CN104718259B - 改良的硫化后粘结 - Google Patents
改良的硫化后粘结 Download PDFInfo
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- CN104718259B CN104718259B CN201380039686.9A CN201380039686A CN104718259B CN 104718259 B CN104718259 B CN 104718259B CN 201380039686 A CN201380039686 A CN 201380039686A CN 104718259 B CN104718259 B CN 104718259B
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- elastomer
- method described
- primer
- epoxy
- substrate
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Abstract
本发明提供一种两部分粘合剂体系,其中第一部分为基底粘合剂,包含聚氨酯基粘合剂、丙烯酸基粘合剂或环氧基粘合剂中的至少一种;并且第二部分为弹性体底胶,包含卤化聚烯烃以及任选的亚硝基化合物。本发明还提供了使用上述粘合剂将弹性体粘结至基底的硫化后粘结方法。
Description
相关申请的交叉引用
本申请要求2012年7月25日提交的标题为“改良的硫化后粘结(IMPROVED POST-VULCANIZATION BONDING)”的美国临时专利申请序号61/675,370的优先权,该申请的公开内容以引用方式并入本文。
技术领域
本发明涉及两部分硫化后粘合剂体系,以及用于弹性体基底的硫化后粘结方法。
背景技术
长期以来,一直需要强力粘合剂以及用于将硫化橡胶或其他固化弹性体粘结于金属和其他基底上的方法。在大多数橡胶粘结工艺中,将传统的橡胶与基底间的粘合剂(例如LORD公司出售的粘合剂)施加到金属件上,然后将其加载于模具上,并将未硫化的橡胶或其他弹性体注入到模具中。接着,将填充橡胶的模具加热,从而使粘合剂在橡胶硫化的过程中共同固化。这确保了橡胶与金属基底之间的强力粘结。
但是,在一些应用中,粘合剂与橡胶共同固化是不切实际或不可行的。例如,在诸如某些支架和套管之类的部件的制造过程中,粘结必须在形成橡胶部件,并且硫化后才能进行。在一些情况中,橡胶与基底间的硫化后粘结还可以提供比模具中粘结更大的成本益处。在这些情况下,必须在硫化橡胶与刚性基底(例如金属)之间产生粘结。
现有技术的解决方案通常使用环氧基金属粘结用粘合剂,从而提供与金属面的粘合,并且橡胶表面经过化学处理,以增强橡胶与环氧基金属粘结用粘合剂之间的粘合。尽管这些方法有时是有效的,但是它们常常不能提供期望那样良好的粘结,特别是这些体系在高温下保持粘结的能力通常较差。
因此,希望提供的是用于将弹性体(例如天然橡胶)硫化后粘结于非弹性体基底(例如钢铁和工程聚合物)上的材料和方法。
本发明所涉及的正是所注意到的这些需要。
发明概述
在本发明的第一个方面中,提供一种两部分粘合剂体系,包含:(a)基底粘合剂,包含聚氨酯基粘合剂、丙烯酸基粘合剂或环氧基粘合剂中的至少一种;以及(b)弹性体底胶,包含卤化聚烯烃以及任选的亚硝基化合物。在本发明的一个实施方案中,卤化聚烯烃包括溴化聚(二氯丁二烯)。在本发明的另一个实施方案中,卤化聚烯烃包括氯化天然橡胶。在本发明的另一个实施方案中,卤化聚烯烃包括氯磺化聚乙烯。在本发明的另一个实施方案中,亚硝基化合物包括聚二亚硝基苯。
在本发明的另一个方面中,基底粘合剂包含聚氨酯基粘合剂,并且进一步包含催化剂。在本发明的另一个方面中,基底粘合剂包含环氧基粘合剂,并且进一步包含胺类硬化剂。在本发明的另一个方面中,基底粘合剂包含丙烯酸基粘合剂,其进一步包含氧化还原引发剂体系。
在本发明的另一个实施方案中,基底粘合剂除了酚醛环氧材料以外,基本不含或不含酚醛树脂。在本发明的另一个实施方案中,基底粘合剂基本不含或不含卤化聚烯烃。在本发明的另一个实施方案中,弹性体底胶除了酚醛环氧材料以外,基本不含或不含环氧树脂。在本发明的另一个实施方案中,弹性体底胶基本不含或不含酚醛树脂。本发明的另一个实施方案包含两部分粘合剂体系,其中弹性体底胶包含双马来酰亚胺材料。在本发明的另一个实施方案中,弹性体底胶包含溶剂基底胶。在本发明的其他实施方案中,弹性体底胶包含水性底胶。
在本发明的另一个方面中,弹性体底胶已被施加到硫化弹性体部件上,并且基底粘合剂已被施加到金属部件上。在本发明的另一个方面中,使弹性体部件和金属部件相接触,以使弹性体底胶与基底粘合剂彼此相接触,从而形成粘结组件。在本发明的另一个实施方案中,当根据ASTM D 429在高于100℃的温度下以90°角牵拉粘结组件时,该粘结组件显示出至少90%的橡胶保持率。
