CN105637049A - 粘合到箔片的方法 - Google Patents
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Abstract
提供一种水性粘着剂组合物,其包含(i)含水介质;(ii)一种或多种分散于所述含水介质中的异氰酸酯化合物,和(iii)一种或多种分散于所述含水介质中的官能性硅烷化合物。还提供一种将金属箔片粘合到聚合物膜的方法,其包含以下步骤:(A)将水性粘着剂组合物的层涂覆到所述金属箔片的表面,(B)干燥所述粘着剂组合物的所述层以产生经干燥粘着剂的层,和(C)所述干燥后,使聚合物膜的表面与所述经干燥粘着剂组合物的所述层接触。
Description
粘着剂组合物的一个重要用途是粘合层压物的层。举例来说,经常需要提供可以将金属箔片粘合到聚合物膜的粘着剂组合物。因安全性和环境保护的原因,需要粘着剂组合物是水性的。使用水性粘着剂组合物以粘合层压物的层的所需方法是干燥粘合层压工艺,其为以下方法:将水性粘着剂组合物的层涂覆到第一衬底,随后将水性粘着剂组合物干燥或使其干燥,随后使第二衬底与经干燥粘着剂组合物接触,通常经由将两个衬底配合在一起并且形成层压物的热紧压夹。
US2010/0081742描述可以用于使沙粒和其它介质着色的水基有色聚氨基甲酸酯涂层。由US2010/0081742描述的涂层任选地含有交联剂,例如β-(3,4-环氧环己基)乙基三乙氧基硅烷。
需要提供一种使用水性粘着剂组合物来将金属箔片粘合到聚合物膜的方法。尤其需要提供一种使用水性粘着剂组合物的干燥粘合层压的方法,其中第一衬底是金属箔片并且第二衬底是聚合物膜。还需要的是能够使用是所述方法的水性粘着剂组合物。
以下是本发明的陈述。
本发明的第一方面是将金属箔片粘合到聚合物膜的方法,其包含以下步骤:
(A)将水性粘着剂组合物的层涂覆到所述聚合物膜或金属箔片的表面,
(B)干燥所述粘着剂组合物的所述层以产生经干燥粘着剂的层,和
(C)所述干燥后,使金属箔片或聚合物膜的表面与所述经干燥粘着剂组合物的所述层接触,
其中所述水性粘着剂组合物包含
(i)含水介质
(ii)一种或多种分散于所述含水介质中的异氰酸酯化合物,和
(iii)一种或多种分散于所述含水介质中的官能性硅烷化合物。
本发明的第二方面是一种水性粘着剂组合物,其包含
(i)含水介质
(ii)一种或多种分散于所述含水介质中的异氰酸酯化合物,和
(iii)一种或多种分散于所述含水介质中的官能性硅烷化合物
以下是本发明的详细描述。
如本文中所使用,除非上下文另作明确指示,否则以下术语具有所指定的定义。
金属箔片是长度和宽度各自是至少1cm并且厚度是0.5mm或小于0.5mm的一块金属。聚合物膜是由有机聚合物制成的长度和宽度各自是至少1cm并且厚度是0.5mm或小于0.5mm的一块材料。
如果组合物在25℃下是液体并且按组合物的重量计含有30重量%或大于30重量%的水,那么组合物在本文中称为水性的。水性组合物含有离散液滴或粒子可以任选地悬浮于其中的连续流体介质。连续流体介质含有水,其量按连续流体介质的重量计是50重量%或大于50重量%。连续流体介质在本文中称为含水介质。
含于水性组合物中的不为水的化合物在本文中称为分散于含水介质中。所述化合物可以经溶解或悬浮或其组合。悬浮化合物呈现为离散液滴或粒子;所述粒子可能含有两种或更多种物质。悬浮液滴或粒子的重量平均直径是5nm或大于5nm。溶解于含水介质中的化合物分散为个别分子。
异氰酸酯是含有一个或多个侧异氰酸酯基-NCO的化合物。每分子含有一个以上异氰酸酯基的异氰酸酯是聚异氰酸酯。恰好含有两个异氰酸酯基的异氰酸酯是二异氰酸酯。单体二异氰酸酯具有结构OCN-R1-NCO,其中-R1是二价有机基团,不具有异氰酸酯基的,不具有氨基甲酸酯键,并且分子量小于500。
多元醇是每分子具有两个或更多个-OH基团的化合物。二醇恰好每分子具有两个-OH基团。
如本文中所使用,着色剂是任何染料或颜料。着色剂可以是有机或无机的或其组合。
