CN103210050A - 异丁烯(共)聚合物型粘合剂组合物 - Google Patents
异丁烯(共)聚合物型粘合剂组合物 Download PDFInfo
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- CN103210050A CN103210050A CN2011800539543A CN201180053954A CN103210050A CN 103210050 A CN103210050 A CN 103210050A CN 2011800539543 A CN2011800539543 A CN 2011800539543A CN 201180053954 A CN201180053954 A CN 201180053954A CN 103210050 A CN103210050 A CN 103210050A
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Abstract
本发明描述了一种粘合剂组合物,所述粘合剂组合物包含a)非官能化异丁烯(共)聚合物,b)胺-官能化聚(异丁烯)聚合物,可任选地为酸官能化(甲基)丙烯酸酯共聚物并且可任选地为增粘剂。
Description
相关专利申请的交叉引用
本专利申请要求2010年11月17日提交的美国临时专利申请No.61/414492的优先权,所述专利申请的公开内容全文以引用方式并入本文。
技术领域
本发明涉及由异丁烯共聚物制备的压敏粘合剂和粘合密封剂,以及由其制备的胶带制品。压敏粘合剂的特征在于,对于低表面能基材和经受湿、湿润或潮湿环境的基材表现出粘合和内聚特性的总体平衡和出色的粘附力。
背景技术
压敏胶带在家庭和工作场所中几乎随处可见。在压敏胶带的最简单的构造中,其包括粘合剂和背衬,且整体构造在使用温度下是粘性的,并且仅使用适度的压力便可以粘附至多种基材以形成结合。以此方式,压敏胶带构成了完整自持的结合***。
根据压敏胶带协会,已知压敏粘合剂(PSA)具有以下性质:(1)有力而持久的粘着力;(2)用不超过指压的压力即可粘附;(3)具有足够固定在粘附体上的能力;以及(4)足够的内聚强度,使其可干净地从粘附体上移除。已发现的可很好地用作PSA的材料包括经设计和配制以表现出所需粘弹特性的聚合物,所述粘弹特性可实现所期望的粘着力、剥离粘附力与剪切保持力的平衡。PSA的特征在于通常在室温(例如20℃)下是发粘的。PSA不包括仅具有粘性或仅能够附着到某种表面上的组合物。
通常使用设计用来逐个地测量粘着力、粘附力(剥离强度)和内聚力(剪切保持力)的测试方法来评估这些要求,如A.V.Pocius在由俄亥俄州辛辛那提汉瑟加德纳出版社(Hanser Gardner Publication,Cincinnati,OH)于2002年出版的Adhesion and Adhesives Technology:An Introduction(粘附和粘合剂技术:概论)(第2版)中所指明的那样。这些量度合在一起构成了通常用于表征PSA的诸性质的平衡。
如今存在多种可得的压敏粘合剂(PSA)材料,其包括天然未加工或合成橡胶、嵌段共聚物和丙烯酸酯基聚合物组合物。对于所有PSA极为重要的是粘附力和内聚力的所需平衡,所述平衡常常通过优化粘合剂的物理性质(如玻璃化转变温度和模量)而实现。例如,如果弹性体的玻璃化转变温度(Tg)或模量过高,并高于粘性的Dahlquist标准(在室温和1Hz的振动频率下3×106达因/cm2的储能模量),则所述材料将不是粘性,且本身不可用作PSA材料。通常在这种情况中,低分子量高Tg树脂聚合物(增粘剂)或低分子量低Tg聚合物(增塑剂)常用于将Tg和模量调节至最佳PSA范围内。
发明内容
本公开的粘合剂组合物包含a)非官能化异丁烯(共)聚合物,b)胺-官能化聚(异丁烯)聚合物,可任选地为酸-官能化(甲基)丙烯酸酯共聚物,可任选地为增粘剂并且可任选地为增塑剂。
本发明的压敏粘合剂提供所需的粘着力、剥离粘附力和剪切保持力的平衡,且还符合Dahlquist标准;即,频率为1Hz时,粘合剂在涂敷温度(通常室温)下的模量小于3×106达因/厘米。
在一些实施例中,本公开提供附着到湿、湿润或潮湿环境中的表面上的压敏粘合剂(所谓的“湿粘”粘合剂),该压敏粘合剂可用于选定的工业、商业和消费应用中。在医药和其他医疗领域中,此类湿粘粘合剂通常用于将诸如胶带、绷带、敷料和盖布之类的制品附着到潮湿皮肤表面(如伤口或易于变湿的身体区域)。湿粘粘合剂也可发现用于室外或外部应用,例如道路材料、交通管制标牌以及船舶或汽车的涂层和表面。暴露于水分(由于冷凝或经受水或冰浸渍而引起)的食品容器和其他产品的标签也必须用湿粘粘合剂涂覆。本文所用的“湿粘粘合剂”是指当粘附到已在随后暴露于水或高湿度的基材上时,表现出压敏粘合剂性质的材料。
近年来,低表面能、烯烃型热塑性塑料(如聚乙烯、聚丙烯、乙烯丙烯双烯单体橡胶(EPDM))在汽车、油漆、器具和电子器件市场中的使用显著增加。该新材料的优点包括成本较低、易于加工和优异的机械性能。然而,这种趋势在对这些低表面能表面进行粘合剂粘合方面带来了一定的挑战。