在本发明的另一个方面中,提供了用于弹性体的硫化后粘结的方法,包括:(a)提供硫化弹性体;(b)将弹性体底胶组合物施加到硫化弹性体上,其中弹性体底胶组合物包含卤化聚烯烃和二亚硝基苯;(c)提供待粘结的基底;(d)将基底粘合剂施加到基底上,其中基底粘合剂包含环氧基粘合剂、丙烯酸基粘合剂或聚氨酯基粘合剂中的至少一种;以及(e)使弹性体底胶涂覆的硫化弹性体与基底粘合剂涂覆的基底相接触,使得环氧粘合剂的至少一部分与卤化聚烯烃底胶的至少一部分相接触,从而形成组件。
在本发明的另一个实施方案中,所述的方法还包括加热组件,以使弹性体底胶固化的步骤(f)。在本发明的另一个实施方案中,将组件加热到至少250℉,持续大约5分钟。在本发明的另一个实施方案中,在未实施预处理步骤的条件下将弹性体底胶施加到弹性体上。
至此,稍微宽泛地概括了本发明的较重要的特征,以便可以更好地理解以下的详细描述,并可以更好地领会本发明对本领域的贡献。显然,下文将描述本发明的其他特征,并且这些特征形成了本发明所附权利要求书的主题。在这个方面,在详细地解释本发明的多个实施方案之前,应该理解的是本申请中的发明不限于以下描述中的细节和构造、以及组件的排列。本发明能够具有其他的实施方案,并且能够以多种方式实施并进行。
此外,应该理解的是本文中的用语和术语是为了说明的目的,不应该被认为是在任何方面进行的限定。本领域的技术人员将理解本发明公开所基于的概念,这些概念可以容易地作为用于实施本研发的多个目的而设计的其他结构、方法和系统的基础。重要的是,权利要求书被认为是包括了这些等价的构造,只要它们不脱离本发明的精神和范围即可。
优选实施方案的详细描述
在本发明的第一个方面中,提供了两部分粘合剂体系,其包含基底粘合剂和弹性体底胶。基底粘合剂优选地包括对于粘结基底(例如金属或工程聚合物)具有亲和性的环氧基粘合剂、丙烯酸基粘合剂或聚氨酯基粘合剂。弹性体底胶优选地包括对于粘结弹性体具有亲和性的底胶。使用这种两部分粘合剂体系意想不到地提供了硫化后的橡胶和其他弹性体与金属和其他刚性基底之间的强力粘结。特别是,相对于现有技术的解决方案,这种粘合剂体系的高温性能得到极大改善。
基底粘合剂优选地包括环氧基粘合剂、丙烯酸基粘合剂或聚氨酯基粘合剂。此类环氧粘合剂的实例包括LORD公司出售的 系环氧粘合剂。此类聚氨酯和丙烯酸粘合剂的实例包括LORD公司出售的系粘合剂。
在本发明的优选实施方案中,基底粘合剂具有高的Tg,从而在较高的温度下提供较好的粘合。在本发明的一个实施方案中,金属粘结用粘合剂的Tg为至少70℃,更优选为至少95℃,最优选为高于110℃。据推测由于在足够高的温度下,当基底粘合剂对橡胶粘结用底胶失去粘合时,发生失效,所以高的Tg是优选的。在金属粘结用粘合剂部件中选择具有较高Tg的材料会增加最终粘合剂粘结的操作温度。
在本发明的优选实施方案中,弹性体底胶包含卤化聚烯烃基粘合剂,优选包含亚硝基化合物。具有与这些弹性体底胶相关的化学性质的市售产品的实例包括LORD公司出售的系粘合剂。此类弹性体底胶可以按照本领域已知的溶剂、水性或粉末形式输送。
环氧基
在本发明的优选实施方案中,基底粘合剂包含环氧基粘合剂。本发明的环氧化合物可以为包含环氧(环氧乙烷)基团的任何材料。所包含的环氧树脂为环氧甲酚酚醛清漆、环氧苯酚酚醛清漆、以及它们的任一种与双酚A环氧树脂的共混物。单体的环氧化合物和聚合型的环氧衍生物可以为脂肪族、脂环族、芳香族或杂环的。每个分子中环氧基团的“平均”数是通过含环氧材料中的环氧基团的总数除以所存在的环氧分子的总数而测定的。有用的环氧材料通常每个分子中包含平均至少1.5个可聚合的环氧基团。优选的是,每个分子包含2个或更多个环氧基团。聚合的环氧衍生物包括具有末端环氧基团的线性聚合物(例如聚氧亚烷基二醇的缩水甘油醚)、具有环氧乙烷单元主链的聚合物(例如聚丁二烯聚环氧化物)、以及具有环氧基团支链的聚合物(例如甲基丙烯酸缩水甘油酯聚合物或共聚物)。环氧衍生物可以为纯的化合物,但是通常为每个分子包含1个、2个或更多个环氧基团的混合物。
含环氧的材料可以从低分子量的单体材料至高分子量的聚合物而变化,并且在它们的主链和取代基的性质方面可以大不相同。例如主链可以为任何类型,而其上的取代基可以不含活性氢原子。举例说明可行的取代基包括卤素、酯基、醚、磺酸基、硅氧烷基、硝基、磷酸酯基等。含环氧的材料的分子量可以不同,为大约50至100000或更高。多种含环氧的材料的混合物也可以用于本发明的组合物中。
本发明的环氧化合物可以为脂环族环氧化物。脂环族环氧化物的实例包括二羧酸脂环族酯的二环氧化物,例如双(3,4-环氧环己基甲基)草酸酯、双(3,4-环氧环己基甲基)己二酸酯、双(3,4-环氧-6-甲基环己基甲基)己二酸酯、双(3,4-环氧环己基甲基)庚二酸酯等。其他合适的二羧酸脂环族酯的二环氧化物在例如美国专利号2,750,395中有所描述,该文献的内容以引用方式并入本文。
