CN102712732B - 硅烷交联的单组份层合粘合剂 - Google Patents

硅烷交联的单组份层合粘合剂 Download PDF

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Publication number
CN102712732B
CN102712732B CN201080061460.5A CN201080061460A CN102712732B CN 102712732 B CN102712732 B CN 102712732B CN 201080061460 A CN201080061460 A CN 201080061460A CN 102712732 B CN102712732 B CN 102712732B
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weight
tackiness agent
film
package adhesive
prepolymer
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CN102712732A (zh
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H-G·金策尔曼
P·根特舍韦
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Henkel AG and Co KGaA
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Henkel AG and Co KGaA
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Abstract

本发明涉及可交联的单组分层合粘合剂，其包含：25重量%-80重量%的含有至少2个可交联的烷氧基硅烷基且分子量为2000-30000g/mol的聚酯预聚物、聚醚预聚物和/或聚氨酯预聚物，75重量%-19重量%的沸点最高达130°C的有机溶剂，1重量%-20重量%的包含酸酐基的聚合物，以及0重量%-15重量%的添加剂，其中所述粘合剂的粘度在15-45°C测得为50-20000mPas(按照DIN？ISO？2555)。

Description

硅烷交联的单组份层合粘合剂
技术领域
本发明涉及用于粘合平坦基材的基于包含可水解硅烷基的聚氨酯预聚物的粘合剂。本发明还涉及此粘合剂作为多层膜的层合粘合剂的用途。
背景技术
在EP0464483中得知作为多元醇与异氰酸酯的反应产物的透明NCO-交联单组分粘合剂，其中使用包含脲基的异氰酸酯。这些脲基形成许多氢键，由此通常是高粘度聚合物。此外，单体异氰酸酯在制备聚合物时产生了必须通过附加措施减少的有害的异氰酸酯残余单体含量。
此外，US5990257是已知的。这描述制备含有硅烷基的聚氨酯的方法，其中相对于多元醇使用低于化学计量的异氰酸酯。其它OH基团则与异氰酸酯基硅烷反应形成含硅烷基的预聚物。聚合物的分子量大于12000g/mol。粘度大于57Pa.s。作为应用，描述用作密封剂的用途，其应在固化后表现出低粘性。
尚未公布的DE102009026900描述包含作为溶剂的醇的层合粘合剂。为此，描述基于聚氨酯的预聚物，其包含可交联的硅烷基。但是，这些粘合剂含有高含量的醇，例如，甲醇或乙醇。
此外，EP1674546是已知的。在其中，描述湿气固化的组合物，其由含NCO基的聚氨酯与亲核取代的硅烷反应而得。描述这些粘合剂与湿气的快速反应。该粘合剂用作热熔性粘合剂，即它们在室温下为固体并且仅趁热施用。
现有技术的组合物当用作层合粘合剂时具有各种缺点。含异氰酸酯的粘合剂就职业健康和安全而言通常被视为不安全。此外，仅可在严格无水的条件下储藏。硅烷固化系统包含羧酸或醇，或者在交联过程中形成它们。这些同样在生理上有害，而且这些物质还可能对膜包装的内容物有负面影响。