最近,聚(异丁烯)(PIB)和其他异丁烯共聚物(如异丁烯-异戊二烯共聚物)已被认为是低表面能(LSE)粘合应用的受欢迎材料,因为其对于烯烃型热塑性塑料具有优异的粘附性质。另外,PIB出色的水分和氧气阻隔性表明PIB型材料在电子和光伏封装应用中具有潜在用途。尽管它具有有益的性质,但材料的低内聚强度限制了它在高剪切应用中的用途。PIB型材料的另一个可能的应用是医用粘合剂领域。大部分丙烯酸酯型PSA不适用于医学应用,因为丙烯酸酯PSA在高温下往往会散发有毒蒸汽。丙烯酸酯型PSA通常包含即使在通常的室温下也会散发气味的单体材料,这使得丙烯酸酯PSA胶带一般不适用于医学用途。聚(异丁烯)PSA通常用于医学用途,因为它们是生理惰性的,但它们在内部强度方面也往往不足。
本发明的粘合剂组合物提供了改进的压敏粘合剂组合物,其可以在很宽的温度范围内粘附到包括低表面能(LSE)的基材以及处于湿、湿润或潮湿环境中的基材在内的多种基材上,并提供了良好的粘附强度和保持特性。本发明的粘合剂组合物还提供了压敏粘合剂制品,例如胶带和密封剂。在多个实施例中,粘合剂提供良好的阻隔性涂层、多种PIB聚合物的特征性,但由于高内聚强度可将其从基材中干净地去除。
如本文所用
“烷基”是指具有一至约十二个碳原子的直链或支链、环状或无环的饱和单价烃基,如甲基、乙基、1-丙基、2-丙基、戊基等。
“亚烷基”是指具有一至约十二个碳原子的直链饱和二价烃基或具有三至约十二个碳原子的支链饱和二价烃基,如亚甲基、亚乙基、亚丙基、2-甲基亚丙基、亚戊基、亚己基等。
“芳基”是指单价芳族,例如苯基、萘基等。
“亚芳基”是指多价芳族,例如亚苯基、萘等。
“亚芳烷基”是指连接有芳基基团的上述定义的亚烷基,如苄基、1-萘乙基等。
具体实施方式
本公开的粘合剂组合物包含a)非官能化异丁烯(共)聚合物,b)胺-官能化聚(异丁烯)聚合物,任选地为酸-官能化(甲基)丙烯酸酯共聚物,可任选地为增粘剂并且可任选地为增塑剂。如本文所用,术语“异丁烯(共)聚合物”是指异丁烯聚合物和共聚物的合成橡胶,并且包括(但不限于)聚(异丁烯)和异丁烯-异戊二烯共聚物。
粘合剂组合物包含至少一个非官能化异丁烯(共)聚合物型合成橡胶材料。非官能化异丁烯(共)聚合物型合成橡胶通常为具有聚异丁烯主链或侧链的树脂。在一些实施例中,异丁烯(共)聚合物基本上为异丁烯的均聚物,例如,可以商品名OPPANOL(BASF AG)和GLISSOPAL(BASF AG)获得的聚(异丁烯)树脂。在一些实施例中,异丁烯(共)聚合物型树脂包含异丁烯的共聚物,例如,其中异丁烯与另一种单体共聚的合成橡胶。合成橡胶包括丁基橡胶,该丁基橡胶是大部分异丁烯与少量异戊二烯的共聚物,例如,可以商品名VISTANEX(埃克森化学公司(Exxon Chemical Co.))和JSR BUTYL(日本丁基聚合物有限公司(Japan Butyl Co.,Ltd.))获得的丁基橡胶。合成橡胶还包括大部分异丁烯与正丁烯或丁二烯的共聚物。在一些实施例中,可使用异丁烯均聚物和丁基橡胶的混合物,即第一聚异丁烯包含异丁烯的均聚物,而第二聚异丁烯包含丁基橡胶;或第一聚异丁烯包含丁基橡胶,而第二聚异丁烯包含异丁烯的均聚物。
非官能化异丁烯(共)聚合物型合成橡胶(如PIB)材料通常具有显著高于胺-官能化(如PIB)合成橡胶材料的分子量(如下文进一步所述)。在一些实施例中,非官能化异丁烯(共)聚合物型合成橡胶(如PIB)的重均分子量(Mw)为至少35,000克/摩尔、至少100,000克/摩尔、至少250,000克/摩尔、至少500,000克/摩尔或甚至至少1,000,000克/摩尔。重均分子量通常不大于4,000,000克/摩尔。
非官能化异丁烯(共)聚合物型合成橡胶可为均聚物、共聚物或它们的混合物。共聚物可为无规共聚物或嵌段共聚物。嵌段共聚物可在聚合物的主链、侧链或主链和侧链两者中含有聚异丁烯部分。通常通过在存在诸如氯化铝、三氯化硼(四氯化钛作为助催化剂)或三氟化硼的路易斯酸催化剂的情况下,单独地聚合异丁烯或聚合异丁烯外加烯键式不饱和单体(例如异戊二烯)来制备聚异丁烯材料。
非官能化异丁烯(共)聚合物型橡胶可从多个制造商处商购获得。均聚物可(例如)以商品名OPPANOL(例如,OPPANOL B10、B15、B30、B50、B80、B100、B150和B200)从新泽西州弗洛勒姆帕克的巴斯夫公司(BASF Corp.(Florham Park,NJ))商购获得。这些聚合物的重均分子量(Mw)通常在约35,000至4,000,000克/摩尔的范围内。其他示例性的均聚物可以宽泛的分子量范围商购自UnitedChemical Products(UCP)(St.Petersburg,Russia)。例如,以商品名SDG商购自UCP的均聚物的粘均分子量(Mv)在约35,000至65,000克/摩尔的范围内。以商品名EFROLEN商购自UCP的均聚物的粘均分子量(Mv)在约480,000至约4,000,000克/摩尔的范围内。以商品名JHY商购自UCP的均聚物的粘均分子量在约3000克/摩尔至约55,000克/摩尔的范围内。这些均聚物通常不具有反应性双键。应意识到未官能化(如PIB)合成橡胶可具有极小浓度的反应性双键或其聚合残基的其他官能团。此类反应性双键或其他官能团的浓度通常小于5、4、3或2mo1%。此类烯属不饱和基团也通常不是经由自由基聚合形成共价键的合适官能团。