基于双酚A的环氧树脂(为固体且能够溶解于载体中;或者为液体)优选为相对廉价的那些。可用的环氧材料是多种多样的,不论它们是树脂的化合物还是简单的化合物,都统称为环氧树脂。具体而言,易得的简单的环氧化合物包括环氧十八烷;甲基丙烯酸缩水甘油酯;双酚A的二缩水甘油醚(例如得自壳牌化学公司商品名为EPON以及得自陶氏化学公司商品名为DER的那些);乙烯基环己烯二氧化物(例如得自Union Carbide公司的ERL-4206);3,4-环氧环己基甲基-3,4-环氧环己烷羧酸酯(例如得自Union Carbide公司的ERL-4221);3,4-环氧-6-甲基环己基甲基-3,4-环氧-6-甲基环己烯羧酸酯(例如得自Union Carbide公司的ERL-4201);双(3,4-环氧-6-甲基环己基甲基)己二酸酯(例如得自Union Carbide公司的ERL-4289);双(2,3-环氧环戊基)醚(例如得自Union Carbide公司的ERL-0400);聚丙二醇改性的脂肪族环氧树脂(例如得自Union Carbide公司的ERL-4050和ERL-4052);二氧化二戊烯(例如得自Union Carbide公司的ERL-4269);环氧化的聚丁二烯(例如得自FMC公司的OXIRON 2001);包含环氧树脂官能性的有机硅树脂;阻燃性环氧树脂(例如DER-580,得自陶氏化学公司的溴化双酚型环氧树脂);苯酚甲醛清漆的1,4-丁二醇二缩水甘油醚(例如得自陶氏化学公司的DEN-431和DEN-438);以及间苯二酚二缩水甘油醚。
在本发明的另一个实施方案中,环氧基粘合剂包含胺类硬化剂,其包括用于环氧树脂的胺型固化剂。例如,脂肪族多胺、脂环族多胺、叔胺、聚氨基酰胺和它们的各种混合物均可用于该目的。用于本发明的目的的胺类硬化剂的实例包括二乙撑三胺,三乙撑四胺,四乙撑五胺,2-甲基-1,5-戊二胺,二乙醇胺,甲基二乙醇胺,三乙醇胺,五乙撑六胺,乙二胺,四亚甲基二胺,已二胺,聚醚二胺,双(六亚甲基三胺),二乙氨基丙胺,三甲基六(亚甲基二胺),油胺,二亚丙基三胺,1,3,6-三(氨基甲基己烷),3,9-双(3-氨基丙基)-2,4,8,10-四氧代螺旋[5,5]-十一烷,1,3-双(氨基甲基环己烷),双(4-氨基环己基)甲烷,双(4-氨基-3-甲基环己基)甲烷,异佛尔酮二胺,N-氨基乙基哌嗪等。通过与环氧树脂或丙烯腈加成或者通过与脂肪酸缩合而改性的脂肪族多胺也都可以用作胺类硬化剂。此外,就本发明的目的而言,多种曼尼希碱可以用作胺类硬化剂。
其中胺基与芳香环直接连接的芳香族多胺(例如二甲苯二胺等)也都可以用于实施本发明,但是与脂肪族二胺相比较不优选。芳香族多胺的实例包括二氨基苯基甲烷、苯胺-甲醛的低分子量缩合物、间苯二胺、二氨基二苯基砜等。
本文中的未受阻脂肪胺类硬化剂是指包含与伯碳原子连接的伯胺基团的胺化合物。任选地,胺类硬化剂的使用量可以为,占基底粘合剂组合物的主要组分的大约10重量%至50重量%、优选为大约20重量%至40重量%。
在使用胺固化的环氧树脂作为基底粘合剂的本发明的另一个实施方案中,EEW/AHEW的比值(环氧当量与胺氢当量的重量比值)为0.5-1.5,优选为0.8-1.2。
丙烯酸基
在本发明的另一个实施方案中,基底粘合剂包含丙烯酸基粘合剂。根据本发明的实施方案,优选的自由基可聚合的单体包括特征在于存在-C=C-基团的烯烃单体。代表性的烯烃单体包括(甲基)丙烯酸的酯,例如甲基丙烯酸甲酯,甲基丙烯酸乙酯,甲基丙烯酸丁酯,丙烯酸甲酯,丙烯酸丁酯,丙烯酸环己酯,丙烯酸己酯,丙烯酸2-乙基己酯,丙烯酸月桂酯,丙烯酸乙酯,二甲基丙烯酸二乙二醇酯,甲基丙烯酸二环戊二烯基氧基乙酯(dicyclopentadienyloxyethyl methacrylate),甲基丙烯酸环己酯,甲基丙烯酸月桂酯,甲基丙烯酸缩水甘油酯和甲基丙烯酸四氢糠酯;甲基丙烯酸;丙烯酸;取代的(甲基)丙烯酸,例如衣康酸,丙烯腈,甲基丙烯腈,丙烯酰胺和甲基丙烯酰胺;苯乙烯;取代的苯乙烯,例如乙烯基苯乙烯,氯苯乙烯,甲基苯乙烯和正丁基苯乙烯;乙酸乙烯酯;偏二氯乙烯;以及丁二烯,例如2,3-二氯-1,3-丁二烯和2-氯-1,3-丁二烯。其他烯烃单体包括马来酸酯;富马酸酯;以及苯乙烯类化合物,例如苯乙烯,氯苯乙烯,甲基苯乙烯,丁基苯乙烯和乙烯基苯乙烯。
在本发明的一个实施方案中,所述的单体在丙烯酸粘合剂中以占主要成分的10-90重量%的量存在。在本发明的另一个实施方案中,所述的单体以占主要成分的20-70重量%的量存在。在本发明的另一个实施方案中,所述的单体以占主要成分的30-60重量%的量存在。
在一个实施方案中,丙烯酸粘合剂包含环境温度反应性氧化还原引发剂或催化剂体系。环境温度反应性催化剂体系是公知的氧化还原对体系,本文中无需大范围详细地讨论,但是它们包含在环境温度下共反应的至少一种氧化剂和至少一种还原剂,从而产生有效引发加聚反应并固化粘合剂的自由基。合适的氧化还原(氧化作用-还原作用)引发剂包括但不限于过硫酸盐引发剂与还原剂(如焦亚硫酸钠和亚硫酸氢钠)的组合;基于有机过氧化物和叔胺的体系(例如过氧化苯甲酰加上二甲基苯胺);以及基于有机氢过氧化物和过渡金属的体系(例如氢过氧化枯烯加上环烷酸钴)。
