CN107603501B - 聚氨酯粘合膜 - Google Patents

聚氨酯粘合膜 Download PDF

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CN107603501B
CN107603501B CN201710646965.1A CN201710646965A CN107603501B CN 107603501 B CN107603501 B CN 107603501B CN 201710646965 A CN201710646965 A CN 201710646965A CN 107603501 B CN107603501 B CN 107603501B
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adhesive film
supporting adhesive
polyurethane
composite
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CN107603501A (zh
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F·D·马伊
B·W·卡尔森
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HB Fuller Co
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Abstract

要求保护薄自持性粘合膜，其包含第一聚氨酯和固体表面钝化异氰酸酯。

Description

聚氨酯粘合膜
本申请是申请日为2014年7月30日、申请号为201480003890.X、国际申请号为PCT/US2014/048876的名称为“聚氨酯粘合膜”的中国发明专利申请的分案申请。
相关申请的交叉引用
本申请要求2013年7月30日提交的并结合到本文中的美国临时申请No.61/860,006的权益。
背景
粘合剂通常用于将基质粘合在一起以保持两个基质彼此的固定关系。
基于聚氨酯分散体(PUD)的粘合剂可用固体表面钝化异氰酸酯配制。可将这类组合物预先应用于基质上并干燥，使得异氰酸酯仍未活化(即热保持在小于活化和固化所需的)。这赋予使用者选择稍后用热将异氰酸酯活化以形成粘合并引发聚氨酯与异氰酸酯之间的固化反应的可能性。
在生产环境中，便利的是粘合剂可作为薄自持性(self-supporting)粘合膜提供给最终使用者。最终使用者由此不必争抢应用和干燥粘合剂的设备和方法。
概述
一方面，本发明的特征是自持性粘合膜，其包含：
固体表面钝化异氰酸酯和大于70重量％第一聚氨酯，所述第一聚氨酯具有不大于约90,000的重均分子量(Mw)和至少约25J/g的熔化焓。
在一个实施方案中，自持性粘合膜由含水组合物得到。在另一实施方案中，固体表面钝化异氰酸酯衍生自甲苯二异氰酸酯。在又一实施方案中，所述第一聚氨酯的膜具有至少约35J/g的熔化焓。
在一个实施方案中，第一聚氨酯衍生自聚酯，所述聚酯衍生自选自1,4-丁二醇和1,6-己二醇的多元醇。在第二实施方案中，第一聚氨酯衍生自聚酯，所述聚酯衍生自己二酸以及1,6-己二醇和新戊二醇的混合物；和脂族异氰酸酯。
在不同的实施方案中，当根据粘合测试方法在约64℃的粘合层温度(bond linetemperature)下测试时，膜显示出至少约20N/2.5cm的粘合强度。在另一实施方案中，当根据粘合测试方法在约82℃的粘合层温度下测试时，膜显示出至少约30N/2.5cm的粘合强度。
在一些实施方案中，自持性粘合膜具有约1密尔至约8密尔的厚度。在其它实施方案中，自持性粘合膜进一步包含释放衬里。
在其它实施方案中，自持性粘合膜还包含第二聚合物。在一个实施方案中，固体表面钝化异氰酸酯、第一聚氨酯和第二聚合物的和总计为自持性粘合膜的至少约95重量％。