压敏粘合剂组合物中非官能化异丁烯(共)聚合物型合成橡胶材料的浓度通常大于50重量%、优选大于60重量%、优选为65至80重量%。
粘合剂组合物还包含胺-官能化聚(异丁烯)聚合物。胺官能团可为端基。胺官能团可形成键合至酸官能共聚物的酸性基团(如侧羧酸基团)的氢。因此,此类官能团不形成共价键。具有非极性共价键的官能团不形成氢键。
在一些实施例中,胺-官能化聚异丁烯聚合物为异丁烯的胺-官能化均聚物,即聚(异丁烯)。在其他实施例中,官能化聚异丁烯聚合物可为共聚物,该共聚物包含异丁烯重复单元和少量的衍生自具有胺官能团的另一单体(例如胺-官能化苯乙烯、异戊二烯、丁烯或丁二烯)的单元。这些共聚物通常由单体混合物制备,所述单体混合物包含基于单体混合物中的单体重量计至少70重量%、至少75重量%、至少80重量%、至少85重量%、至少90重量%、或至少95重量%的异丁烯。示例性的共聚物包括与异戊二烯共聚的异丁烯。
胺-官能化聚(异丁烯)可由以下通式表示
其中
R1为异丁烯和其他任选单体单元(如上所述)的聚合物链,具有5至100个重复单元,并且R2和R3独立地选自H、C1-C10-烷基或芳基基团。
胺官能化聚异丁烯通常为具有较低至中等数均(Mn)分子量的液态聚合物。Mn通常为至少500克/摩尔、750克/摩尔或约1,000克/摩尔。在一些实施例中,官能化聚异丁烯的Mn不大于25,000克/摩尔,或10,000克/摩尔,或5,000克/摩尔。在其他实施例中,据信,具有较高分子量的胺-官能化聚(异丁烯)混合物会增大剥离值并减少移除时的残余物。
根据差示扫描量热法(DSC)测定,胺官能化聚异丁烯的玻璃化转变温度通常不大于约-30℃或更低,不大于约-50℃,或不大于约-65℃。
可通过U.S.4,832,702(Kummer等人)中描述的方法来制备胺官能化PIB,其中先羰基化聚异丁烯,然后使所得羰化产物经受还原胺化或曼尼希反应。更具体地讲,胺-官能化聚异丁烯可通过以下方式制备:在存在CO和H2、温度为80至200℃且CO/H2的压力最多为600巴的情况下,用铑或钴催化剂羰基化合适的聚异丁烯,然后使羰化产物经受曼尼希反应或在加氢条件下胺化。胺化反应有利地在80至200℃且在最多至600巴(60MPa)(优选80至300巴)的压力下进行。
在制备过程中,有利的是,使用合适的惰性溶剂以降低反应混合物的粘度。特别合适的溶剂为具有低硫含量的脂族、脂环族和芳族烃。尤其优选不含硫化合物且含有小于1%芳烃的脂族溶剂。它们的优点是,在高胺化温度下,不释放氢化热且不消耗氢。在胺化和羰基化反应中,根据聚合物和溶剂的粘度,溶剂含量为0至70重量%。更大的稀释度就像羰化反应和胺化之间的溶剂变化那样是不经济的。
在Kummer等人的方法中,可以容易地实现80至90%的聚丁烯转化。可包含丁烷和异丁烯单元两者的聚丁烯的分子量MN为例如300-5000,优选为500至2500。
多种胺官能化PIB材料可商购获得。例如,聚(异丁烯)胺(Mn为约1,000克/摩尔并且摩尔质量分布Mw/Mn=1.6)可以商品名“KerocomTM PIBA03”从新泽西州弗洛勒姆帕克的巴斯夫公司(BASFCorporation(Florham Park,NJ))商购获得。
胺官能化PIB材料内的胺官能团的存在和浓度可通过质子核磁共振来确定。通常,官能化PIB材料包含至少3摩尔%的胺官能团。胺官能团的浓度通常不大于10摩尔%。
粘合剂组合物中胺官能化PIB材料的量可根据粘合剂组合物的所需最终用途而变化。然而,相对于总的粘合剂组合物而言,官能化PIB材料的浓度通常为胺-官能化聚(异丁烯)聚合物的0.25至20重量%,优选为1至15重量%,以提高对于高表面能基材(例如湿、湿润或潮湿环境下的玻璃或瓷)的粘附力。已经发现的是,向基于异丁烯(共)聚合物的粘合剂加入少量的胺-官能化聚异丁烯会保持暴露于湿润或湿度环境的粘合基材的剥离强度。当暴露于相同环境时,粘合有增粘异丁烯(共)聚合物型粘合剂但不包含胺-官能化聚异丁烯的基材显示出显著降低的剥离强度。
粘合剂组合物还可任选地包含酸-官能化(甲基)丙烯酸酯共聚物,该酸-官能化(甲基)丙烯酸酯共聚物包含(甲基)丙烯酸酯单体和酸-官能化单体的共聚单体单元。
用于制备酸-官能化(甲基)丙烯酸酯粘合剂共聚物的(甲基)丙烯酸酯单体为非叔醇的单体(甲基)丙烯酸酯,所述醇包含1至14个碳原子,并且优选包含平均4至12个碳原子。