在本发明的一个实施方案中,可以使用实质上任何已知的氧化剂。代表性的氧化剂包括但不限于有机过氧化物,例如过氧化苯甲酰和其他过氧化二酰;氢过氧化物,例如氢过氧化枯烯;过酸酯,例如β-丁基过氧化苯甲酸酯;酮氢过氧化物,例如甲基乙基酮氢过氧化物;过渡金属的有机盐,例如环烷酸钴;以及包含不稳定氯的化合物,例如磺酰氯。在其中在弹性体底胶中使用亚硝基化合物的本发明的实施方案中,优选的是基底粘合剂不包含过氧化物化合物,这是因为亚硝基化合物可能干扰过氧化物的固化机制。
代表性的还原剂包括但不限于亚磺酸;偶氮化合物,例如偶氮二异丁腈;α-氨基砜,例如双(甲苯基磺酰基甲基)苄胺;叔胺,例如二异丙醇对甲苯胺(DIIPT)、二甲基苯胺、对位卤化苯胺衍生物和二甲基对甲苯胺;以及胺醛缩合产物,例如脂肪族醛(例如丁醛)与伯胺(例如苯胺或丁胺)的缩合产物。优选的还原剂为对位卤化苯胺衍生物。示例性的还原剂包括但不限于N,N-二异丙醇-对氯代苯胺;N,N-二异丙醇-对溴代苯胺;N,N-二异丙醇-对溴代-间甲基苯胺;N,N-二甲基-对氯代苯胺;N,N-二甲基-对溴代苯胺;N,N-二乙基-对氯代苯胺;以及N,N-二乙基-对溴代苯胺。
优选的是,氧化剂以占可聚合的粘合剂组合物的大约0.5重量%至大约50重量%的量存在,并且还原剂的量占可聚合的粘合剂组合物的大约0.05重量%至大约10重量%、优选为大约0.1重量%至大约6重量%的范围。
任选地,可以使用占丙烯酸粘合剂的主要成分的大约0至80重量%、更优选的是2重量%至50重量%的增韧剂聚合物。示例性的低分子量增韧剂的重均分子量(Mw)低于大约18000,或者数均分子量(Mn)低于大约10000。增韧剂聚合物材料可以包含或不包含自身能够聚合的或者与上文所述的至少一种自由基可聚合的单体共聚的烯烃不饱和结构。聚合材料可以为(例如)各种固体和液体弹性体聚合材料,具体为在美国专利号4,223,115、4,452,944、4,769,419、5,641,834和5,710,235中所述的液体烯烃封端的弹性体,以及在美国专利号4,223,115、4,452,944、4,467,071和4,769,419中所述的异氰酸酯官能的预聚物和羟基官能的单体的烯烃聚氨酯反应产物,每一份所述文献的全部内容均以引用方式并入本文。
在本发明的另一个实施方案中,丙烯酸粘合剂还包含促黏剂。根据本发明的实施方案的促黏剂包括本领域的普通技术人员已知的、用于在丙烯酸粘合剂中促进粘合的任何促黏剂。根据本发明的实施方案的优选的促黏剂为增强金属粘合的含磷化合物,并且可以为具有至少一个P-OH基和至少一个有机部分的次膦酸、膦酸或磷酸的任何衍生物,其中所述的有机部分的特征在于存在烯基,该烯基优选位于末端。此类磷化合物的列举可以在美国专利号4,223,115中找到。
在本发明的另一个实施方案中,丙烯酸粘合剂组合物任选地包含环氧组分。在本发明的一个实施方案中,环氧组分包括可硬化的环氧官能的化合物(液态树脂),其每个分子(聚环氧化物)中包含统计学上多于1个的环氧乙烷环。优选的环氧官能的材料在每个分子中都包含2个环氧基团。单官能的环氧化合物还可以与聚环氧化物组分结合,其中所述的聚环氧化物组分作为起活性稀释剂作用的粘度调节剂。适用于本文所述的用途的环氧树脂包括多元醇的多缩水甘油酯以及多羧酸的多缩水甘油酯。多缩水甘油酯可以通过使表卤代醇(例如表氯醇或表溴醇)与脂肪族或芳香族多羧酸(例如草酸、琥珀酸、戊二酸、对苯二酸、2,6-萘二甲酸和二聚亚油酸)反应而获得。芳香族多元醇的多缩水甘油酯是优选的,并且可以通过使表卤代醇在碱存在下与多羟基苯酚化合物反应来制备。合适的起始多羟基苯酚包括间苯二酚,邻苯二酚,对苯二酚,双(4-羟基苯基)-2,2-丙烷(也称为双酚A),双(4-羟基苯基)-1,1-异丁烷,4,4-二羟基二苯甲酮,双(4-羟基苯酚)-1,1-乙烷,双(2-羟基苯基)-甲烷,1,5-羟基萘,以及双酚A的二缩水甘油醚。
聚氨酯基
在本发明的另一个实施方案中,基底粘合剂包含聚氨酯基粘合剂。本发明的聚氨酯粘合剂以聚氨酯预聚物为基础,所述的聚氨酯预聚物是由某些多羟基化合物和异氰酸酯化合物(优选为多官能的异氰酸酯,其可以用于产生粘合剂粘结)制备得到的。
合适的多官能异氰酸酯包括在每个分子中含有至少2个异氰酸酯基团的脂肪族、脂环族和/或芳香族的多异氰酸酯。由于脂肪族二异氰酸酯对UV光具有良好的抗性,所以其产生了变黄趋势低、但是比芳香族多异氰酸酯更昂贵的产物。在第一部分中,异氰酸酯组分基本上可以为具有2至4个、优选为2至3个异氰酸酯官能度的脂肪族或芳香族、环状或线性的有机异氰酸酯化合物。粘合剂混合物中所需的多异氰酸酯还可以包含官能度大于2的多异氰酸酯部分。三异氰酸酯可以通过二异氰酸酯的三聚作用或低聚作用或者通过使二异氰酸酯与含有OH或NH基团的多官能化合物反应而得到。