另一方面，本发明包括包含第一层和第二层的复合结构，第一层和所述第二层中的至少一个包含自持性粘合膜，其中自持性粘合膜包含固体表面钝化异氰酸酯和大于70重量％第一聚氨酯，所述第一聚氨酯具有不大于约90,000的重均分子量(Mw)和至少约25J/g的熔化焓。
在一个实施方案中，第一层包含自持性粘合膜且第二层为柔性的并选自织物、箔和纸。
另一方面，本发明的特征是包含自持性粘合膜、刚性层和柔性层的复合结构，其中刚性层通过自持性粘合膜粘合在柔性层上。在一些实施方案中，刚性层包含金属、金属复合物、塑料、塑料复合物、木材和木材复合物中的至少一种。在其它实施方案中，柔性层包含织物、箔和纸中的至少一种。在又另外的实施方案中，刚性层为尼龙且软织物层为微纤维。
另一方面，本发明的特征是制备复合物的方法，其包括使柔性层与自持性粘合膜的第一主表面接触，在将膜应用于柔性基质上以前和以后将热施加在膜上；使刚性层与自持性粘合膜的第二主表面接触，使得第二主表面与刚性层直接接触以形成复合物；和将热和压力施加在复合物上。
在不同的方面中，自持性粘合膜由含水组合物得到，所述含水组合物包含固体表面钝化异氰酸酯和第一聚氨酯分散体，其干燥膜具有至少约25J/g的熔化焓，其中自持性粘合膜具有约1密尔至约8密尔的厚度。在一个实施方案中，异氰酸酯衍生自芳族异氰酸酯。在不同的实施方案中，自持性粘合膜具有约2密尔至约6密尔的厚度。在另一实施方案中，得到包含自持性粘合膜、第一刚性层和第二刚性层的复合结构，其中刚性层通过自持性粘合膜彼此粘合。在又另外的实施方案中，复合结构包含自持性粘合膜、刚性层和柔性层，其中刚性层通过自持性粘合膜粘合在柔性层上。或者，自持性粘合膜包含第二聚合物。
术语
自持性粘合膜为不存在任何基质的粘合膜。
基质为使用粘合剂粘合或涂覆的最终材料。释放衬里不被认为是基质。
详述
发明人发现粘合剂组合物可作为具有或不具有释放衬里的自持性粘合膜提供给使用者。
膜包含异氰酸酯反应性聚合物和固体表面钝化异氰酸酯。异氰酸酯反应性聚合物为聚氨酯。就本申请而言，聚氨酯包括聚氨酯、聚脲和聚氨酯-脲。
申请人发现自持性粘合膜的薄层能够以低粘合层温度形成强初始粘合。这使制备各部分所需的时间最小化并提高生产线上的生产速度。
当根据粘合测试方法测试时，自持性粘合膜显示出至少约20N/2.5cm、至少约30N/2.5cms、至少约50N/2.5cms，或者甚至约15N/2.5cm至约90N/2.5cm的粘合强度。
含水组合物
自持性粘合膜可衍生自含水组合物，所述含水组合物包含含有第一聚氨酯分散体的第一聚合物和固体表面钝化异氰酸酯交联剂。第一聚氨酯分散体和固体表面钝化异氰酸酯交联剂可作为双组分体系分别提供，然后在形成膜以前混合，或者，可作为其中将两种已经混合的单组分体系提供。
第一聚氨酯分散体
有用的第一聚氨酯分散体包含阴离子聚氨酯分散体。第一聚氨酯具有一定的结晶度和足够低以使得容易活化的熔融峰。结晶度的一个有用指示是熔化焓—化合物的熔化焓越高，它的结晶度越高。测定聚氨酯的熔化焓(ΔH)和熔融峰的有用方法利用了使用PYRIS1DSC以10℃/分钟的加热速率进行的差示扫描量热法(DSC)。
干燥第一聚氨酯优选具有至少约15焦耳/克(J/g)、至少约25J/g、至少约35J/g，或者甚至约15J/g至约70J/g的熔化焓。干燥第一聚氨酯优选具有不大于约65℃、不大于约60℃，或者甚至不大于约55℃的熔融峰。
第一聚氨酯具有较低的重均分子量(Mw)。优选地，第一聚氨酯具有不大于约90,000、不大于约85,000，或者甚至不大于约80,000的分子量。
第一聚氨酯衍生自至少一种二醇、多元醇或其组合，和至少一种二-和或多异氰酸酯。
有用多元醇的实例包括部分衍生自脂族二醇的聚酯多元醇，所述脂族二醇的有用实例包括乙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇和新戊二醇。在一个实施方案中，第一聚氨酯部分衍生自部分衍生自1,4-丁二醇或1,6-己二醇的聚酯多元醇。
其它有用的聚酯多元醇衍生自线性二羧酸和/或其衍生物(例如酐、酯和酰氯)，和脂族、脂环族、线性和支化多元醇，及其组合。在一个实施方案中，第一聚氨酯衍生自衍生自二羧酸的聚酯多元醇，所述二羧酸选自己二酸、琥珀酸、癸二酸和十二烷二酸(dodecanedioic diacid)。