适用作(甲基)丙烯酸酯单体的单体的例子包括丙烯酸或甲基丙烯酸与非叔醇的酯,所述非叔醇为例如乙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、1-戊醇、2-戊醇、3-戊醇、2-甲基-1-丁醇、3-甲基-1-丁醇、1-己醇、2-己醇、2-甲基-1-戊醇、3-甲基-1-戊醇、2-乙基-1-丁醇、3,5,5-三甲基-1-己醇、3-庚醇、1-辛醇、2-辛醇、异辛醇、2-乙基-1-己醇、1-癸醇、2-丙基庚醇、1-十二烷醇、1-十三烷醇、1-十四烷醇、香茅醇、二氢香茅醇等等。在一些实施例中,优选的(甲基)丙烯酸酯单体是(甲基)丙烯酸与丁醇或异辛醇或它们的组合的酯,但是两种或更多种不同的(甲基)丙烯酸酯单体的组合也是合适的。在一些实施例中,优选的(甲基)丙烯酸酯单体是(甲基)丙烯酸与衍生自可再生资源的醇(例如2-辛醇、香茅醇或二氢香茅醇)的酯。
在一些实施例中,希望(甲基)丙烯酸酯单体包括高Tg单体,具有至少25℃,并且优选至少50℃的Tg。合适的高Tg单体的例子包括(但不限于)丙烯酸叔丁酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸异丙酯、甲基丙烯酸正丁酯、甲基丙烯酸异丁酯、甲基丙烯酸仲丁酯、甲基丙烯酸叔丁酯、甲基丙烯酸硬脂酯、甲基丙烯酸苯酯、甲基丙烯酸环己酯、丙烯酸异冰片酯、甲基丙烯酸异冰片酯、甲基丙烯酸苄酯、丙烯酸3,3,5三甲基环己酯、丙烯酸环己酯、N-辛基丙烯酰胺和甲基丙烯酸丙酯或其组合。
以用于制备聚合物的100份总单体重量计,(甲基)丙烯酸酯单体的存在量为85至99.5重量份。优选的是,按100份总单体重量计,(甲基)丙烯酸酯单体的存在量为90至99重量份。在包含高Tg单体时,共聚物可包含85至99.5重量份(甲基)丙烯酸酯单体组分的最多至30重量份、优选最多至20重量份。
所述聚合物还包含酸官能化单体,其中的酸官能团可以是酸本身,如羧酸,或者一部分可以是其盐,如碱金属羧酸盐。可用的酸官能单体包括(但不限于)选自烯键式不饱和羧酸、烯键式不饱和磺酸、烯键式不饱和膦酸、以及它们的混合物的那些。这种化合物的例子包括选自丙烯酸、甲基丙烯酸、衣康酸、富马酸、巴豆酸、柠康酸、马来酸、油酸、(甲基)丙烯酸β-羧乙酯、甲基丙烯酸2-磺乙酯、苯乙烯磺酸、2-丙烯酰胺基-2-甲基丙磺酸、乙烯基膦酸以及它们的混合物的那些。
出于可获性的原因,酸官能化共聚物的酸官能化单体通常选自烯键式不饱和羧酸,即(甲基)丙烯酸。当需要更强的酸时,酸性单体包括烯键式不饱和磺酸和烯键式不饱和膦酸。按100重量份酸官能化共聚物的总单体计,所述酸官能化单体通常以0.5至15重量份,优选0.5至10重量份的量使用。
可用于制备共聚物的可选极性单体多少有些油溶性且多少有些水溶性,从而导致极性单体在乳液聚合中分布在水相与油相之间。如本文所用,术语“极性单体”不包括酸官能化单体。
合适的极性单体的代表性例子包括但不限于:(甲基)丙烯酸2-羟乙酯;N-乙烯基吡咯烷酮;N-乙烯基己内酰胺;丙烯酰胺;单-或二-N-烷基取代的丙烯酰胺;叔丁基丙烯酰胺;二甲氨基乙基丙烯酰胺;N-辛基丙烯酰胺;聚(烷氧基烷基)(甲基)丙烯酸酯,包括(甲基)丙烯酸2-(2-乙氧基乙氧基)乙酯、(甲基)丙烯酸2-乙氧基乙酯、(甲基)丙烯酸2-甲氧基乙氧基乙酯、甲基丙烯酸2-甲氧基乙酯、聚乙二醇单(甲基)丙烯酸酯;烷基乙烯基醚,包括乙烯基甲基醚;以及它们的混合物。优选的极性单体包括选自(甲基)丙烯酸2-羟乙酯和N-乙烯基吡咯烷酮的那些。按100重量份酸官能化共聚物的总单体计,极性单体可以0至10重量份、在一些实施例中以0.5至5重量份的量存在。
可用于(甲基)丙烯酸酯聚合物的可选乙烯基单体包括乙烯基酯(例如乙酸乙烯酯和丙酸乙烯酯)、苯乙烯、取代的苯乙烯(例如α-甲基苯乙烯)、乙烯基卤化物以及它们的混合物。如本文所用,乙烯基单体不包括酸官能化单体、丙烯酸酯单体和极性单体。按100重量份酸官能化共聚物的总单体计,此类乙烯基单体的用量通常为0至5重量份、在一些实施例中为1至5重量份。
在此类实施例中,(甲基)丙烯酸共聚物可包含:
i.80至99.5重量份的非叔醇的(甲基)丙烯酸酯;
iii.0.5至15重量份的酸官能化烯键式不饱和单体;
iv.0至10重量份的非酸官能化烯键式不饱和极性单体;
v.0至5份的乙烯基单体;和
vi.0至5份的多官能(甲基)丙烯酸酯;
按100重量份(甲基)丙烯酸酯共聚物或酸官能化共聚物的总单体计。
为了提高涂覆的粘合剂组合物的内聚强度,可将多官能(甲基)丙烯酸酯掺入到可聚合单体的共混物中。多官能丙烯酸酯特别可用于乳液或浆料聚合。可用的多官能(甲基)丙烯酸酯的例子包括(但不限于)二(甲基)丙烯酸酯、三(甲基)丙烯酸酯和四(甲基)丙烯酸酯,如1,6-己二醇二(甲基)丙烯酸酯、聚(乙二醇)二(甲基)丙烯酸酯、聚丁二烯二(甲基)丙烯酸酯、聚氨酯二(甲基)丙烯酸酯和丙氧基化甘油三(甲基)丙烯酸酯以及它们的混合物。多官能(甲基)丙烯酸酯的量和种类取决于粘合剂组合物的应用来定制。通常,按粘合剂组合物的总干重计,多官能(甲基)丙烯酸酯以小于5份的量存在。更具体地讲,按100份酸官能化共聚物的总单体计,交联剂可以以0.01至5份,或0.05至1份的量存在。