本发明的粘着剂组合物包含含水介质。优选地,含水介质中水的量按水的重量计是70重量%或大于70重量%;或80重量%或大于80重量%;或90重量%或大于90重量%。
本发明的粘着剂组合物含有一种或多种异氰酸酯化合物。优选地,粘着剂组合物含有一种或多种聚异氰酸酯。优选聚异氰酸酯是一种或多种氨基甲酸酯预聚物、一种或多种异氰酸酯三聚体以及其混合物。
异氰酸酯三聚体是单体二异氰酸酯的三聚体。优选的是亲水改性的异氰酸酯三聚体,其具有结构
其中三个R基团彼此相同,并且其中G是含有至少一个亲水性基团的有机基团。优选的R基团是脂肪族基;更优选的是正己基和二甲基环己基;更优选的是正己基。优选的亲水性基团是阴离子基团和亲水性环氧烷基团;更优选的是亲水性环氧烷基团。优选的亲水性环氧烷基团是-(CH2CH2O)n-,其中n是3到50。在阴离子基团之中,优选的是硫酸根和羧酸根;更优选的是硫酸根。
氨基甲酸酯预聚物是一种或多种聚异氰酸酯与一种或多种多元醇或一种或多种多元胺或其混合物的反应产物。在制备氨基甲酸酯预聚物中,使用摩尔过量的聚异氰酸酯,并且氨基甲酸酯预聚物是聚异氰酸酯。对于制备氨基甲酸酯预聚物,优选的聚异氰酸酯是单体二异氰酸酯,其分子量是300或小于300;更优选地275或小于275。对于制备氨基甲酸酯预聚物,优选的聚异氰酸酯是芳香族单体二异氰酸酯;更优选的是一种或多种MDI异构体;更优选的是4,4′-MDI和4,4′-MDI与其它MDI异构体的混合物;更优选的是4,4′-MDI。对于制备氨基甲酸酯预聚物,一种或多种聚异氰酸酯优选地与一种或多种多元醇反应。优选的多元醇的重量平均分子量是500或大于500;更优选地800或大于800。优选的多元醇的重量平均分子量是5000或小于5000;更优选地2500或小于2500。优选地,重量平均分子量小于800的多元醇不用于制备氨基甲酸酯预聚物。优选的多元醇是二醇。优选的多元醇是聚醚多元醇、聚酯多元醇以及其混合物;更优选的是聚醚多元醇。优选的聚醚多元醇是聚四亚甲基醚二醇、聚丙二醇以及其混合物。
优选的氨基甲酸酯预聚物制备为聚氨基甲酸酯分散体,其是氨基甲酸酯预聚物的粒子悬浮于含水介质中的组合物。
本发明的组合物含有一种或多种官能性硅烷。官能性硅烷是具有以下结构的化合物
其中A是氨基、环氧基、甲基丙烯酰基、乙烯基、巯基、脲或异氰酸酯基。基团-R1-是二价有机基团。优选地,-R1-是烃基;更优选地烷基;更优选地直链烷基,更优选地具有1到6个碳原子的直链烷基;更优选地具有2到4个碳原子的直链烷基。-R2、-R3和-R4中的每一个独立地是-O-R5或-R6,其中-R5和-R6中的每一个独立地是烷基;优选地具有1到6个碳原子的烷基;更优选地甲基、乙基或异丙基;更优选地甲基或乙基。优选地,-R2、-R3和-R4中的一个或多个是-O-R5;更优选地-R2、-R3和-R4中的两个或更多个是-O-R5。优选地,-R2、-R3和-R4中的两个或更多个彼此一致。
环氧基是含有环氧环的任何基团。环氧基包括例如环氧醚基和β-(3,4-环氧环己基)基团。环氧醚基具有结构
优选地,A-是环氧醚基、氨基或巯基。
优选地,官能性硅烷可溶于水中或可悬浮于水中。如果在25℃下一个或多个pH值在1与7之间,在所述pH值下可以溶解于水中的官能性硅烷的量按水的重量计是2重量%或大于2重量%,那么官能性硅烷在本文中视为可溶于水中。无论是否在官能性硅烷的溶解形式中,一个或多个-OR5基团转化成-OH基团,官能性硅烷在本文中视为可溶的。如果在25℃下2克或大于2克的官能性硅烷可以悬浮于100克水中,以形成在25℃下存放时不沉降或聚结24小时的悬浮液,那么官能性硅烷在本文中视为可悬浮。
优选地,水性粘着剂组合物不含有任何着色剂。也就是说,水性粘着剂组合物完全不含着色剂或含有以按组合物的总重量计0.1重量%或小于0.1重量%的量的着色剂。本文中认为,如果水性粘着剂组合物含有以按组合物的总重量计0.1重量%或小于0.1重量%的量的着色剂,那么组合物将含有此类少量的着色剂,着色剂的量视为可忽略,并且组合物被视为等效于不含有任何着色剂的组合物。