因此，本发明的目的是提供在室温下粘度低的粘合剂，其可以以薄层被涂布于大面积基材上。它应表现出对基材良好的粘附性和快速发生粘合。在交联后，若可能，粘合剂层不应具有任何可转移的生理上有害的组分，例如，伯芳香族胺或醇。
发明内容
本发明通过可交联的单组分层合粘合剂实现，其包含25重量%-80重量%的含有至少2个可水解的烷氧基硅烷基并且预聚物分子量为2000-30000g/mol的聚酯预聚物、聚醚预聚物和/或聚氨酯预聚物、75重量%-20重量%沸点最高达130°C的有机溶剂、1重量%-20重量%含酸酐基的聚合物、低聚物和/或单体、0重量%-15重量%添加剂，所述粘合剂的粘度在15-45°C(按照DINISO2555)测得为50-20000mPas。
适合用于制备本发明的预聚物的聚酯是已知的聚酯多元醇，例如，聚酯多元醇或聚氨酯多元醇形式，使其在至少2个位点与含有与聚合物骨架反应的基团及至少1个可交联的硅烷基的双官能的硅烷化合物反应。具体地，所述聚酯多元醇应具有大于/等于2个OH基团。
适合的聚酯多元醇可通过例如缩聚制得。例如，双官能和/或三官能的低分子量醇可与低于化学计量的二元羧酸和/或三元羧酸缩合。不用游离的多元羧酸，还可使用相应的多元羧酸酐或相应的多元羧酸酯与优选的含有1-3个C原子的醇。适合的二元羧酸是，例如，琥珀酸、己二酸、辛二酸、壬二酸、癸二酸及其含有最多达16个C原子的较高级的同系物，以及不饱和二元羧酸，例如马来酸或富马酸，二聚体脂肪酸或三聚体脂肪酸或者芳香族二元羧酸，特别是苯二甲酸异构体如邻苯二甲酸、间苯二甲酸或对苯二甲酸，酸酐例如四氢邻苯二甲酸酐、六氢邻苯二甲酸酐、戊二酸酐、马来酸酐、或者两种或更多种此类酸的混合物。作为可任选地部分添加的三元羧酸，适合的是，例如柠檬酸或偏苯三酸。选择数量以获得末端OH-官能的聚酯二醇。在一个优选的实施方案中，包含脂肪族和芳香族羧酸的混合物。
适合与上述羧酸反应的具体是脂肪醇。适合的脂肪醇包括，例如，乙二醇、丙二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、1,7-庚二醇、1,8-辛二醇及其高级同系物或异构体，1,4-羟基甲基环己烷、2-甲基-1,3-丙二醇、三乙二醇、乙二醇、聚乙二醇、二丙二醇、聚丙二醇、二丁二醇和聚丁二醇
适合的还有多官能的醇，例如丙三醇、三羟甲基丙烷、季戊四醇、新戊二醇和所述物质自身的低聚醚或者两种或更多种所述醚的混合物。
适合用于制备所述聚酯的多元醇还有低分子量多官能醇与环氧烷烃的反应产物，所谓的聚醚。所述环氧烷烃优选含有2-4个C原子。适合的实例是乙二醇、丙二醇、丁二醇异构体、己二醇或4,4'-二羟基二苯基丙烷与环氧乙烷、环氧丙烷或环氧丁烷或者其两种或更多种的混合物的反应产物。适合的还有多官能醇如丙三醇、三羟甲基乙烷或三羟甲基丙烷、季戊四醇或糖醇或者其两种或更多种的混合物与所述环氧烷烃形成的反应产物聚醚多元醇，这些应具有约400-约2000g/mol的分子量。
适合的还有聚酯多元醇，其通过低分子量醇特别是乙二醇、二乙二醇、新戊二醇、己二醇、丁二醇、丙二醇、丙三醇或三羟甲基丙烷与内酯特别是己内酯反应制得。适合的醇还有1,4-羟甲基环己烷、2-甲基-1,3-丙二醇、1,2,4-丁三醇、三乙二醇、四乙二醇、聚乙二醇、二丙二醇、聚丙二醇、二丁二醇和聚丁二醇。
但是，还可使用石油化学来源的聚酯多元醇。石油化学的多元醇应理解为是指基于天然的油和脂肪的多元醇，例如，环氧化的脂肪物质与单官能的、双官能的或多官能的醇的反应产物，或者至少部分被羟基取代的长链脂肪酸的丙三醇酯。此类聚酯多元醇可通过例如含有至少部分烯键式不饱和的脂肪酸的脂肪混合物的环氧化的甘油三酯与一种或多种含有1-12个C原子的醇完全开环，而后甘油三酯衍生物部分酯交换形成在烷基残基中含有1-12个C原子的烷基酯多元醇进行制备。其它适合的多元醇是聚碳酸酯多元醇和二聚体二醇(Henkel)以及蓖麻油及其衍生物。