在另一实施方案中，第一聚氨酯衍生自基于己二酸和1,4-丁二醇的聚酯多元醇，或者基于己二酸和1,6-己二醇的聚酯多元醇，或者基于己二酸以及1,6-己二醇和新戊二醇的混合物的聚酯多元醇。
有用的二-和多异氰酸酯包括例如每个分子中具有至少2个自由(free)异氰酸酯基团的任何有机化合物。优选的二异氰酸酯包括例如脂族二异氰酸酯(例如六亚甲基二异氰酸酯(HDI)、1-异氰酸酯-3,3,5-三甲基-5-异氰酸酯甲基-环己烷(1-isocyanto-3,3,5-trimethyl-5-isocyanatomethyl-cyclohexane,IPDI))及其组合。
第一聚氨酯可作为一种聚氨酯或者作为两种或更多种聚氨酯的混合物存在。
干燥自持性粘合膜包含至少约30重量％、至少约50重量％、至少约70重量％、至少约80重量％、约30重量％至约97重量％第一聚氨酯，或者甚至约50重量％至约95重量％第一聚氨酯。
有用的市售第一聚氨酯分散体包括例如DISPERCOLL U XP 2682、DISPERCOLL U56和DISPERCOLL U 2815XP，其都可由德国的Bayer Material Science AG得到，和WD4047，其可由HB Fuller Company(St.Paul，MN)得到。
固体表面钝化异氰酸酯交联剂
含水组合物包含固体表面钝化异氰酸酯交联剂。有用的固体表面钝化异氰酸酯交联剂衍生自多异氰酸酯和钝化剂。多种多异氰酸酯是合适的，包括例如脂族、脂环族、杂环和芳族多异氰酸酯(例如亚甲基二苯基二异氰酸酯(MDI)、甲苯二异氰酸酯(TDI)和异佛尔酮二异氰酸酯(IPDI))，以及例如US 6,348,548B1中公开的那些多异氰酸酯，通过引用将其并入本文中。衍生自芳族异氰酸酯的表面钝化异氰酸酯是优选的，因为它们比脂族异氰酸酯更快地反应，从而使得在低粘合层温度下形成强初始粘合。
多种钝化剂是合适的，包括例如伯和仲脂族胺、二胺、多胺、肼衍生物、脒、胍及其组合。钝化剂的有用实例包括乙二胺、1,3-丙二胺、二亚乙基三胺、三亚乙基四胺、2,5-二甲基-哌嗪、3,3'-二甲基-4,4'-二氨基-二环己基甲烷、甲基壬二胺、异佛尔酮二胺、4,4'-二氨基二环己基甲烷、二氨基和三氨基聚丙烯醚、聚酰胺胺及其组合，以及US 6,348,548 B1中公开的那些钝化剂。
有用的固体表面钝化异氰酸酯交联剂可以以多种方法制备，包括US 6,348,548B1中所述那些方法。
固体表面钝化异氰酸酯交联剂可以为多种形式，包括例如含水悬浮液和微米化(micronized)颗粒。
有用的市售固体表面钝化异氰酸酯包括例如包含约40％TDI二聚物的潜反应性(latent-reactive)异氰酸酯的DISPERCOLL BL XP 2514含水悬浮液。能够钝化的有用固体颗粒异氰酸酯包括DISPERCOLL LP BUEJ471，可由德国的Bayer Material Science AG的100％固体微米化IPDI异氰尿酸酯，以及可由德国Mannheim的Rhein Chemie Rheinau GmBH得到的ADDOLINK TT和ADDOLINK ST。
可将固体表面钝化异氰酸酯与第一聚氨酯分散体混合以形成稳定的含水组合物。
其它组分
含水组合物任选包含第二聚合物。可能的第二聚合物的一些实例包括例如第二聚氨酯(例如由德国的Bayer Material Science AG市购的DISPERCOLL U 53)、VAE(乙酸乙烯酯乙烯)、PVA(聚乙烯醇)、丙烯酸类、丁二烯丙烯腈和苯乙烯丁二烯橡胶(SBR)。
含水组合物任选包含多种其它添加剂，包括例如催化剂(例如基于胺的)、防腐剂、pH改进剂(例如氨水)、粘着力促进剂(例如增粘剂、含硅烷化合物)、色素、表面活性剂、消泡剂、杀真菌剂、杀菌剂、增稠剂、封闭剂和稳定剂(例如胺)、填料(例如碳酸盐、滑石、淀粉)、帮助粘合膜形成屏障的材料(例如纳米粘土)、绝缘材料(例如矿物填料、玻璃微泡)、导电材料(例如各种金属(例如银))及其组合。