粘合剂组合物通常包含0至10重量%的酸官能化(甲基)丙烯酸酯共聚物。加入少量(即小于10重量%)的酸官能化(甲基)丙烯酸酯共聚物会提高对极性基材的粘合强度。高于约10重量%,粘合剂组合物会在移除时留下不期望的残余物,或使得粘合持久。本公开的粘合剂可有利地从基材上移除并且不留下任何明显的残余物。在某些实施例中,粘合剂组合物可包含0.5至5重量%的酸官能化(甲基)丙烯酸酯共聚物。
常规的粘合剂对某些基材(例如某些类型的汽车油漆和低能表面)不良好粘附。已努力改进粘合剂的粘附力,即发展对这些类型的表面更有力的粘性;常常实施将基体聚合物增粘。各种类型的增粘剂包括酚改性的萜烯、烃类树脂(如聚乙烯基环己烷和聚(叔丁基苯乙烯)),和松香酯(如松香的甘油酯和松香的季戊四醇酯)。
各种类型的增粘剂包括酚改性的萜烯和松香酯,例如可以商品名NurozTM、NutacTM(纽卜特工业有限公司(Newport Industries))、PermalynTM、StaybeliteTM、ForalTM(伊士曼公司(Eastman))得到的松香的甘油酯和松香的季戊四醇酯。通常来自石油脑裂解的C5和C9单体副产物的烃类树脂增粘剂也可得到,并可以商品名PiccotacTM、EastotacTM、RegalrezTM、RegaliteTM(伊士曼公司(Eastman))、ArkonTM(荒川公司(Arakawa))、NorsoleneTM、WingtackTM(克雷威利公司(Cray Valley))、Nevtack、LX(内维尔化学公司(Neville ChemicalCo.))、HikotackTM、HikorezTM(可隆化学公司(Kolon Chemical))、NovaresTM(罗格斯N.V.公司(Rutgers N.V.))、QuintoneTM(瑞翁公司(Zeon))、EscorezTM(埃克森美孚化工公司(ExxonmobileChemical))、NuresTM和H-RezTM(纽卜特工业有限公司(NewportIndustries))得到。
在许多实施例中,本发明提供了克服本领域中所述的问题的经增粘的粘合剂组合物。所述增粘剂优选选自基本上不含任何烯键式不饱和键或炔键式不饱和键的材料。所述增粘剂包括但不限于氢化松香树脂、氢化和酯化的松香树脂、氢化萜烯树脂、脂族石油树脂、芳族石油树脂、通过氢化芳族石油树脂而获得的脂环族石油树脂等。优选地,所用的增粘剂选自氢化的C9石油树脂,例如但不限于EscorezTM增粘剂(埃克森美孚公司(ExxonMobile))、RegalrezTM增粘剂(伊士曼公司(Eastman))或ArkonTM增粘剂(荒川公司(Arakawa))。相对于粘合剂组合物的总重量而言,此类“疏水性增粘剂”可以0至40重量%,优选1至40重量%的增粘剂的量在粘合剂组合物中使用。在某些优选实施例中,胺官能化PIB和增粘剂的结合量为25至35重量%。
增塑剂也可以用于粘合剂配方中,以提供润湿作用和/或粘度控制。这些增塑剂在本领域中是熟知的,并且可以包括烃油;液态或柔软的增粘剂,包括液态烃类树脂、液态聚萜烯、液态聚(异丁烯)诸如GlissopalTM等;蜡;以及油的混合物。增塑剂可以以0至约200重量份/100重量份粘合剂组合物的量存在于本发明的压敏粘合剂中。
本发明的粘合剂可使用常规涂覆技术涂覆在多种柔性和非柔性背衬材料上以制成粘合剂涂覆的材料。柔性基底在本文中定义为通常用作胶带背衬或可具有任何其它柔性材料的任何材料。例子包括(但不限于)塑料薄膜,例如聚丙烯、聚乙烯、乙烯醋酸乙烯酯(EVA)、聚氯乙烯、聚酯(聚对苯二甲酸乙二醇酯)、聚碳酸酯、聚甲基(甲基)丙烯酸酯(PMMA)、醋酸纤维素、三乙酸纤维素和乙基纤维素。可使用泡沫背衬。非柔性基材的例子包括(但不限于)金属、金属化聚合物薄膜、铟锡氧化物涂覆的玻璃和聚酯、PMMA板、聚碳酸酯板、玻璃或陶瓷片状材料。粘合剂涂覆的片状材料可采用常规已知能够与粘合剂组合物一起使用的任何制品形式,例如标签、胶带、指示牌、封面、标记标志、显示组件、触摸面板等等。也可设想具有微复制表面的柔性背衬材料。
取决于基材待用于的特定应用而选择基材。例如,可将粘合剂施用至薄膜、片材产品(例如装饰性图形和反射性产品)、标签纸(labelstock)和胶带背衬。另外,可将粘合剂直接施用至基材(如汽车面板或玻璃窗口)上,使得另一基材或物体可被附接至所述面板或窗口。
本发明的粘合剂可特别用于形成对低表面能(LSE)基材的强结合。本文所用的低表面能基材为表面能小于约45达因/厘米,更通常小于约40达因/厘米,最通常小于约35达因/厘米的那些。诸如聚丙烯之类的低能量基材通常具有大于约20达因/厘米的表面能。聚丙烯、聚乙烯(例如高密度聚乙烯或HDPE)、聚苯乙烯和聚(甲基丙烯酸甲酯)(PMMA)包括在这种材料中。其他基材也可由于在基材的表面上有残余物(如油状残余物)或薄膜(如涂料)的原因而具有低表面能性质。
然而,即使本发明的粘合剂良好地粘合于低表面能表面,本发明也不局限于粘合至低表面能基材,因为已发现,本发明的粘合剂也可良好地粘合于较高表面能的基材,例如其他塑料、陶瓷、瓷、玻璃和金属。具体地讲,粘合剂组合物可用于粘合至暴露于水分或高湿度的高表面能基材。已经发现的是,即使在此类暴露之后,粘合的基材仍保持显著/足够的剥离强度。