制备此类OH-官能的聚酯的方法是已知的。此类聚酯多元醇也可商购获得。
适合用作聚合物骨架的另一类多元醇是聚醚多元醇。适合作为聚醚多元醇的是二元醇或三元醇如乙二醇、1,2-丙二醇或1,3-丙二醇、1,4-丁二醇或1,3-丁二醇、1,6-己二醇、1,8-辛二醇、新戊二醇、1,4-羟基甲基环己烷、2-甲基-1,3-丙二醇、丙三醇、三羟甲基丙烷、1,2,6-己三醇与环氧烷烃如环氧丙烷或环氧丁烷的已知反应产物。这些多元醇可含有2或3个OH基。此类聚醚多元醇可商购获得。
适合的多元醇的分子量应为约400-25000g/mol(数均分子量MN,通过GPC测定)，特别是2000-20000g/mol。若使用多元醇的混合物来制备所述预聚物，优选地应使用至少50%的聚酯多元醇，特别是全部聚酯多元醇，特别优选含有末端OH基的聚酯二醇。
在一个实施方案中，包含NCO基的预聚物可通过使上述聚酯和/或聚醚多元醇与过量的二异氰酸酯反应制得。在此，使多元醇以液态或熔解形式，任选地还含有溶剂，与二异氰酸酯反应。这还可通过升高的温度实施，还已知可添加少量的催化剂。通过选择异氰酸酯和用量，可确保在反应混合物中仅含有小比例的游离的未被反应的二异氰酸酯。若需要，还可通过蒸馏分离过量的单体异氰酸酯。这样的方法是本领域技术人员已知的。在此情况中，聚酯可仅包含末端NCO基，或者通过分子量增加形成含有反应性NCO基的聚氨酯预聚物。这些聚氨酯预聚物也适合用于合成用于本发明的含有硅烷的预聚物。
作为异氰酸酯，更具体地，适合的有已知的脂肪族或芳香族二异氰酸酯，例如，1,6-己二异氰酸酯(HDI)、1-异氰酸基-3,3,5-三甲基-5-异氰酸基甲基环己烷(IPDI)、二甲苯二异氰酸酯(XDI)、四甲基苯二甲基二异氰酸酯(TMXDI)、2,4-甲苯二异氰酸酯或2,6-甲苯二异氰酸酯(TDI)、2,4'-二苯基甲烷二异氰酸酯、2,2'-二苯基甲烷二异氰酸酯或者4,4'-二苯基甲烷二异氰酸酯(MDI)以及其异构体混合物，环己基二异氰酸酯(CHDI)、氢化苯二甲基二异氰酸酯(hexahydroxylylenediisocyanate,HXDI)、间苯二甲基二异氰酸酯(XDI)、萘二异氰酸酯(NDI)或亚联甲苯基二异氰酸酯(bitolylenediisocyanate,TODI)。选择数量从而获得NCO封端的预聚物。
在本发明的一个实施方案中，这些含NCO基的反应产物而后与包含可水解的硅烷基和亲核基团的硅烷反应。
作为适合的硅烷，使用有机官能的硅烷，例如具有以下通式的羟基官能的、巯基官能的、或者氨基官能的硅烷
Nu-(烷基-Si(R2)a(OR1)b)c，
其中Nu=NH、NH2、SH、OH
烷基=C1、C2、C3、C4、C6直链或支链的烷基或环烷基
R2=甲基、乙基、丙基、丁基，
a=0、1，
R1=含有1-20个C原子的烷基或H
B=2、3，
C=1、2。
所述硅烷基应包含至少1个，优选2或3个可水解的基团。具体地，适合的是C1-C6醇或OH基。在硅原子上可单独地或混合地包含这些基团。此外，在硅原子上可包含0或1个烷基，特别是甲基、乙基、丙基或丁基。具体地，适合的是，含有甲氧基、乙氧基、丙氧基或丁氧基的三烷氧基硅烷或二烷氧基硅烷。
巯基官能的硅烷的实例是3-巯基丙基三甲氧基硅烷、3-巯基丙基三甲氧基硅烷，或者相应的烷基二甲氧基或烷基二乙氧基化合物。