异氰酸酯可以为低、高或中等分子量,并且可以为多种有机多异氰酸酯中的任意一种。可用于本发明的典型的脂肪族异氰酸酯化合物包括六亚甲基二异氰酸酯,例如2,2,4-三甲基六亚甲基-1,6-二异氰酸酯和六亚甲基-1,6-二异氰酸酯(包括其二聚物和三聚物);亚乙基二异氰酸酯;三亚甲基二异氰酸酯;十二亚甲基二异氰酸酯;六亚甲基二异氰酸酯;四亚乙基二异氰酸酯;五亚甲基二异氰酸酯;亚丙基-1,2-二异氰酸酯;2,3-二甲基四亚甲基二异氰酸酯;亚丁基-1,3-二异氰酸酯;亚丁基-1,3-二异氰酸酯;1,4-二异氰酸根合环己烷;乙基亚乙基二异氰酸酯;以及三甲基己烷二异氰酸酯等。具有至少2个异氰酸酯官能度的多异氰酸酯在美国专利号3,350,362和3,382,215中公开。本质为聚合的多异氰酸酯(包括所有类型的异氰酸酯预聚物)包含在本发明中。
脂环族多异氰酸酯包括环丁烷二异氰酸酯;亚环戊基二异氰酸酯,例如环戊烯-1,3-二异氰酸酯;亚环己基二异氰酸酯,例如甲基亚环己基二异氰酸酯;二环己基甲烷二异氰酸酯,例如双(4-异氰酸根合环己基)甲烷;以及1,4-环己烷二异氰酸酯,例如1,4-双(异氰酸根合甲基)环己烷。
可以使用的芳香族多异氰酸酯的实例为亚苯基二异氰酸酯,甲苯二异氰酸酯,亚二甲苯基二异氰酸酯,双亚苯基二异氰酸酯的异构体,亚萘基二异氰酸酯的异构体,二苯基甲烷二异氰酸酯的异构体,对亚苯基二异氰酸酯,1-甲基亚苯基-2,4-二异氰酸酯,萘-1,4-二异氰酸酯,甲苯二异氰酸酯,二苯基-4,4'-二异氰酸酯,苯-1,2,4-三异氰酸酯,二甲苯-1,4-二异氰酸酯,二甲苯-1,3-二异氰酸酯,4,4'-二亚苯基甲烷二异氰酸酯,4,4'-二亚苯基丙烷二异氰酸酯,以及多亚甲基多苯基异氰酸酯。
在第二部分中的多羟基化合物可以用于与第一部分中的异氰酸酯化合物反应,并且为混合物,其主要包含占主要的短链和长链二级多元醇。任选地,不超过大约25重量%的多元醇混合物可以由初级多元醇组成。更优选的是,不超过15重量%的多元醇混合物包含初级多元醇,并且对所存在的初级多元醇的最优选的限定为占总多元醇的总多元醇重量的至多约5重量%。
术语“长链”是指分子量为2000至12000的多元醇。长链多元醇包括聚醚、聚酯、聚己酸内酯、聚碳酸酯、丙烯酸多元醇和聚丁二烯类型等在内的广泛类别。长链二级多元醇的官能度不是关键的。长链二级多元醇的官能度可以为1.6至大约4的范围。用于本发明的长链多元醇主要是二级多元醇,优选的是通过加入(例如)环氧丙烷而用仲羟基加帽或封端的聚醚多元醇,并且最优选的是只包含聚氧化亚丙基。可以包含重量不超过25%的伯羟基,例如1重量%至25重量%的使用环氧乙烷封端的多元醇。优选的是,初级多元醇的量不超过15%,并且更优选的是不超过5%。
任选地,至多大约2.0重量%的催化剂可以用于聚氨酯基粘合剂。优选的催化剂是指延迟作用的催化剂。这些催化剂包括已知会促进链传递和粘合剂中的交联反应(例如胺与异氰酸酯之间、和/或多元醇和异氰酸酯之间)的那些催化剂。本领域已知的催化剂化合物包括锡催化剂,例如硫醇二烷基锡、巯基乙酸二烷基锡、二巯基酸二烷基锡、并包括混合物。具体的示例性的锡催化剂包括二月桂酸二丁基锡,二乙酸二丁基锡,乙酸锡(II),辛酸锡(II),乙基己酸锡(II),月桂酸锡(II),二乙酸二乙基锡,二乙酸二丁基锡,二月桂酸二丁基锡,马来酸二丁锡,二乙酸二己基锡,二乙酸二辛基锡,和二异辛基马来酸二丁基锡。硫醇二烷基锡包括二硫醇二甲基锡、二硫醇二丁基锡和二硫醇二辛基锡。巯基乙酸二烷基锡包括二异辛基巯基乙酸二丁基锡和混合物。此外,丙酮酸铁和乙酰丙酮镍也是合适的。可以使用0.001重量%至0.5重量%的锡催化剂。锡催化剂购自Air Products and Chemical,Inc。
如本领域所知,多种常规的添加剂可以任选地包含于聚氨酯基粘合剂中,例如填料、增补剂、增塑剂、流变改性剂、颜料、玻璃球、抑制剂、抗氧化剂等。典型的填料包括硅酸盐、滑石和粘土、碳酸钙、氧化铝、二氧化硅、分子筛等;无机和/或有机颜料包括TiO2等;典型的增塑剂包括邻苯二甲酸酯、己二酸酯、壬二酸酯等;典型的抗氧化剂包括受阻多酚,例如由Ciba Specialty化学公司以商品名IRGANOX和AOX出售的抗氧化剂。示例性的市售UV稳定剂可得自Ciba Specialty化学公司,商品名为TINUVIN。
弹性体底胶
在本发明的另一个实施方案中,弹性体底胶包含卤化聚烯烃基底胶。卤化聚烯烃包括任何天然的或合成的卤化聚烯烃弹性体。在卤化聚烯烃弹性体中使用的卤素通常为氯或溴,但是还可以使用氟。此外,还可以使用卤素的混合物,在这种情况下,包含卤素的聚烯烃弹性体具有多于1种的在弹性体上取代的卤素。似乎卤素的量不是关键的,并且取决于基础弹性体或聚合物的性质,可以低至大约3重量%至超过70重量%。卤化聚烯烃及其制备是本领域的技术人员所公知的。
代表性的卤化聚烯烃包括氯化的天然橡胶;含氯和含溴的合成橡胶,包括聚氯丁烯,氯化的聚氯丁烯,氯化的聚丁二烯,六氯戊二烯,丁二烯/卤化环状共轭二烯加成物,氯化丁二烯苯乙烯共聚物,氯化乙烯丙烯共聚物和乙烯/丙烯/非共轭二烯三聚物,氯化聚乙烯,氯磺化聚乙烯,溴化聚(2,3-二氯-1,3-丁二烯),α-卤代丙烯腈和2,3-二氯-1,3-丁二烯的共聚物,氯化聚(氯乙烯)等,如上文所述,包括此类含卤素弹性体的混合物。因此,实质上天然和合成弹性体中的任意一种已知的含卤素衍生物都可以用于实施本发明,包括此类弹性体的混合物。