粘附至湿、湿润或潮湿环境中的表面上的本发明的压敏粘合剂可用于多种工业、商业和消费应用中。这些湿粘粘合剂在涉及粘合至暴露于湿、湿润或潮湿条件下的表面的应用中可能有用。此类表面常常存在于浴室中,包括淋浴器或浴缸内的表面。这些湿粘粘合剂也可用于医疗应用中,例如粘附至潮湿皮肤表面(如伤口或易于变湿的身体区域)的胶带、绷带、敷料和盖布。另外,湿粘粘合剂也可发现用于室外或外部应用,例如道路材料、交通管制标牌、室外遮蔽胶带、室外管道胶带以及船舶或汽车的涂层和表面。此外,暴露于水分(由于冷凝或经受水或冰浸渍而引起)的食品容器和其他产品的标签也必须用湿粘粘合剂涂覆。
粘合剂也可以以压敏粘合剂转移胶带的形式提供,其中粘合剂的至少一层设置于剥离衬垫上以用于在以后施用至第二基材。粘合剂也可作为单一涂布或双涂布的胶带提供,其中粘合剂设置于持久背衬上。背衬可由塑料(例如聚丙烯(包括双轴取向的聚丙烯)、乙烯基、聚乙烯、乙烯醋酸乙烯酯(EVA)、聚酯(如聚对苯二甲酸乙二醇酯))、非织造物(例如纸、布、非织造稀松布)、金属箔、泡沫(例如聚丙烯酸类、聚乙烯、聚氨酯、氯丁橡胶)等制成。
泡沫可购自各种供应商,如3M Co.,Voltek,Sekisui和其他。泡沫可成型为共挤出的片材,所述片材在泡沫的一侧或两侧上具有粘合剂,或者粘合剂可被层合至所述片材。当粘合剂被层合至泡沫时,可能有利的是处理表面以改进粘合剂对泡沫或对任何其他类型的背衬的粘附力。这种处理通常基于粘合剂的材料的性质和泡沫或背衬的性质进行选择,并包括底漆和表面改性(例如电晕处理、表面磨损)。另外的胶带构造包括描述于U.S.5,602,221(Bennett等人)的那些,所述专利以引用方式并入本文。本领域的技术人员还将会知道,可以将其他添加剂(例如填料、抗氧化剂、稳定剂和着色剂)与粘合剂共混,以获得有益的性质。
对于单侧胶带,与设置粘合剂之处相对的背衬表面的侧面通常涂布有合适的剥离材料。剥离材料是已知的,并包括例如有机硅、聚乙烯、聚氨基甲酸酯、聚丙烯酸类等的材料。对于双涂布胶带,另一粘合剂层设置于与本发明的粘合剂设置之处相对的背衬表面上。另一粘合剂层可不同于本发明的粘合剂,例如,常规丙烯酸类PSA,或者其可为具有相同或不同配方的与本发明相同的粘合剂。双涂布的胶带通常承载在剥离衬垫上。
采用改进得适用于具体基材的常规的涂覆技术,将上述组合物涂覆在基材上。例如,可通过诸如辊涂、流涂、浸涂、旋涂、喷涂、刮涂和压模涂覆之类的方法将这些组合物涂覆至各种固体基材。这些多种多样的涂覆方法可以将这些组合物按照不同厚度涂覆在基材上,从而使得这些组合物得到更广泛的应用。涂层的厚度可以有差别,但是可设想2至500微米(干燥厚度),优选约25至250微米的涂层厚度。
实例
以下非限制性实例进一步描述本发明的示例性粘合剂和粘合剂制品,以及制备此类粘合剂和粘合剂制品的示例性方法。所有百分比均按重量计,除非另外指明。除非另外指明,所使用的溶剂及其他试剂均购自威斯康辛州密尔沃基的奥尔德里奇化学公司(Aldrich ChemicalCompany(Milwaukee,WI))。
表1:材料
粘合剂的制备
通过混合如表2中指定的合适材料成分来制备粘合剂。参见表1获取所用材料成分的描述。除非另外指明,否则混合容器为广口玻璃瓶。所有聚异丁烯聚合物被用作甲苯溶液。将M1和M2溶解在甲苯中从而得到10重量%的溶液。将M0和M3溶解在甲苯中从而得到20重量%的溶液。M6被用作乙酸乙酯/庚烷中的28%固体混合物。向粘合剂制剂中加入所提供的M5和M7。向粘合剂制剂中加入作为白色固体的M4。加入所有成分之后,用特氟隆带衬金属帽、特氟隆胶带和SCOTCH牌电工胶带密封粘合剂制剂的广口瓶,并在环境温度下通过在辊上滚动16小时将其混合。然后使用刮刀式涂胶机将粘合剂溶液涂覆到S7上。将含有涂覆溶液的S7的样品贴在薄铝板上,并将该薄铝板放置在烘箱中于50℃下干燥15分钟,然后于70℃下干燥30分钟。然后允许将S7上的干燥粘合剂涂层在恒温/恒湿房间(50%相对湿度和23℃)中均衡约24小时,之后将S8剥离衬垫层合至粘合剂的顶部。除非另有说明,否则粘合剂的干燥涂层厚度为101至114微米(4至4.5密耳)。
在进行淋浴测试之前,将粘合剂层合至S6。从提供的辊上切下S6的一部分并将其扣紧到工作台顶部。从粘合剂样品上移除S8衬垫,然后将粘合剂侧小心地放置在S6表面上。然后用塑料卡片挤出气泡。然后在413至551kPa(60至80psi.)下层合S6/粘合剂/S7构造的2.54cm(1英寸)宽的胶带。然后允许将样品在环境温度下存放至少一小时,之后将其切割为约12.7至15.4cm(5至6英寸)长×2.54cm(1英寸)宽的胶带。
测试方法:
90°角剥离粘附强度测试
如ASTM国际标准D3330中的方法F所述,用5.08cm×15.2cm(2英寸×6英寸)试件和IMASS SP-2000滑动/剥离试验机(得自马萨诸塞州阿科德的IMASS公司(IMASS,Inc.,Accord,MA))以及11.34Kg(25磅)测力传感器以432毫米/分钟(17英寸/分钟)的剥离速率进行90°角剥离粘附强度评价。使用2秒延迟在90度下执行剥离测试。剥离速率为43.18cm(17英寸)/分钟并且该数据为20秒以上的平均值。通过用2.0kg(4.5磅)的橡胶辊在胶带上滚动4次将样品粘附到测试基材上。