氨基官能的硅烷的实例是：3-氨基丙基三甲氧基硅烷(AMMO)、3-氨基丙基三乙氧基硅烷(AMEO)、3-氨基丙基甲基二甲氧基硅烷、3-氨基丙基甲基二乙氧基硅烷、N-(2-氨基乙基)-3-氨基丙基三甲氧基硅烷(DAMO)、N-(2-氨基乙基)-3-氨基丙基三乙氧基硅烷、N-(2-氨基乙基)-3-氨基丙基甲基二甲氧基硅烷、N-(2-氨基乙基)-3-氨基丙基甲基二乙氧基硅烷、N,N-二(2-氨基乙基)-3-氨基丙基三甲氧基硅烷、N,N-二(2-氨基乙基)-3-氨基丙基三乙氧基硅烷、N,N-二(2-氨基乙基)-3-氨基丙基甲基二甲氧基硅烷、N,N-二(2-氨基乙基)-3-氨基丙基甲基二乙氧基硅烷、N-(2-氨基乙基)-N'-(2-氨基乙基)-3-氨基丙基三甲氧基硅烷、N-(2-氨基乙基)-N'-(2-氨基乙基)-3-氨基丙基三乙氧基硅烷、N-(2-氨基乙基)-N'-(2-氨基乙基)-3-氨基丙基甲基二甲氧基硅烷、N-(2-氨基乙基)-N'-(2-氨基乙基)-3-氨基丙基甲基二乙氧基硅烷)、双(三乙氧基甲硅烷基丙基)胺、双(三甲氧基甲硅烷基丙基)胺、N-(2-氨基丁基)-3-氨基丙基三乙氧基硅烷、N-(2-氨基丁基)-3-氨基丙基三甲氧基硅烷、N-(正丁基)-3-氨基丙基三甲氧基硅烷、N-(正丁基)-3-氨基丙基三乙氧基硅烷、N-(正丁基)-3-氨基丙基烷氧基二乙氧基硅烷、3-羟基丙基三甲氧基硅烷、3-羟基丙基三乙氧基硅烷、4-羟基丁基三甲氧基硅烷或其混合物，以及以其它烷基替代各自的丙基的相应的化合物。一个实施方案使用氨基硅烷与异氰酸酯预聚物反应，特别是α-官能化的硅烷，特别优选α-氨基硅烷。还可使用若干种硅烷的混合物。
选择要反应的硅烷化合物的量以使所述预聚物的所有异氰酸酯基与所述硅烷化合物的亲核基团反应。可使用稍微过量的亲核性硅烷。如此可确保在硅烷封端的预聚物中没有游离的异氰酸酯基。应避免过度过量的硅烷以使低分子量化合物的含量小。
本发明的另一个实施方案使上述OH-官能的聚酯和/或聚醚作为聚合物骨架与上式的硅烷反应，条件是Nu是异氰酸酯基。在此情况中，此硅烷化合物则包含可水解的基团和异氰酸酯基。这样的硅烷的实例是：三甲氧基甲硅烷基丙基异氰酸酯、三甲氧基甲硅烷基戊基异氰酸酯、三甲氧基甲硅烷基丁基异氰酸酯，或者相应的三乙氧基或三丙氧基化合物。适合的还有相应的二烷氧基烷基甲硅烷基异氰酸酯化合物。
选择异氰酸酯基硅烷化合物的量以使异氰酸酯基的摩尔量相当于羟基官能的多元醇的OH基的摩尔量。在此情况中，还获得硅烷官能的预聚物。
另一个实施方案选择上述聚合物作为聚合物骨架，从而它们包含可与硅烷化合物反应的官能团，除了可水解基团之外，它们还含有环氧基或酸酐基。在此情况中，聚合物，特别是多元醇，而后通过酯基或缩水甘油基醚与可水解的硅烷基相连。
适合于本发明的预聚物必须含有可交联的硅烷基。每分子的可水解的硅烷基数应为至少2或更多。在一个特定的实施方案中，硅烷基在聚合物链的末端。预聚物应优选地没有NCO基。
适合于本发明的反应产物是包含硅烷基的预聚物。这些预聚物平均含有2或更多个氨基甲酸酯基，优选2-4个。无溶剂形式的反应产物的玻璃转化温度应为-40至0℃，特别是-35℃至-10℃(用DSC测定)。玻璃转化温度可受到聚合物骨架或异氰酸酯的芳香族部分的量的影响。已表明，特别适合的是以含有芳香环的异氰酸酯为基础制得的反应性硅烷预聚物。这些的实例是与原料多元醇反应的TDI、NDI、4,4'-MDI、2,4-MDI、MXDI或TMXDI。
从上述硅烷官能化的预聚物可配制层合粘合剂。这些层合粘合剂可包含额外的组分，例如溶剂、增塑剂、催化剂、稳定剂、粘合促进剂，并且在一个较不优选的实施方案中，包含颜料和填充剂。
根据本发明，单组分层合粘合剂还必须包含具有可与醇反应的官能团的化合物。在此情况中，优选地，醇与所选化合物的反应性基团之间的反应是加成反应。优选地，在此反应中应不释放低分子量物质。特别适合作为官能团的是有机羧酸的酸酐。这些可以是单体羧酸酐，特别是在30°C为固态的那些，例如马来酸酐(MA)、邻苯二甲酸酐、苯均三甲酸酐或者此类化合物的衍生物。还可使用包含多于1个有机酸酐基团的化合物的低聚物。