在本发明的另一个实施方案中,弹性体底胶组合物优选地包含亚硝基化合物。亚硝基化合物可以是亚硝基化合物本身,或者是亚硝基化合物的前体。可用作本发明的交联剂的亚硝基化合物可以为任何芳烃,例如苯、萘、蒽、联苯等,其包含至少2个与不相邻的环上的碳原子直接相连的亚硝基。更具体而言,此类亚硝基化合物描述为这样的芳香族化合物:具有1至3个芳香核(包括稠合的芳香核),并具有2至6个与不相邻的核上的碳原子直接相连的亚硝基。本发明优选的亚硝基化合物为二亚硝基芳香族化合物,特别是二亚硝基苯和二亚硝基萘,例如间-或对-二亚硝基苯、和间-或对-二亚硝基萘。芳香核的核上氢原子可以被烷基、烷氧基、环烷基、芳基、芳烷基、烷芳基、芳基胺、芳基亚硝基、氨基、卤素等基团取代。在本发明中,在芳香核上存在这些取代基对亚硝基化合物的活性几乎没有影响。就目前所知,对取代基的特征没有限定,并且此类取代基在在本质上可以是有机的或无机的。因此,在本发明中涉及亚硝基化合物时,除非另作说明,否则应该理解为包括取代的和未取代的亚硝基化合物。
特别优选的亚硝基化合物可通过下式表征:
(R)m--Ar--(NO)2
其中Ar选自由亚苯基和萘构成的组;R为一价有机基团,其选自由具有1至20个碳原子的烷基、环烷基、芳基、芳烷基、烷芳基、芳基胺和烷氧基;氨基;或卤素构成的组,并且优选是具有1至8个碳原子的烷基;m为0、1、2、3或4,优选为0。
适用于实施本发明的亚硝基化合物的部分非限定性列表包括:间二亚硝基苯、对二亚硝基苯、间二亚硝基萘、对二亚硝基萘、2,5-二亚硝基-对异丙基甲苯、2-甲基-1,4-二亚硝基苯、2-甲基-5-氯-1,4-二亚硝基苯、2-氟-1,4-二亚硝基苯、2-甲氧基-1-3-二亚硝基苯、5-氯-1,3-二亚硝基苯、2-苄基-1,4-二亚硝基苯、2-环己基-1,4-二亚硝基苯和它们的组合。特别优选的亚硝基化合物包括对二亚硝基苯和间二亚硝基苯。
就本发明的目的而言,能够作为亚硝基化合物交联剂的亚硝基化合物前体基本上可以为在升高的温度(通常为大约120℃至200℃的范围)下能够被转化(通常通过氧化)为亚硝基化合物的任意化合物。最常见的亚硝基化合物前体为醌化合物的衍生物。可用作本发明的亚硝基化合物前体的醌化合物衍生物的实例包括醌二肟、二苯并醌二肟、1,2,4,5-四氯苯醌、2-甲基-l,4-苯并醌二肟、1,4-萘并醌二肟、1,2-萘并醌二肟、以及2,6-萘并醌二肟。
在本发明的另一个实施方案中,弹性体底胶组合物任选地包含酸清除化合物,用于清除在粘结过程中产生的任何酸性化合物副产物。酸清除化合物优选为金属氧化物或含铅化合物。本发明的金属氧化物可以为任何已知的金属氧化物,例如锌、镉、镁、铅和锆的氧化物;一氧化铅;四氧化三铅;锆盐;以及它们的组合。代替金属氧化物或者除了金属氧化物以外,多种含铅化合物还可以用作酸清除化合物。此类含铅化合物的实例包括铅盐,例如磷酸、饱和的和不饱和的有机二羧酸和酸酐的多元铅盐。铅盐的具体实例包括两部分邻苯二甲酸铅、三元马来酸铅一水合物、四元富马酸铅、两部分亚磷酸铅和它们的组合。含铅化合物的其他实例包括碱式碳酸铅、一氧化铅和铅二氧化铅。就本发明的目的而言,由于环境原因,金属氧化物优选于含铅化合物。
在本发明的另一个实施方案中,本发明的弹性体底胶组合物还可以包含马来酰亚胺化合物交联剂。马来酰亚胺化合物交联剂基本上可以为包含至少2个马来酰亚胺基的任何化合物。马来酰亚胺基可以彼此相连,或者可以连接到中间的二价基团中并被中间的二价基团分开,其中所述的中间的二价基团例如为亚烷基、环亚烷基、环氧二亚甲基、亚苯基(所有3个异构体)、2,6-二亚甲基-4-烷基苯酚或磺酰基。其中马来酰亚胺基与亚苯基相连的马来酰亚胺化合物的实例为间亚苯基双马来酰亚胺,可得自E.I.Du Pont de Nemours&Co的HVA-2。
在本发明的另一个实施方案中,本发明的基底粘合剂和弹性体底胶组合物都可任选地包含一定量的其他公知的添加剂,包括增塑剂、填料、颜料、表面活性剂、分散剂、润湿剂、增强剂等,其中所述的量可以使得粘合剂领域中的技术人员获得所需的颜色和一致性。任选的组分的实例包括炭黑、二氧化硅(例如气相二氧化硅)、铝硅酸钠和二氧化钛。
实施例
在以下实施例中,根据美国专利号5,268,404制备弹性体底胶,其包含氯磺化聚乙烯、氯化天然橡胶、二亚硝基苯、有机溶剂或水,以及任选地包含酸清除剂、聚双马来酰亚胺化合物、氯化石蜡、环氧树脂清漆、硒和炭黑中的一种或多种。这些弹性体底胶在实施例中命名为EP-1至EP-7。基底粘合剂A为EEW/AHEW比值(环氧当量与胺氢当量的重量比值)为0.8至1.2的胺固化的环氧粘合剂。