通过在表面上喷涂乙醇,然后使用纸巾将表面擦拭干净来清洁测试基材。根据需要移除的残余物的量将其清洗2至4次。
从测试胶带中移除S7,然后通过用4.5磅的辊滚动两次将S6/粘合剂样品层合至测试基材。将测试胶带层合至每个5.08cm×15.2cm×0.635cm(2英寸×6英寸)基材。然后允许将样品存放30分钟,之后将其放置在淋浴室中,该淋浴室为样品置于其中并经受指定环境条件的封装件。在7.252kPa(50psi.)的压力下,向淋浴室中的46.67℃(116℉)的基材喷水。在淋浴室中测得的温度为35.55℃(96℉)。
使样品在淋浴室中停留约18至24小时,在该时间之后将其取出并用纸巾轻轻干燥。然后在将其从淋浴室中取出的5分钟之内在粘合剂样品上执行剥离测试。基于2个试样,从基材上移除胶带所需的平均剥离粘附力以盎司测量,并以盎司/英寸表示。所得结果列于表3中。
表2
表3:
实例号 | S1玻璃 | S2瓷 | S3丙烯酸类树脂 | S4聚乙烯 | S5不锈钢 |
对照物1 | 0.8 | ||||
对照物2 | 1.1 | ||||
对照物3 | 0.1 | ||||
对照物4 | 0.5 | ||||
对照物5 | 3 | 1 | 65 | ||
实例1 | 52 | ||||
实例2 | 81 | ||||
实例3 | 73 | ||||
实例4 | 28 | 20 | 38 | ||
实例5 | 21 | 12 | 70 | ||
实例6 | 28 | 24 | 33 | ||
实例7 | 43 | 25 | 33 | 36 | 44 |
实例8 | 29 | 20 | 32 | 22 | 38 |
实例9 | 28 | 13 | 37 | 16 | 34 |
由下面的实施例进一步说明本公开:
1.一种粘合剂组合物,包含:
a)大于50重量%的非官能化异丁烯(共)聚合物,
b)0.25至20重量%的胺官能化聚(异丁烯)聚合物,
c)0至10重量%的酸官能化(甲基)丙烯酸酯共聚物,
d)0至40重量%的增粘剂;和
e)0至40重量%的增塑剂。
2.实施例1的粘合剂组合物包含0重量%的酸官能化(甲基)丙烯酸酯共聚物。
3.实施例1的粘合剂组合物包含0.5至5重量%的酸官能化(甲基)丙烯酸酯共聚物。
4.实施例1的粘合剂组合物包含组合的25至35重量%的胺-官能化聚(异丁烯)聚合物和增粘剂。
5.实施例1的粘合剂组合物,其中酸-官能化(甲基)丙烯酸酯共聚物包含80至99重量%的(甲基)丙烯酸酯单体和1至20重量%的酸-官能化单体。
6.实施例1至5中任一者的粘合剂组合物,其中所述胺-官能化聚(异丁烯)聚合物具有小于10,000克/摩尔的数均分子量。
7.实施例1至6中任一者的粘合剂组合物,其中(甲基)丙烯酸酯单体为C4至C20(甲基)丙烯酸酯单体。
8.实施例7的压敏粘合剂组合物,其中(甲基)丙烯酸酯单体为C4至C8(甲基)丙烯酸酯单体。
9.前述实施例中任一者的粘合剂组合物还包含增粘树脂、增塑剂或其混合物。
10.前述实施例中任一者的粘合剂组合物在室温和1Hz的摆动频率下具有3×106达因/厘米2的储能模量。
11.实施例1的粘合剂组合物,其中胺-官能化聚(异丁烯)聚合物由以下通式表示:
其中
R1为具有5至100个重复单元的异丁烯的聚合物自由基,并
且R2和R3独立地选自H、C1-C10-烷基或芳基基团。
12.前述实施例中任一者的粘合剂组合物包含1至15重量%的胺-官能化聚(异丁烯)聚合物。
13.前述实施例中任一者的粘合剂组合物包含1至40重量%的增粘剂。
14.一种制品,其包括:基材;和
实施例1至13中任一者的压敏粘合剂,该压敏粘合剂涂覆在基材的至少一个表面上。
15.实施例14的制品,其中基材以聚合物薄膜基材的形式。
16.实施例14的制品,其中基材以非织造基材的形式。
17.一种粘合方法,包括:
提供基材;
在基材的表面上施加实施例1至13中任一者的粘合剂;以及
使粘合剂与另一个基材接触。
18.实施例17的方法,其中基材具有小于37达因/厘米的表面能。
19.实施例17的方法,其中基材随后暴露于潮湿、湿润或湿度条件下。
20.一种制备压敏粘合剂的方法,该方法包括共混:
a)大于50重量%的非官能化异丁烯(共)聚合物,
b)0.25至20重量%的胺-官能化聚(异丁烯)聚合物,
c)0至10重量%的酸-官能化(甲基)丙烯酸酯共聚物,
d)0至40重量%的增粘剂;和
e)0至40重量%的增塑剂。
Claims (20)
1.一种粘合剂组合物,包含:
a)大于50重量%的非官能化异丁烯(共)聚合物,
b)0.25重量%至20重量%的胺-官能化聚(异丁烯)聚合物,
c)0重量%至10重量%的酸官能化(甲基)丙烯酸酯共聚物,
d)0重量%至40重量%的增粘剂;和
e)0重量%至40重量%的增塑剂。
2.根据权利要求1所述的粘合剂组合物包含0重量%的酸官能化(甲基)丙烯酸酯共聚物。
3.根据权利要求1所述的粘合剂组合物包含0.5重量%至5重量%的酸官能化(甲基)丙烯酸酯共聚物。