本发明的一个特别的实施方案使用分子量大于1000g/mol的含有酸酐基的聚合物。适合的聚合物是已知的，特别是含有MA基的那些。这些可通过共聚被插入相应的聚合物中；MA还可被接枝在聚合物上。适合的共聚物的实例是MA与苯乙烯、乙酸乙烯酯或(甲基)丙烯酸酯的共聚物。可用MA接枝的共聚物的实例是聚丙烯、聚苯乙烯、聚酯或聚丁二烯的基础聚合物。这些在聚合物-类似反应中制备它们后可通过已知的方法用MA接枝。MA在适合的聚合物中的含量可占酸酐基的3mol%至约60mol%。根据本发明，有利的是所述聚合物中含有较高比例的MA，特别是10mol%-55mol%。
一个特别优选的实施方案使用MA-苯乙烯共聚物。这些含有20mol%-55mol%含量的MA。这些是固体物质。
相对于所述层合粘合剂，所述聚合物或低聚物的量应为1重量%-20重量%，特别是2重量%-15重量%。可选择其量以使酸酐基的量相当于本发明的粘合剂中的烷氧基的量。还可过量使用。具有可额外存在的亲核基团的任何低分子量物质，例如含胺的化合物，也可与此组分反应。
作为所述粘合剂中任选包含的其它添加剂，可包含，例如增塑剂。适合的增塑剂是例如，医用白油、环烷烃矿物油、石蜡烃油、聚丙烯、聚丁烯、聚异戊二烯低聚物、氢化聚异戊二烯和/或聚丁二烯低聚物、邻苯二甲酸酯、己二酸酯、苯甲酸酯、植物或动物油及其衍生物。作为可使用的稳定剂或抗氧化剂，可选择苯酚、高分子量的空间受阻的苯酚、多官能的苯酚、含硫的和含磷的苯酚或胺。
本发明的粘合剂还可包含颜料或填充剂。含量应为0-5重量%。所述粘合剂应优选是透明的。为此，纳米级填充剂特别适合。还可选择在所述粘合剂中具有适当折射率的填充剂，从而获得透明或仅稍微混浊的粘合剂。
还可向所述粘合剂添加硅烷化合物作为粘合促进剂。作为粘合促进剂，可使用上述硅烷或优选有机官能的硅烷，例如，(甲基)丙烯酰氧基官能的，环氧基官能的，或者非反应性取代的硅烷。在一个优选的实施方案中，将0.1重量%-3重量%的这样的硅烷添加至所述粘合剂。这些的实例是：3-丙烯酰氧基丙基三烷氧基硅烷或3-(甲基丙烯酰氧基)丙基三烷氧基硅烷；环氧基官能的硅烷，例如3-缩水甘油氧基甲基三甲氧基硅烷、3-缩水甘油氧基甲基三乙氧基硅烷、2-缩水甘油氧基乙基三甲氧基硅烷；乙烯基三甲氧基硅烷、烷基三乙氧基硅烷，或者相应的二烷氧基或三烷氧基衍生物。这些可任选地被插入聚合物网中。
本发明的适合的粘合剂还可包含催化剂作为可任选包含的额外的添加剂。可催化硅烷类的可水解基团的水解分裂以及从Si-OH产生硅氧烷类的后续缩合的所有已知的化合物可用作催化剂。这些的实例是：钛酸酯如钛酸四丁基酯或四乙酰丙酮酸钛；铋化合物如三(-2-乙基己酸)铋；羧酸锡(如二月桂酸二丁基锡(DBTL)、二乙酸二丁基锡或二(乙基己酸)二丁基锡、锡氧化物如二丁基氧化锡和二辛基氧化锡；有机铝化合物如三乙酰丙酮酸铝；螯合化合物如四乙酰丙酮酸锆；胺化合物或其与羧酸的盐，例如辛胺、环己基胺、苄胺、二丁基胺、单乙醇胺、二乙醇胺或三乙醇胺、三乙胺、三丙基胺、三丁基胺、二乙醇胺、二丙基胺、二丁基胺、二亚乙基三胺、三亚乙基四胺、三亚乙基二胺、胍、吗啉、N-甲基吗啉和1,8-二氮杂双环-(5,4,0)-十一-7-烯(DBU)；含有氨基的硅烷化合物。相对于配制物的总重量，催化剂或混合物的用量为0.01重量%-约5重量%。优选0.05重量%-4重量%，特别优选0.2重量%-3重量%的催化剂。优选地，所述粘合剂不包含任何锡催化剂。具体地，还可避免其它含重金属的催化剂。
根据本发明，所述粘合剂还包含溶剂。这些是可在最高达130°C的温度下蒸发的常规溶剂，特别是沸点低于100°C的溶剂。所述溶剂可选自：脂肪烃、芳香烃、酮或酯。所述溶剂用于降低和调整粘度。相对于所述粘合剂，溶剂的比例可在宽范围内变动，例如19%-75%。已知在一种交货形式中将粘合剂调整至高粘度；然后在应用前可用其它溶剂将其稀释至适合的粘度。所有组分的总和应为100%。为了良好的储藏稳定性，有用的是，本发明所用的溶剂仅包含少量水或没有水。