水性粘着剂组合物任选地含有一种或多种非氨基甲酸酯聚合物。优选的非氨基甲酸酯聚合物是乙烯基聚合物,其为含有烯系不饱和单体的聚合单元的聚合物。更优选的非氨基甲酸酯聚合物含有一种或多种丙烯酸单体、一种或多种乙烯基芳香族单体或其组合的聚合单元。丙烯酸单体是丙烯酸、甲基丙烯酸、其酯以及其酰胺。乙烯基芳香族单体包括苯乙烯和经取代苯乙烯。
当存在一种或多种非氨基甲酸酯聚合物时,所述聚合物的优选形式是如悬浮于含水介质中的粒子。
优选地,水性粘着剂组合物不含有任何乙烯基聚合物,所述任何乙烯基聚合物含有任何乙烯基硅烷单体的任何聚合单元。乙烯基硅烷单体是在其分子中具有可聚合的碳-碳双键和一个或多个硅原子的单体。
在本发明的实践中,水性粘着剂组合物的层优选地涂覆到金属箔片或聚合物膜的表面。更优选地,水性粘着剂组合物的层涂覆到金属箔片的表面。优选地,金属箔片是铝箔。优选地,金属箔片的厚度是1μm或大于1μm;更优选地3μm或大于3μm。优选地,金属箔片的厚度是25μm或小于25μm;更优选地15μm或小于15μm。
优选地,将水性粘着剂组合物的层干燥或使其干燥以形成经干燥粘着剂组合物的层。可以通过任何方法实现干燥,包括例如时间推移、施加热和曝露于流动空气中的一种或多种。当按水(作为水性粘着剂组合物的一部分而应用)的重量计,粘着剂组合物的层中剩余的水量是10重量%或小于10重量%时,粘着剂组合物的层被视为干燥的。
粘着剂组合物的干燥层优选地与聚合物膜或金属箔片的表面接触。更优选地,粘着剂组合物的干燥层与聚合物膜的表面接触。优选地,粘着剂组合物的干燥层使用将两个衬底配合在一起并且形成层压物的热紧压夹来使得与聚合物膜或金属箔片的表面接触。
用于聚合物膜的优选聚合物是有机聚合物和金属化有机聚合物;更优选的是聚烯烃、聚烯烃共聚物、聚酯、聚碳酸酯、聚酰胺以及其金属化膜。聚烯烃是烯烃单体的均聚物和共聚物,所述烯烃单体是含有一个或多个碳-碳双键的烃分子。聚烯烃共聚物是一种或多种烯烃单体的共聚物,所述烯烃单体具有一种或多种乙酸乙烯酯、丙烯酸酯单体和甲基丙烯酸酯单体。优选的聚合物是聚乙烯、聚对苯二甲酸乙二醇酯和尼龙;更优选的是聚乙烯。
聚合物膜与经干燥粘着剂组合物的层接触后,因此形成的复合物品优选地经历机械力以使聚合物膜和金属箔片压向彼此。所述机械力优选地通过在滚筒之间传送复合物品来施加。
在本发明的一些实施例中,由金属箔片、粘着剂组合物的层和聚合物膜制成的复合物品是含有其它层的较大复合物品的一部分。其它层可能含有一个或多个聚合物膜、粘着剂组合物的一个或多个层和一个或多个金属箔片;存在于其它层中的任何聚合物膜、粘着剂组合物或金属箔片可能彼此相同或不同,并且来自存在于上文所描述复合物品中的聚合物膜、粘着剂组合物和金属箔片。
举例来说,在一些实施例中,较大复合物品制备如下。将粘着剂组合物的第一层涂覆到聚对苯二甲酸乙二醇酯膜,并且使第一粘着剂组合物与金属箔片的一个表面接触。随后,在金属箔片的相反表面上,涂覆粘着剂组合物的第二层,并且使第二粘着剂组合物与聚乙烯的聚合物膜的表面接触。优选地,在所述实施例之中,粘着剂组合物的第一层和粘着剂组合物的第二层是本发明的水性粘着剂组合物的层,并且优选地每一层在与下一衬底接触前干燥。
以下是本发明的实例。
在实例中使用以下成分:
SPU1+CatF=AdcoteTM545-75EA(“SPU1”)加催化剂F(“CatF”)是来自陶氏化学公司(DowChemicalCompany)的双组分溶剂型粘着剂产品
乳胶“L”是ROBONDTML-168A,来自陶氏化学公司的水性乳胶共聚物;含有一种或多种丙烯酸单体的聚合单元。
异氰酸酯1=ROBONDTMCOREACTANTCR3A,来自陶氏化学公司的水可分散性脂肪族异氰酸酯三聚体
PTMEG1=TetrathaneTM2000聚四亚甲基醚二醇,MW=2000,来自英威达(Invista)。
