2)、聚脲分散体(B.3)、聚酯多元醇(B.4)和PIPA多元醇(B.5)的化合物组成，优选由至少一种选自聚醚多元醇(B.1)、聚合物多元醇(B.2)、聚脲分散体(B.3)的化合物组成的附着力促进剂：和
(γ)包含聚氨酯和/或聚异氰脲酸酯的泡沫层，
其中所述层以顺序(α)-(β)-(γ)，优选以顺序(α)-(β)-(γ)-(β)-(α)布置。
实施例
附着力根据标准DIN53292测试。步骤与根据DIN53292-82的垂直于覆盖层平面的拉伸试验不同在于不同的样品厚度和覆盖层数目。在根据DIN53292-82的试验中，以覆盖层的总厚度为基础。整个样品的最弱区域由此决定了断裂点。相反，在这里所述的改进中的附着力试验允许侧面相关的附着力评价。因此通过垂直于覆盖层切割复合元件以取得样品。在测量中使用具有50mm边长和15mm样品高度(包括覆盖层)的正方形样品。
为了测量泡沫/覆盖层界面的瑕疵(“气泡形成”)，使金属复合元件在105℃回火1小时。然后取下金属复合元件的上部和/或底部覆盖层。检查除了硬聚氨酯泡沫的规则孔结构外是否出现塌陷-孔穴。
没有瑕疵:没有塌陷-孔穴。
微小瑕疵:塌陷-孔穴数目：1至小于5件，每个具有小于5mm的直径。
中等瑕疵:塌陷-孔穴数目：5至小于10件，和/或5－10mm的塌陷-孔穴直径。
大的瑕疵:塌陷-孔穴数目：至少10件，和/或大于10mm的塌陷-孔穴直径。
在实施例中使用以下附着力促进剂：
附着力促进剂HVA：基于甘油、环氧乙烷和环氧丙烷的聚醚多元醇的聚脲分散体，具有3的官能度和28mgKOH/g羟值。
附着力促进剂HVB:基于甘油、环氧乙烷和环氧丙烷的聚醚多元醇的聚合物多元醇，具有3的官能度和28mgKOH/g羟值，包含20重量%的基于SAN(60/40)填料。
附着力促进剂HVC:基于甘油、环氧乙烷和环氧丙烷的聚醚多元醇的聚合物多元醇，具有3的官能度和20mgKOH/g羟值，包含43重量%的基于SAN(60/40)填料。
附着力促进剂HVD：由50重量%附着力促进剂HVC和50重量%具有3的官能度和28mgKOH/g羟值的甘油、环氧乙烷和环氧丙烷的聚醚多元醇组成的混合物。
附着力促进剂HVE：具有3官能度和28mgKOH/g羟值的甘油、环氧乙烷和环氧丙烷的聚醚多元醇。
实施例1－6：
泡沫体系1：
a-组分：
39重量份聚醚酯多元醇1(通过在第一阶段使邻苯二甲酸酐、二甘醇和乙二醇反应得到聚酯多元醇，其在第二阶段用环氧乙烷增链制备。所得的聚醚酯多元醇1具有2的官能度和310mgKOH/g羟值)；
15.7重量份聚醚多元醇1(由丙二醇作为起始化合物以及环氧丙烷和环氧乙烷制备；所得的聚醚多元醇1具有2的官能度和28mgKOH/g羟值)；
12重量份聚醚多元醇2(由糖和乙二醇作为起始化合物以及环氧丙烷制备；所得的聚醚多元醇2具有3的官能度和380mgKOH/g羟值)；
25重量份阻燃剂1(磷酸三氯异丙酯，TCPP)；
5重量份稳定剂1(含硅酮的稳定剂)；
2.5重量份聚酯多元醇1(由邻苯二甲酸酐和二甘醇制备；所得的聚酯多元醇1具有795mgKOH/g羟值)；
0.8重量份水。
b-组分：
Desmodur44V70L(聚合的MDI，可由BayerMaterialScienceAG获得)。
将a-和b-组分以比例a:b=100:200彼此混合。为了制造具有200mm厚度的金属复合元件，还加入13重量份戊烷作为发泡剂，以及3重量份三聚催化剂乙酸钾和0.6重量份76重量%环己基二甲胺和24重量%五甲基三亚乙基二胺的混合物，所述重量份基于100重量份组分A。
使用如EP1593438A2中所述的设备，将附着力促进剂组合物施加至预热到40℃的钢片。使用的附着力促进剂的量均示于表1中。然后向其上施加根据泡沫体系1的具有上述组成的聚异氰脲酸酯泡沫。
表1.用泡沫体系1试验
实施例 附着力促进剂 施加的附着力促进剂的量[g/m2] 附着力[N/mm2] 气泡形成
1 (对比) 没有附着力促进剂 - 0.13 无
2 HV A 32 0.25 无
3 HV B 39 0.16 无
4 HV C 32 0.19 显著8 -->
5 HV D 45 0.27 轻微
6 HV E 34 0.18 轻微
对比＝对比例。