可在制备过程中添加本发明的粘合剂的溶剂。但是，另一个实施方案的操作方式是在制备过程中仅使用一定比例的溶剂，以将粘度调至适合于制备。但是，在本发明的组合物的情况中，为了获得适合的涂布粘度，在加工之前立刻将另一部分溶剂添加至粘合剂。在此实施方案中，直至应用所述粘合剂之前即刻添加的溶剂还可包含至少部分的有机单官能的醇。这些醇应符合所述溶剂的要求在低于130°C的温度下蒸发。特别适合的是甲醇、乙醇或丙醇。相对于溶剂总含量，醇的量应不大于50%，特别是小于25%。
已表明含有溶剂的粘合剂的加工稳定性足够长。持续长达6小时，可加工被稀释的粘合剂并且在交联过程中反应性没有显著变化。因为在应用过程中溶剂蒸发，未损及本发明的粘合剂的操作方式。
所述层合粘合剂的粘度在涂布温度下应该低。这可以最高达45°C，特别是最高达35°C。适合的层合粘合剂的粘度在15-45°C下测定应为50-20000mPas，优选100-5000mPas(按照ISO2555通过Brookfield方法测定)。为了应用通常用溶剂稀释所述粘合剂。在此粘度可以为50mPas-800mPas(在20-45°C下)。应用相关的测定应为12–28秒(Fordcup.4mm,ASTMD1200)。涂布制剂中的固体含量优选为15重量%-60重量%，特别优选30重量%-50重量%。由于需要快速进一步加工，所述粘合剂应快速交联并且产生良好的内聚性和粘附性。根据本发明，即使要粘合的基材仅有低含水量，涂布的粘合剂仍然可交联。这还可由所述粘合剂中的含水比例证明。
本发明的粘合剂在储藏时是稳定的。通常以低溶剂形式储藏。在此情况中，这可具有较高的粘度。在一个实施方案中，为了涂布，可加热这些溶剂减少的层合粘合剂而后涂布它们。在另一个实施方案中，用溶剂将粘合剂稀释至便于使用的低粘度，而后施用。
本发明的粘合剂的具体实施方案包括：
-单组分粘合剂，其中聚酯预聚物通过聚酯多元醇与摩尔过量的二异氰酸酯反应形成NCO聚酯预聚物而后该NCO预聚物的所有NCO基与包含烷氧基和亲核基团的双官能的硅烷化合物反应进行制备；
-单组分粘合剂，其中所述预聚物通过聚酯多元醇与NCO取代的烷基烷氧基硅烷反应制得；
-单组分粘合剂，其中聚醚预聚物通过聚醚多元醇与包含烷氧基和亲核基团的双官能的硅烷化合物反应制得；
-单组分粘合剂，其中还包含烷氧基硅烷作为粘合促进剂；
-单组分粘合剂，其中在全部溶剂中醇的量小于50重量%；
-单组分粘合剂不含有NCO基。
本发明还提供本发明的可交联的硅烷官能化的粘合剂用于制备多层膜的用途。作为用于制备多层膜的膜材料，可使用已知的柔性膜。这些是膜形式的热塑性聚合物基材，例如聚烯烃如聚乙烯(PE)或聚丙烯(PP、CPP、OPP)、聚氯乙烯(PVC)、聚苯乙烯(PS)、聚酯如PET、聚酰胺、有机聚合物如赛璐玢，以及金属箔或纸也可用作基材。这些膜材料还可通过例如用官能团改性聚合物、通过金属或氧化物涂层进行改性，或者所述膜中可包含额外的组分，例如颜料、染料或发泡层。它们可以是被染色的、印刷的、无色或透明的膜。
在本发明的用途中，利用适合于本发明的单组分粘合剂将两个或更多个相同或者特别是不同的膜粘合在一起。在本发明的一个实施方案中，膜可已经被印刷颜色而后涂布所述层合粘合剂。然后将本发明的液体层合粘合剂涂布于任选的经预处理的膜上。这可利用例如网纹辊或平压延辊通过本身已知的印刷法进行，或者通过喷嘴喷涂所述粘合剂，或者利用狭缝式喷嘴涂布所述粘合剂。根据所述粘合剂的粘度选择涂布方法。
通过选择本发明的可交联的单组分层合粘合剂，可获得低涂布粘度。适合于本发明的粘合剂具有低粘度，因此可涂布1-25μm，特别是2-15μm低的层厚度。
通过连接涂有所述粘合剂的膜与第二膜制得多层膜。可粘合两个被涂布的膜，但较不优选。可在压力和升高的温度下进行粘合。若干膜可任选地也被粘合在一起。这样的层合方法是本领域技术人员已知的。
本发明的粘合剂可特别地用作层合粘合剂。在此，所述粘合剂以薄层被涂布于膜上。其后立即蒸发所含的溶剂，而后将第二模涂布于粘合剂层上并利用压力压制。使用本发明的组合物时，还可使用一定比例的低分子量醇例如甲醇、乙醇或丙醇作为溶剂。根据食品管理法规，这些比其它溶剂有害性较小。在涂布步骤中醇快速蒸发。仅少量的残余醇或来自交联反应的那些被所含的含有酸酐基团的低聚物/聚合物捕获。利用本发明的操作模式，由此可减少和避免其它溶剂。