然后,如在标准的橡胶粘结测试方法ASTM D 429中所概括的那样,对粘结的试件进行牵拉测试。所报告的结果的学术名词包括:R=表示橡胶失效;RC=表示在橡胶/橡胶-底胶的界面处失效;CP=表示在橡胶-底胶/基底-粘合剂的界面处失效;M=表示在基底/基底-粘合剂的界面处失效。混合结果表示在牵引失效模式之间分开时,失效的表面积百分比,例如50%R、50%RC表示50%的橡胶保持在试件上,50%的试件不具有橡胶,而基底粘合剂保持在试件上的失效模式。强力粘结可得到的测试结果为100%的R或者接近100%的R。
试验1-使用EP-1和环氧树脂SA-A进行PV粘结的评价
使用刷子将EP-1施加到1”x5”x1/4”硫化橡胶试件的中心部分上,其中所述的硫化橡胶试件首先已经用异丙醇(IPA)擦拭,从而除去了任何松散的表面污染物。将EP-1在室温下干燥稍稍超过2小时。将E涂覆的不锈钢试件(1”x5”)进行掩蔽,以暴露1”x1”的中心区域。将SA-A分布在不锈钢试件的上述中心区域上,然后使用0.030”的不锈钢垫片(用于控制粘结层的厚度)将不锈钢试件放置在制备好的橡胶试件上。将成对的样品放置于热压机中,并仅采用设定于≤300℉的温度从上方加热。在压制中使用垫片以助于控制板的缝隙。固化时间≤5分钟。
然后,将样品放置于120℃的烘箱中进行调理,以用于120℃牵拉测试。使样品在上述温度下平衡大约30分钟。在从烘箱中移除样品后,即刻以90°至180°之间的牵拉角度由加热的试件上牵拉橡胶。
固化时间研究:
固化时间 | 在120℃下失效 |
4分钟 | 100%R |
3分钟 | 100%R |
2分钟 | 100%R |
注意到一些SA-A粘合剂被挤出粘结层,并且在4分钟时未完全固化,在3分钟和2分钟时未固化。
更高的牵拉温度研究(标准试件制备,5分钟固化时间)
牵拉温度 | 失效模式 |
120℃ | 100%R |
130℃ | 90%R,10%E-C |
140℃ | 20%R,80%E-C |
150℃ | 20%R,80%E-C |
试验2-在用SA-A的PV RTM粘结中对EP-2、EP-3和EP-4的评价
按照之前所述制备样品,并在300℉下采用5分钟的固化时间粘结,其中弹性体底胶施加到橡胶上而SA-A施加到e涂覆的钢上。然后,将样品加热至120°用于测试。
所用的弹性体底胶 | 失效模式 |
EP-2 | 100%R |
EP-3 | 100%R |
EP-4 | 100%R |
试验3-在PV RTM粘结中对250℉固化温度的评价
按照之前所述制备样品,并将SA-A施加在e涂覆的钢试件上,在250℉下粘结5分钟,然后在室温下和在120℃下进行牵拉测试。
所用的弹性体底胶 | RT失效模式 | 120℃失效模式 |
EP-5 | 5%R,95%RC | 100%R |
EP-6 | 70%R,30%RC* | 100%R |
EP-1 | 5%R,95%RC | 100%R |
EP-7 | 5%R,95%RC | 100%R |
EP-2 | 100%RC | 20%R,80%RC |
EP-3 | 100%RC | 100%R |
*该样品具有更长的固化时间(大约8分钟)。
试验4-在使用SA-A的PV粘结中对EP-6的评价
使用EP-6作为弹性体底胶,使用SA-A作为基底粘合剂,按照之前所述来制备样品。将样品在以下所示的温度下进行固化,然后在室温下进行牵拉测试。
*牵拉强度较低。
试验5-在PV粘结中对SA-A膜厚度的评价
使用SA-A作为基底粘合剂,使用EP-1作为弹性体底胶,按照之前所述来制备样品。EP-1干膜的目标厚度为1-2密尔。将成对的试件在仅由不锈钢一侧加热的300℉的印压机中加热,固化时间为5分钟。施加各个水平的压力以试图减小SA-A粘结层的厚度。使样品在室温下干燥,然后以90°角牵拉。接着,以横截面切割不锈钢试件,并使用数字显微镜以200x放大倍数下测量粘合剂膜的厚度。
*难以分辨SA-A层。
注意:在所有情况下,EP-1层均为~2密尔厚。
试验6-在PV粘结中使用聚氨酯化学成分作为基底粘合剂
按照之前所述制备样品,用2种聚氨酯基粘合剂(SA-B和SA-C)替代环氧基SA-A,并按如下测试。使聚氨酯粘合剂在室温(RT–20℃+/-5℃)下在成对的组件中固化至不同的程度,然后在300℉下进行热固化。
试验7-将橡胶粘结在碳纤维复合材料基底上
将复合材料试件的发亮光滑的一侧磨损/砂磨,然后掩蔽1”x1”的区域。使用IPA擦拭硫化橡胶试件,并施加EP-1薄层(1-2密尔DFT),再使其在室温下干燥。将SA-A施加到复合材料试件的掩蔽区域,然后使用0.030”不锈钢垫片(用于控制粘结层的厚度)与橡胶成对。将一个试件立刻在≤300℉下固化8分钟。将另一个试件在室温下固化>24小时,然后在8分钟内加热至≤300℉。在冷却至室温后,牵拉橡胶。两个试件均产生100%R的撕裂失效,表明橡胶与复合材料基底之间的优异粘合。
试验8-环境测试