有用的稳定剂为由Huntsman Corporation(The Woodlands，Texas)市购的JEFFAMINE T-403POLYETHERAMINE。用于水分散体的有用增稠剂包括可由OMG BorchersGmbH(Langenfeld，德国)得到的
Figure BDA0001367064680000071
GEL A LA和可由BASF Chemical Company(Ludwigshafen，德国)市售的STEROCOLL HT。有用的防腐剂为由Thor GmbH(Speyer，德国)市购的ACTICIDE MBS。
自持性粘合膜
将含水组合物干燥成自持性粘合膜。该膜可使用多种方法，包括喷雾(例如螺旋(spiral)、喷溅(splatter)等)和各种涂覆技术(例如辊涂(roll)、狭缝(slot)、凹印(gravure)、图案(pattern)等)由含水组合物形成。
在一种方法中，将含水组合物以所需涂层重量辊涂在释放衬里上。然后使含水组合物通过烘道(drying tunnel)。烘道中的干燥温度可改变，但优选保持在足够低的温度下以防止固体表面钝化异氰酸酯活化。干燥期间粘合膜的温度优选保持在小于约70℃、小于约60℃，或者甚至小于约55℃的温度下。在烘道以后，可以将涂覆在释放衬里上的粘合剂冷却，例如通过冷却辊。然后可将它在例如辊中自身绕制并储存稍后的时间。
自持性粘合膜可包含固体表面钝化异氰酸酯和大于70重量％第一聚氨酯，所述第一聚氨酯具有不大于约90,000的重均分子量(Mw)和至少约25J/g的熔化焓。或者，自持性粘合膜可包含固体表面钝化异氰酸酯和大于70重量％第一聚氨酯，所述第一聚氨酯具有不大于约90,000的重均分子量(Mw)和至少约25J/g的熔化焓，和第二聚合物。固体表面钝化异氰酸酯、第一聚氨酯和第二聚合物的和可总计为自持性粘合膜的至少约90重量％、至少约95重量％，或者甚至至少约98％。
干燥膜具有小于约20密尔、小于约15密尔、小于约10密尔、小于约8密尔、小于约6密尔、约1密尔至约8密尔，或者甚至约2密尔至约6密尔的厚度。膜的厚度可以以多种方法，例如通过直接涂覆、多次通过涂布机或者将两个不同厚度的膜层压在一起而得到。
膜可在两种不同的基质之间形成强粘合。基质可以为分层的。强粘合可以以不大于约90℃、不大于约80℃、不大于约70℃或者甚至约50℃至约90℃的粘合层温度(即在它形成时粘合的温度)。
复合结构
自持性粘合膜可用于形成复合结构。复合结构包含粘合膜和至少一个其它层(例如基质)。该层可以为刚性或柔性的。粘合膜可置于层的至少一个表面上以覆盖它。
有用的刚性层的实例包括瓷砖、陶瓷、金属(例如铝、不锈钢)、塑料(例如聚乙烯、聚丙烯、聚酰胺(例如尼龙)、聚氨酯、聚碳酸酯、丙烯腈-丁二烯-苯乙烯(ABS)、ABS/聚碳酸酯共混物、聚醚醚酮(PEEK)等)、塑料复合物(例如纤维补强塑料)、玻璃、纸板、木材和含木材产品。刚性层可包含一个层或者它可以为多层的(即包含至少两个层)。
可将刚性层预处理以改进自持性粘合膜的粘着力。可通过多种方法，包括(例如电晕、等离子体、火焰、各种化学底漆及其组合)将它预处理。
有用柔性层的实例包括各种纺织品(例如织物(例如基于微纤维的聚乙烯、棉、帆布和非机织物)、人造皮革和毛皮、箔(例如装饰箔)、纸、膜(例如塑料膜(例如聚酯、聚酰亚胺(即Kapton)、聚丙烯和聚乙烯))及其组合。
或者，自持性粘合膜可用于形成包含刚性层和柔性层的复合结构，其中自持性粘合膜层位于刚性层与柔性层之间以将两个层粘合在一起。
自持性粘合膜可进一步用于形成选自双刚性层和双柔性层的复合结构。自持性粘合膜层位于两个层之间以将两个层粘合在一起。双刚性层/双柔性层复合物可包含相同的材料或者它们可包含不同的材料。
复合结构可通过大量不同的方法形成。
在一种方法中，柔性层与自持性膜的第一主表面接触并在将膜应用于柔性基质上以前或以后将热施加在膜上，或其组合。然后使刚性层与自持性膜的第二主表面接触，使得第二主表面与刚性层直接接触以形成复合物。将复合物加热至至少约70℃的温度以将异氰酸酯活化并开始固化方法。或者，将复合物加热至恰好足够热的温度以形成粘合。可使用压力帮助形成粘合(例如膜或轮胎压床)。需要有限的时间形成粘合。