选择通过烷氧基硅烷基交联，所述粘合剂可快速交联。反应没有形成气泡，在高度反应性系统在基于异氰酸酯的粘合剂中难以避免。本发明的粘合剂的优点是所需的溶剂不必被干燥。因此，简化了本发明的粘合剂的制备、储藏和涂布方法。本发明的层合粘合剂的另一优点是它的良好柔性。已表明本发明的粘合剂具有预定的Tg。这些粘合剂即使在交联前也表现出粘合多层膜的良好的内聚性。
交联的粘合剂的Tg应为-15至+30°C，特别是-10至+20°C。以10K/分钟的加热速度从0被加热至200°C的小于0.5g的完整粘合剂的样品被视为无溶剂的交联状态。然后可通过DSC(差示扫描量热法)测定交联材料的Tg。
通过选择硅烷官能的预聚物，同时可确保被粘合的膜之间良好的瞬时粘性。在涂布步骤中溶剂蒸发。在本发明的单组分粘合剂交联过程中形成醇。这些与所含的含有MA基的额外的聚合物/低聚物缓慢反应，于是挥发性可提取或可迁移的醇的含量显著降低。交联速度受到额外的聚合物的积极影响，并且从反应系统除去醇。
本发明还提供用本发明的适合的层合粘合剂粘合的多层膜，其中例如已知的聚丙烯、聚乙烯、聚酯、PVC、聚酰胺等的塑料膜可用作基材。在此膜上，用本发明的粘合剂制备连续层，其在涂布后立即与相同或不同的第二膜粘合。除了双层膜之外，还可通过其它步骤制备多层膜。本发明的一个实施方案粘合透明膜，在此情况中有用的是本发明的粘合剂也是澄清的并且没有变色。
这些多层膜中还可包含其它层，例如包括纸、金属箔或其它阻挡层。这些多层膜在粘合后还可立即被进一步加工，因为存在高初始粘性和快速交联。不需要耗时的储藏同时等待交联或副反应。
本发明的粘合剂表现出不同层之间良好的粘附性。具体地，它是无色且透明的。在粘合剂层中没有出现气泡或缺陷。因此，它特别适合作为层合粘合剂用于粘合膜形式的柔性基材。此外，在交联时形成的醇被含有酸酐基的聚合物捕获。这产生不能够迁移的高分子量反应产物。因此，获得交联的粘合剂层，其仅包含少量的能够迁移的物质。因此，这样的多层膜特别适合用于包装工业，例如用于制备食品或医学产品的包装。
具体实施方式
实施例
实施例聚酯1：
由己二酸和间苯二甲酸及乙二醇制备聚酯。
聚酯的分子量为约2000g/mol。OH值为约58，酸值小于2。
实施例聚酯2：
从己二酸、间苯二甲酸、壬二酸和邻苯二甲酸及二乙二醇、乙二醇、丙二醇和新戊二醇制备聚酯。
聚酯的分子量为5100g/mol。聚酯的OH值为约22。
粘合剂的实施例
实施例3a：
将51.5份聚酯1溶于38.5份乙酸乙酯中，然后与6份TDI80反应。而后加入4.3份双(3-三乙氧基硅烷基丙基)胺。
所得产品的固体含量为62%。它不再包含异氰酸酯基。粘度约1400mPas(20°C)。Tg(交联)为-2°C。
实施例3b：
向实施例3a的粘合剂添加1.6份(相对于固体约2.5%)的包含约50重量%MA结构单元的苯乙烯共聚物，使混合物均匀。
实施例4a：
将63.0份聚酯2溶于30.0份乙酸乙酯中，然后与3.45份TDI100和4.15份双(3-三乙氧基甲硅烷基丙基)胺反应。
所得产物的固体含量为70%。它不再包含异氰酸酯基。粘度为约7750mPas(20°C)。
Tg(交联的)为+4°C。
实施例4b：
向实施例4a的粘合剂添加1.7份(相对于固体约2.5%)的包含约50重量%MA结构单元的苯乙烯共聚物，使混合物均匀。
实施例5a：
将61.2份聚酯2溶于34.5份乙酸乙酯中，然后与5.0份TDI100和1.4份n-环己基氨基甲基甲基二乙氧基硅烷。所得产物的固体含量为65%。它不再包含异氰酸酯基。粘度为约6700mPas(20°C)。
实施例5b：
向实施例5a的粘合剂添加3.5份(相对于固体约5%)的包含约50重量%MA结构单元的苯乙烯共聚物，使混合物均匀。粘度为约6800mPas(20°C)。