共同使用3种不同的橡胶样品,测试粘结试件的环境抗性,其中所述的3种不同的橡胶样品包括橡胶A和橡胶B(购自天然橡胶配制物)、以及HC-130(自制的天然橡胶配制物)。使用镀锌磷化钢试件作为基底,在用二甲苯擦拭后准备好橡胶,然后以1.5密尔的DFT来施加所示的橡胶底胶。施加SA-A粘合剂,并且一旦粘结层达到300℉便将组件固化5分钟。
测试粘结试件的初始粘合性,其中所述的粘合试件经历7天的挂盐水喷雾,4小时的加压沸水,在250℉热拔下15分钟的烘箱浸泡(oven soak),在0℉下1周,在200℉下在加压的Plurasafe 800中1周的浸没,以及在200℉下在加压的ASTM Oil#3中1周的浸没。结果如下所示:
Claims (17)
1.一种用于弹性体的硫化后粘结的方法,包括:
(a)提供硫化弹性体;
(b)将弹性体底胶组合物施加到所述的硫化弹性体,其中所述的弹性体底胶组合物包含卤化聚烯烃和二亚硝基苯;
(c)提供待粘结的基底;
(d)将环氧基基底粘合剂施加到所述的基底;
(e)使经所述弹性体底胶涂覆的硫化弹性体与经所述的基底粘合剂涂覆的基底相接触,使得环氧粘合剂的至少一部分与卤化聚烯烃底胶的至少一部分相接触,从而形成组件。
2.权利要求1所述的方法,其中所述的卤化聚烯烃是溴化聚(二氯丁二烯)。
3.权利要求1所述的方法,其中所述的卤化聚烯烃是氯化天然橡胶。
4.权利要求1所述的方法,其中所述的卤化聚烯烃是氯磺化聚乙烯。
5.权利要求1所述的方法,其中所述的二亚硝基苯是聚二亚硝基苯。
6.权利要求1所述的方法,其中所述的基底粘合剂包含环氧基粘合剂,并且进一步包含胺类硬化剂。
7.权利要求1所述的方法,其中所述的基底粘合剂除了酚醛环氧材料以外,基本不含或者不含酚醛树脂。
8.权利要求1所述的方法,其中所述的基底粘合剂基本不含或者不含卤化聚烯烃。
9.权利要求1所述的方法,其中所述的弹性体底胶除了酚醛环氧材料以外,基本不含或者不含环氧树脂。
10.权利要求1所述的方法,其中所述的弹性体底胶基本不含或者不含酚醛树脂。
11.权利要求1所述的方法,其中所述的弹性体底胶包含双马来酰亚胺材料。
12.权利要求1所述的方法,其中所述的弹性体底胶包含溶剂基底胶。
13.权利要求1所述的方法,其中所述的弹性体底胶包含水性底胶。
14.权利要求1所述的方法,其中当根据ASTM D 429在高于100℃的温度下以90°角牵拉所述的粘结组件时,该粘结组件表现出至少90%的橡胶保持率。
15.权利要求14所述的方法,其还包括加热所述的组件,从而固化所述的弹性体底胶的步骤(f)。
16.权利要求15所述的方法,其中将所述的组件加热到至少250℉,持续5分钟。
17.权利要求1所述的方法,其中在未实施预处理步骤的条件下将所述的弹性体底胶施加到所述的弹性体。
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PCT/US2013/052074 WO2014018761A1 (en) | 2012-07-25 | 2013-07-25 | Improved post-vulcanization bonding |
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MY187105A (en) * | 2015-06-30 | 2021-08-31 | Henkel Ag & Co Kgaa | "process for cold bonding rubber on metal substrates" |
CN109642011B (zh) * | 2016-07-11 | 2022-01-14 | 陶氏环球技术有限责任公司 | 高固体含量的基于溶剂的粘着剂组合物和其制造方法 |
IT201800006059A1 (it) * | 2018-06-06 | 2019-12-06 | Composizione adesiva per gomma vulcanizzata | |
CN113402930A (zh) * | 2021-07-21 | 2021-09-17 | 南京宇松材料科技有限公司 | 一种密封防护橡胶涂料及其制备方法 |
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US20140030513A1 (en) | 2014-01-30 |
JP2015527442A (ja) | 2015-09-17 |
US20180333934A1 (en) | 2018-11-22 |
CN104718259A (zh) | 2015-06-17 |
JP6281954B2 (ja) | 2018-02-21 |
KR20150038330A (ko) | 2015-04-08 |
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EP2877544A1 (en) | 2015-06-03 |
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