PPG1=VaranolTMV9287A聚丙二醇,MW=2000,来自陶氏化学公司
PEG1=CarbowaxTMPEG1000聚乙二醇,分子量1000,来自陶氏化学公司
MPEG1=CarbowaxTMMPEG1000甲氧基聚乙二醇,分子量1000,来自陶氏化学公司
MDI=IsonateTM125M,来自陶氏化学公司
Surf1=RhodacalTMDS4表面活性剂,十二烷基苯磺酸钠,来自罗地亚(Rhodia)
箔膜是由中国(China)当地供应商供应的7μm铝箔
Ny是尼龙膜,15μm厚
PET是聚对苯二甲酸乙二醇酯膜,12μm厚
PE是聚乙烯膜,50μm厚
硅烷1=SilquestTMA1100γ氨基丙基三乙氧基硅烷,由迈图(Momentive)供应
硅烷2=SilquestTMA189巯基-丙基三甲氧基硅烷,由迈图供应
硅烷3=SilquestTMA187γ-(2,3-环氧丙氧基)丙基三甲氧基硅烷,由迈图供应
DI水是去离子水
成分如下用于实例。“Comp.”意指比较并且“Ex.”意指实例,“Ingr”意指成分并且“No.”意指编号。
为制备实例1和实例2以及比较实例10,在氮气净化下将成分No.1到No.4添加到1升玻璃瓶子中。随后添加成分No.5和7(如果使用),并且将瓶子缓慢地加热到约80℃。将瓶子保持在80℃下2到3小时;检验NCO含量,并且维持温度直到获得NCO含量的理论值。将所得预聚物放置在塑料瓶子中并且用考雷司(Cowles)桨叶在约3000rpm下搅拌。随后在高速搅拌下在冷温度(5℃)下将成分No.9、之后成分No.8添加到塑料罐中,以确保达到均质的水包油分散体,随后将成分No.6缓慢地添加到分散体中,并且继续搅拌以产生稳定的分散体。对于实例2和比较实例10,在逐滴添加成分No.10的同时用磁性旋转棒对分散体进行搅拌;随后继续搅拌30分钟。
Ingr.No. | 成分 | Ex.3 | Ex.4. | Ex.5. |
1a | 比较实例10 | 50g | 50g | 50g |
2a | 硅烷1 | 0.15g | 0 | 0 |
3a | 硅烷2 | 0 | 0.15 | 0 |
4a | 硅烷3 | 0 | 0 | 0.15 |
Ingr.No. | 成分 | Ex.6 | Ex.7 | Ex.8 | Comp.Ex.9 |
1b | 乳胶L | 50g | 50g | 50g | 50g |
2b | 硅烷1 | 0.15g | 0 | 0 | 0 |
3b | 硅烷2 | 0 | 0.15 | 0 | 0 |
4b | 硅烷3 | 0 | 0 | 0.15 | 0 |
5b | 异氰酸酯1 | 1g | 1g | 1g | 1g |
Ingr.No. | 成分 | Comp.Ex.11 |
1c | SPU1 | 90g |
2c | Cat F | 10g |
对于实例3、4、5、6、7、8、比较9和比较11,使用磁性旋转棒混合以上所展示的成分。
对于每个实例,使用K101控制涂布机(RKPrintCoatInstrumentsLtd.)将粘着剂混合物涂布于第一衬底上,以得到2.3g/m2的干燥涂层重量。将经涂布衬底放置在80℃下的烘箱中,持续30秒到2分钟以去除水。使第二衬底与干燥粘着剂接触,并且使用夹温是约68℃的热轧层压机HL-101(ChemInstruments,Inc.)形成层压物。在约23℃下将层压样品存放3-7,并且随后通过两个不同测试对粘着强度进行测试:粘合强度和沸点强度。
在粘合强度测试中,切割15mm宽的条带并且随后使用拉力测试仪以25cm/min剥离。记录最大剥离力并且以牛顿(Newton)单位报道。失效模式记录如下:
FF:无膜伸长情况下的膜失效(衬底在无伸长的情况下断裂)
FT:拉伸伸长下的膜撕裂(衬底伸长并且还断裂)