4.根据权利要求1所述的粘合剂组合物包含组合的25重量%至35重量%的胺-官能化聚(异丁烯)聚合物和增粘剂。
5.根据权利要求1所述的粘合剂组合物,其中所述酸官能化(甲基)丙烯酸酯共聚物包含80重量%至99重量%的(甲基)丙烯酸酯单体和1重量%至20重量%的酸官能化单体。
6.根据权利要求1所述的粘合剂组合物,其中所述胺官能化聚(异丁烯)聚合物具有小于10,000克/摩尔的数均分子量。
7.根据权利要求1所述的粘合剂组合物,其中所述(甲基)丙烯酸酯单体为C4至C20(甲基)丙烯酸酯单体。
8.根据权利要求7所述的压敏粘合剂组合物,其中所述(甲基)丙烯酸酯单体为C4至C8(甲基)丙烯酸酯单体。
9.根据权利要求1所述的粘合剂组合物,还包含增粘树脂、增塑剂或其混合物。
10.根据权利要求1所述的粘合剂组合物,所述粘合剂组合物在室温和1Hz的摆动频率下具有3×106达因/厘米2的储能模量。
11.根据权利要求1所述的粘合剂组合物,其中所述胺-官能化聚(异丁烯)聚合物由以下通式表示:
其中
R1为具有5至100个重复单元的异丁烯的聚合物自由基,并且R2和R3独立地选自H、C1-C10-烷基或芳基基团。
12.根据权利要求1所述的粘合剂组合物包含1重量%至15重量%的胺-官能化聚(异丁烯)聚合物。
13.根据权利要求1所述的粘合剂组合物包含1重量%至40重量%的增粘剂。
14.一种制品,其包括:
基材;和
涂覆在所述基材的至少一个表面上的根据权利要求1所述的压敏粘合剂。
15.根据权利要求14所述的制品,其中所述基材以聚合物薄膜基材的形式。
16.根据权利要求14所述的制品,其中所述基材以非织造基材的形式。
17.一种粘合方法,包括:
提供基材;
在所述基材的表面上施加根据权利要求1所述的粘合剂;和使所述粘合剂与另一个基材接触。
18.根据权利要求17所述的方法,其中所述基材具有小于37达因/厘米的表面能。
19.根据权利要求17所述的方法,其中所述基材随后暴露于湿、湿润或潮湿条件下。
20.一种制备压敏粘合剂的方法,所述方法包括共混:
a)大于50重量%的非官能化异丁烯(共)聚合物,
b)0.25重量%至20重量%的胺-官能化聚(异丁烯)聚合物,
c)0重量%至10重量%的酸-官能化(甲基)丙烯酸酯共聚物,
d)0重量%至40重量%的增粘剂;和
e)0重量%至40重量%的增塑剂。
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US61/414,492 | 2010-11-17 | ||
US13/282,500 US20120122359A1 (en) | 2010-11-16 | 2011-10-27 | Ionically crosslinkable poly(isobutylene) adhesive polymers |
US13/282,500 | 2011-10-27 | ||
PCT/US2011/059867 WO2012078292A1 (en) | 2010-11-17 | 2011-11-09 | Isobutylene (co)polymeric adhesive composition |
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CN103210050A true CN103210050A (zh) | 2013-07-17 |
CN103210050B CN103210050B (zh) | 2015-04-29 |
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EP (1) | EP2640794B1 (zh) |
JP (1) | JP2014502299A (zh) |
KR (1) | KR101910209B1 (zh) |
CN (1) | CN103210050B (zh) |
WO (1) | WO2012078292A1 (zh) |
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KR101910209B1 (ko) | 2018-10-19 |
KR20130119942A (ko) | 2013-11-01 |
US20140162517A1 (en) | 2014-06-12 |
US20120118469A1 (en) | 2012-05-17 |
EP2640794B1 (en) | 2015-02-25 |
JP2014502299A (ja) | 2014-01-30 |
US8663407B2 (en) | 2014-03-04 |
CN103210050B (zh) | 2015-04-29 |
WO2012078292A1 (en) | 2012-06-14 |
EP2640794A1 (en) | 2013-09-25 |
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