实施例5c：
向实施例5a的粘合剂添加2份(相对于固体约3%)的邻苯二甲酸酐，使混合物均匀。粘度为约6700mPas(20°C)。
在涂布前用乙酸乙酯将所有的粘合剂(系列1)稀释至约31%的固体含量。
粘度在此小于800mPas(20°C)。
用乙酸乙酯/乙醇的混合物稀释实施例3a、3b、5a、5b的粘合剂，从而溶剂中包含总计10%的乙醇(系列2)，固体含量约33%。
粘合：
利用刮刀将本发明的测试系列1的粘合剂涂布于基于聚乙烯(PE)的膜。层厚度为5μm。
以10μm的层厚度相似地涂布另一膜。在30°C下将涂布的表面风干约1min。然后利用辊将基于OPP的第二膜挤压在各涂布膜上。
利用刮刀以3g/m2的层厚度将来自测试系列2的粘合剂涂布于PET膜。在风干后，将这些膜与Al箔粘合。
在6天和14天后，测定膜基材的粘合。在所有情况中，测得彼此间良好的粘附性。
对粘合的膜，在24小时后，通过顶空GC测定乙酸乙酯和乙醇的含量。
试验表明，随着添加含有MA的组分，醇含量降低。
试验表明，不论溶剂中EtOH的比例，粘合膜的测得值仍然降低。这些粘合剂的加工稳定性也足够长，维持了减少醇的效果。

Claims (14)

1.用于粘合柔性多层膜的可交联的单组分粘合剂，其包含
a)25重量%-80重量%的选自聚酯预聚物、聚氨酯预聚物及其混合物的预聚物，其中所述预聚物含有至少2个可交联的烷氧基硅烷基，所述预聚物的分子量为2000-30000g/mol，其中至少50%的预聚物基于聚酯多元醇，
b)75重量%-19重量%的沸点最高达130℃的有机溶剂，其中所述有机溶剂是酯或酯和醇的组合，
c)1重量%-20重量%的包含一或多个酸酐基的聚合物和/或单体，
d)0重量%-15重量%的添加剂，
其中所述粘合剂的粘度按照DINISO2555在15-45℃测得为50-20000mPas，
其中所述含有酸酐基的聚合物和/或单体在25℃为固体并包含5mol%-60mol%的酸酐基，交联的粘合剂的玻璃化温度Tg为-15至+30℃，并且所有组分的总和为100重量%。
2.权利要求1的单组分粘合剂，其中所述包含一或多个酸酐基的聚合物是低聚物，所述低聚物在25℃为固体并包含5mol%-60mol%的酸酐基。
3.权利要求1的单组分粘合剂，其中所述聚酯预聚物或聚氨酯预聚物由包含至少2个OH基团且分子量为400-25000g/mol的聚酯多元醇制得。
4.权利要求1的单组分粘合剂，其中所述预聚物包含三烷氧基硅烷基。
5.权利要求1的单组分粘合剂，其中所述预聚物包含三乙氧基硅烷基或三甲氧基硅烷基。
6.权利要求1的单组分粘合剂，其中所述含有酸酐基的聚合物和/或单体具有环状酸酐基。
7.权利要求2的单组分粘合剂，其中所述低聚物具有环状酸酐基。
8.权利要求6的单组分粘合剂，其中所述粘合剂包含2重量%-15重量%的含有马来酸酐(MA)基的聚合物。
9.权利要求6的单组分粘合剂，其中所述粘合剂包含2重量%-15重量%的MA/苯乙烯共聚物或MA/(甲基)丙烯酸酯共聚物。
10.权利要求1的单组分粘合剂，其中所述粘合剂不含任何锡催化剂。
11.用于粘合柔性多层膜的方法，包括：
提供权利要求1的单组分粘合剂，
在所述单组份粘合剂中加入包含C1-C6醇的溶剂以获得所需的粘度，
在第一膜的表面上涂布粘度调整后的单组分粘合剂，
从第一膜的表面上的粘合剂中除去溶剂，和
将第二膜置于第一膜表面的粘合剂上。
12.柔性多层膜，其包含多个通过权利要求1的单组分粘合剂的固化反应产物而粘合在一起的选自聚合物膜、纸、箔中的膜。
13.柔性多层膜，其包含多个通过权利要求1的单组分粘合剂的固化反应产物而粘合在一起的选自纸、箔和经表面处理的膜中的膜。
14.权利要求12或13的柔性多层膜，其中所述箔是金属箔。
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