用途
自持性粘合膜用于生产多种物品，包括但不限于例如鞋子、汽车部件、车厢覆盖物、纺织品叠片结构(例如室外服饰、妇女贴身内衣)、各种组装商品(例如面板、叠片结构、过滤器、地板等)。
实施例
测试程序
除非另外说明，实施例和整个说明书中所用测试程序包括如下。
分子量
各干燥聚氨酯试样的GPC分子量分布曲线使用与Waters 2414RI检测器连接的Waters 2695分离模块，使0.05M LiBr/DMF流动相通过2个Agilent Resipore GPC柱而得到。分子量数据相对于聚甲基丙烯酸甲酯标准计算。
熔融峰和熔化焓测试方法
干燥聚氨酯分散体的熔融峰和熔化焓(ΔH)使用差示扫描量热法(DSC)使用PYRIS1DSC以10℃/分钟的加热速率测定。
粘合测试方法
干燥膜由表2中的水基组合物制备。使用具有250μm间隙的10cm宽刮涂(drawdown)棒刮涂膜。将膜在40℃的温度下干燥20分钟以形成100μm(3.94密尔)厚干燥膜。
然后在聚碳酸酯与聚氨酯基织物之间制备粘合。该粘合使用指定粘合层温度以5N/cm2的粘合压力和60秒的粘合时间制备。
然后将粘合在室温下老化5分钟并使用ZWICK剥落测试机以300mm/分钟的速度剥离。报告两个粘合的平均值。
根据熔融峰和熔化焓测试方法以及根据分子量测试方法测试市售的聚氨酯分散体。结果描述于下表1中。
表1—聚氨酯分散体对比
Figure BDA0001367064680000101
*如供应商所报告的
实施例1-4
含水组合物通过将下表2所述组分以所述量结合而制备。然后根据粘合测试方法测试所得组合物，结果报告于表2中。
表2—实施例
Figure BDA0001367064680000111
其它实施方案在权利要求书内。

Claims (11)

1.自持性粘合膜，其包含：
固体表面钝化异氰酸酯；
至少50重量％的异氰酸酯反应性的第一聚氨酯，所述第一聚氨酯衍生自聚酯多元醇并且具有不大于90,000的重均分子量和25J/g至70J/g的熔化焓；和
选自不同于第一聚氨酯的第二聚氨酯、乙酸乙烯酯乙烯、聚乙烯醇、丙烯酸类聚合物、丁二烯丙烯腈、苯乙烯丁二烯橡胶及其组合的第二聚合物，其中重均分子量使用与Waters2414RI检测器连接的Waters 2695分离模块，使0.05M LiBr/DMF流动相通过2个AgilentResipore GPC柱，相对于聚甲基丙烯酸甲酯标准计算得到，
其中所述熔化焓使用差示扫描量热法使用PYRIS 1DSC以10℃/分钟的加热速率测定。
2.权利要求1的自持性粘合膜，其中第一聚氨酯具有至少35J/g的熔化焓。
3.权利要求1的自持性粘合膜，其包含至少70重量％的第一异氰酸酯反应性聚氨酯。
4.权利要求1的自持性粘合膜，其中第一聚氨酯具有不大于80,000的重均分子量。
5.权利要求1的自持性粘合膜，其中固体表面钝化异氰酸酯、第一聚氨酯和第二聚合物的和总计为自持性粘合膜重量的至少90重量％。
6.权利要求1的自持性粘合膜，其中固体表面钝化异氰酸酯、第一聚氨酯和第二聚合物的和总计为自持性粘合膜重量的至少95重量％。
7.权利要求1的自持性粘合膜，其中固体表面钝化异氰酸酯、第一聚氨酯和第二聚合物的和总计为自持性粘合膜重量的至少98重量％。
8.制备复合物的方法，其包括：使柔性层与权利要求1的自持性粘合膜的第一主表面接触；
在将膜应用于柔性基质上以前或以后将热施加在膜上；
使刚性层与自持性粘合膜的第二主表面接触使得第二主表面与刚性层直接接触以形成复合物；和
将热和压力施加在复合物上。
9.复合结构，其包含：
权利要求1的自持性粘合膜，
刚性层，和
柔性层，
其中刚性层通过自持性粘合膜粘合在柔性层上。
10.根据权利要求9的复合结构，其中刚性层包含金属、金属复合物、塑料、塑料复合物、木材和木材复合物中的至少一种，并且柔性层包含织物、箔、膜和纸中的至少一种。
11.根据权利要求9的复合结构，其中刚性层为尼龙且柔性层为微纤维。
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