在实施例2－6的试验中，表明通过使用聚醚多元醇作为附着力促进剂，实现了附着力提高。
实施例7－10：
泡沫体系2：
a-组分：
63.8重量份聚酯多元醇2(由邻苯二甲酸酐、己二酸、单甘醇和二甘醇制备；所得的聚酯多元醇2具有240mgKOH/g羟值)；
5重量份聚醚多元醇2(由三羟甲基丙烷作为起始化合物以及环氧乙烷制备；所得的聚醚多元醇2具有3的官能度和240mgKOH/g的OH值)；
2.2重量份聚酯多元醇1(由邻苯二甲酸酐和二甘醇制备；所得的聚酯多元醇2具有795mgKOH/g羟值)；
20重量份阻燃剂TCPP；
5重量份阻燃剂TEP；
4重量份含硅酮的稳定剂。
b-组分：
Desmodur44V70L(聚合的MDI，可由BayerMaterialScienceAG获得)。
将a-和b-组分以比例a:b=100:160彼此混合。为了制造具有40mm厚度的金属复合元件，还加入15重量份戊烷作为发泡剂，以及5重量份三聚催化剂辛酸钾，所述重量份基于100重量份组分A。
使用喷枪将附着力促进剂组合物施加至预热到40℃的钢片。使用的附着力促进剂的量均示于表2中。然后向其上施加根据泡沫体系2的具有上述组成的聚异氰脲酸酯泡沫。
表2.用泡沫体系2试验附着强度
实施例 附着力促进剂 施加的附着力促进剂的量[g/m2] 附着力[N/mm2] 气泡形成
7 (对比) 没有附着力促进剂 - 0.17 轻微1)
8 HV D 18 0.20 无
9 HV D 25 0.34 无
10 HV D 32 0.20 无
对比＝对比例
1)在泡沫/钢片界面(产品下侧)的轻度瑕疵。
在用泡沫体系2的系列试验中，在没有附着力促进剂的参考试验中在复合元件回火后，在产品下侧的泡沫/钢片界面中发现微小瑕疵。
在泡沫体系2中用附着力促进剂D实现了至少0.2N/mm2的附着力值，其有利于标准板生产(实施例8－10)。

Claims (13)

1.用于制造泡沫复合元件的方法，包括以下步骤：
A)提供覆盖层；
B)将附着力促进剂施加到该覆盖层；和
C)将包含聚氨酯和/或聚异氰脲酸酯的泡沫层施加到该附着力促进剂，特征在于该附着力促进剂由至少一种选自以下的化合物组成：聚醚多元醇、聚合物多元醇、聚脲分散体、和聚酯多元醇，其中所述聚醚多元醇选自聚醚碳酸酯多元醇、聚氧丙烯和聚氧丙烯-聚氧乙烯多元醇。
2.根据权利要求1的方法，其中所述覆盖层的材料包括铝、钢、沥青、纸、矿物非织造物、包含有机纤维的非织造物、塑料板、塑料膜和/或木板。
3.根据权利要求1的方法，其中所述附着力促进剂具有2-8的羟基官能度。
4.根据权利要求1的方法，其中所述附着力促进剂具有15-500的羟值。
5.根据权利要求1-4任一项所述的方法，其中所述附着力促进剂由至少一种选自聚醚多元醇和聚合物多元醇的化合物组成。
6.根据权利要求5的方法，其中聚合物多元醇包含1-45重量％填料，基于该聚合物多元醇。
7.根据权利要求1的方法，其中所述附着力促进剂以≥20g/m2至≤50g/m2的量施加到该覆盖层。
8.根据权利要求1的方法，其中在施加所述附着力促进剂前将所述覆盖层加热至≥20℃至≤70℃的温度。
9.根据权利要求1的方法，其中所述泡沫层能由多异氰酸酯和包含至少一种选自聚酯多元醇和聚醚多元醇的化合物的反应混合物反应而获得，其中在反应开始时反应混合物中异氰酸酯基团与羟基的摩尔比为≥100∶100至≤400∶100。
10.根据权利要求1的方法，其中所述泡沫层的表观密度为≥30g/l至≤48g/l。
11.根据权利要求1的方法得到的泡沫复合元件，其中所述覆盖层与所述泡沫层之间的附着力为≥0.20N/mm2至≤1.00N/mm2。
12.包含以下层的泡沫复合元件：(α)覆盖层，(β)由至少一种选自以下的化合物组成的附着力促进剂：聚醚多元醇、聚合物多元醇、聚脲分散体、和聚酯多元醇，和(γ)包含聚氨酯和/或聚异氰脲酸酯的泡沫层，其中所述层以顺序(α)-(β)-(γ)布置，其中所述聚醚多元醇选自聚醚碳酸酯多元醇、聚氧丙烯和聚氧丙烯-聚氧乙烯多元醇。
13.根据权利要求12的泡沫复合元件，其中所述层以顺序(α)-(β)-(γ)-(β)-(α)布置。
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