在袋中沸腾测试中,将固化层压物切成8cm×12cm大小,并且使用HSG-C热封机器(BruggerFeinmechanikGmbH)在140℃和300N/15mm压力的条件下制备成内部具有去离子水的袋子,持续1秒。避免将水喷溅于热封区域上。用不可消除的标记来标记热封区域或层压区域中任何明显的预先存在的缺陷。随后将袋子小心地放置于沸水中并且留在其中30分钟,确保所有袋子在整个沸腾过程期间始终浸没于水中。当完成时,记录隧穿、分层或泄漏的程度,与预先存在的缺陷进行比较。通过测试的样品将展示无超出任何预先存在的热封或层压缺陷的隧穿、分层或泄漏迹象。随后打开袋子,清空袋子并且使其冷却下来,随后切成15mm宽的条带,以使用InstronTM5943机器在25cm/min速度下测试T-剥离粘合强度。
测试结果如下。“Ex”是实例,“Comp”是比较,并且“nt”意指未测试。其中未展示失效模式,失效模式是粘着剂失效(当一个衬底上的粘着剂之间的粘合失效或粘着剂分裂时,样品失效,其中粘着剂层分裂)
粘合强度(牛顿和失效模式)
袋中沸腾(牛顿和失效模式)
粘合强度(牛顿和失效模式)
袋中沸腾(牛顿和失效模式)
尤其重要的是针对第一衬底是箔片并且第二衬底是PE的层压物的结果。本发明实例均比水性比较实例进行地更好。测试溶剂型比较实例(comp.Ex.11)以提供关于不为水性的粘着剂能力的信息。
对于所有其它衬底,本发明实例表明粘着强度的适用等级。
Claims (5)
1.一种将金属箔片粘合到聚合物膜的方法,其包含以下步骤:
(A)将水性粘着剂组合物的层涂覆到所述金属箔片的表面,
(B)干燥所述粘着剂组合物的所述层以产生经干燥粘着剂的层,和
(C)所述干燥后,使聚合物膜的表面与所述经干燥粘着剂组合物的所述层接触,其中所述水性粘着剂组合物包含
(i)含水介质
(ii)一种或多种分散于所述含水介质中的异氰酸酯化合物,和
(iii)一种或多种分散于所述含水介质中的官能性硅烷化合物。
2.根据权利要求1所述的方法,其中所述聚合物膜是聚烯烃。
3.根据权利要求1所述的方法,其中所述一种或多种异氰酸酯化合物包含一种或多种氨基甲酸酯预聚物,其中所述氨基甲酸酯预聚物包含4,4′-MDI与一种或多种多元醇的反应产物。
4.根据权利要求1所述的方法,其中所述一种或多种异氰酸酯化合物包含一种或多种亲水改性的异氰酸酯三聚体。
5.根据权利要求1所述的方法,其中所述水性粘着剂组合物另外包含一种或多种非氨基甲酸酯聚合物,所述非氨基甲酸酯聚合物包含一种或多种丙烯酸单体的聚合单元。
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EP3030621B1 (en) | 2021-02-17 |
EP3030621A1 (en) | 2016-06-15 |
US20160257796A1 (en) | 2016-09-08 |
JP6404919B2 (ja) | 2018-10-17 |
MX2016004746A (es) | 2016-07-26 |
AR097871A1 (es) | 2016-04-20 |
JP2016537453A (ja) | 2016-12-01 |
TWI565594B (zh) | 2017-01-11 |
EP3030621A4 (en) | 2017-04-26 |
US9605117B2 (en) | 2017-03-28 |
BR112016008310B1 (pt) | 2021-07-27 |
CN105637049B (zh) | 2020-04-17 |
TW201529327A (zh) | 2015-08-01 |
WO2015054821A1 (en) | 2015-04-23 |
RU2016118666A (ru) | 2017-11-17 |
RU2638394C2 (ru) | 2017-12-13 |
BR112016008310A2 (pt) | 2017-08-01 |
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