CN116426229A - 包括至少一种丙烯腈-丁二烯橡胶的基于聚(甲基)丙烯酸酯的压敏胶粘剂 - Google Patents
包括至少一种丙烯腈-丁二烯橡胶的基于聚(甲基)丙烯酸酯的压敏胶粘剂 Download PDFInfo
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- CN116426229A CN116426229A CN202310031654.XA CN202310031654A CN116426229A CN 116426229 A CN116426229 A CN 116426229A CN 202310031654 A CN202310031654 A CN 202310031654A CN 116426229 A CN116426229 A CN 116426229A
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- acrylate
- sensitive adhesive
- pressure sensitive
- acrylonitrile
- meth
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Abstract
本发明涉及压敏胶粘剂,其包括至少一种聚(甲基)丙烯酸酯;和至少一种丙烯腈‑丁二烯橡胶,其中所述至少一种丙烯腈‑丁二烯橡胶以1至49重量%存在,基于压敏胶粘剂的总重量。本发明还涉及本发明的压敏胶粘剂的制造,以及本发明的压敏胶粘剂用于粘合电子设备的部件或汽车中的部件的用途。最后,本发明涉及胶带,其包括至少一个根据本发明的压敏胶粘剂的层。
Description
技术领域
本发明涉及压敏胶粘剂,其包括
-至少一种聚(甲基)丙烯酸酯;和
-至少一种丙烯腈-丁二烯橡胶,其中
所述至少一种丙烯腈-丁二烯橡胶以1至49重量%存在,基于压敏胶粘剂的总重量。本发明还涉及本发明的压敏胶粘剂的制造、以及本发明的压敏胶粘剂用于粘合电子设备的部件或汽车中的部件的用途。最后,本发明涉及包括至少一个根据本发明的压敏胶粘剂的层的胶带。
背景技术
压敏胶粘剂(PSA)在现有技术中是已知的。例如,DE 102013215297 A1描述了基于聚(甲基)丙烯酸酯与至少一种合成橡胶和至少一种与一种或多种聚(甲基)丙烯酸酯相容的增粘剂的PSA。然而,这类PSA具有差的耐化学性,例如相对于油酸。
具有耐化学性的PSA例如描述于WO 2017/025492A1中。然而,它们基于丙烯腈-丁二烯橡胶。但是,这样的胶粘剂具有低的内聚力。
发明内容
因此,本发明的目的是提供基于聚(甲基)丙烯酸酯的压敏胶粘剂,其不仅表现出高的耐化学性,特别是对油酸的耐化学性,而且表现出高的剪切强度。
令人惊讶地,所述目的通过本发明的压敏胶粘剂,更特别地通过基于聚(甲基)丙烯酸酯的化合物与1至49重量%的至少一种丙烯腈-丁二烯橡胶的组合得以实现。
本发明的第一总主题是压敏胶粘剂,其包括
-至少一种聚(甲基)丙烯酸酯;和
-至少一种丙烯腈-丁二烯橡胶,其中
所述至少一种丙烯腈-丁二烯橡胶以1至49重量%、优选地10至45重量%、更优选地20至45重量%存在,基于压敏胶粘剂的总重量。
本发明的第二方面是用于制造根据本发明的压敏胶粘剂的方法,其中所述制造包括通过配混和挤出设备,并且所述方法是连续工艺。
在第三方面,本发明涉及根据本发明的压敏胶粘剂用于粘合电子设备的部件或汽车中的部件的用途。
在第四方面,本发明涉及包括至少一个根据本发明的压敏胶粘剂的层的胶带。
附图说明
图1示出由其获得玻璃化转变温度的温谱图。
具体实施方式
如通常的一般说法,根据本发明的压敏胶粘剂或PSA是至少在室温下是永久粘性和胶粘性的物质。压敏胶粘剂的特征在于,它可通过压力施加至基材并在其上保持粘附,而无需具体定义施加的压力和该压力的作用的持续时间。通常,但基本上取决于压敏胶粘剂的确切性质、温度和空气湿度、以及基材,不超过短暂时间的温和接触的短暂最小压力的作用足以实现粘合效果;在其他情况下,在较高压力下的作用较长的持续时间也可为必要的。
压敏胶粘剂具有特定的特征性粘弹性性质,其导致持续的粘性和胶粘性。这些的特征是,如果它们机械形变,存在粘性流动过程和弹性恢复力的形成两者。所述两种过程就它们相应的比例而言彼此具有特定的比率,既取决于PSA的确切组成、结构和交联水平,也取决于形变的速率和持续时间,以及取决于温度。
粘性流动分量(组分)对于粘附性的实现是必要的。仅通常由具有相对高迁移性的大分子产生的粘性分量使得能够良好地润湿待粘合的基材和对待粘合的基材良好的流动。高的粘性流动的比例导致高的压敏粘性(也称为粘性或表面粘性),并因此常常也导致高的粘附性。高度交联的体系、结晶聚合物或以玻璃状形式固化的聚合物由于缺乏自由流动的分量而通常不是粘性的或至少仅具有很小的粘性。
弹性恢复力分量(组分)是内聚性的实现所需要的。这些力例如由非常长链且高卷曲度的大分子以及由物理或化学交联的大分子导致,并且使得能够传递作用在胶粘粘合上的力。它们具有以下效果:胶粘粘合可在长的时间段内承受作用在其上的持续应力(例如以持续剪切应力的形式)至足够的程度。
为了更精确地描述和量化弹性和粘性分量的程度、以及所述分量相对于彼此的比率,引入借助于动态机械分析(动态力学分析,DMA)可测定的储能模量(G')和损耗模量(G")的参数。G'是物质的弹性分量的量度,G"是物质的粘性分量的量度。两个参数都取决于形变频率和温度。
所述参数可借助流变仪确定。在此,待检查的材料例如在板-板装置中经受正弦振荡的剪切应力。在剪切应力控制的仪器中,测量作为时间的函数的形变、以及相对于剪切应力的引入的在时间上的该形变的偏移。该在时间上的偏移被称为相位角δ。
储能模量G'如下定义:G'=(τ/γ)·cos(δ)(τ=剪切应力,γ=形变,δ=相位角=剪切应力向量和形变向量之间的相位移)。损耗模量G"的定义如下:G”=(τ/γ)·sin(δ)(τ=剪切应力,γ=形变,δ=相位角=剪切应力向量和形变向量之间的相位移)。
当在23℃下,在100至101rad/秒的形变频率范围内G'和G"两者都至少部分地在103至107Pa的范围内时,胶粘剂尤其被认为是压敏胶粘剂并且特别地就本发明而言是如此定义的。“部分地”意味着,G'曲线的至少一部分(段)在由100至101rad/秒(包括端点)的形变频率范围(横坐标)和103至107Pa(包括端点)的G'值的范围(纵坐标)限定的窗口之内,并且G"曲线的至少一部分同样在相应的窗口内。
“聚(甲基)丙烯酸酯”理解为是指通过丙烯酸类单体和/或甲基丙烯酸类单体以及任选地其他可共聚单体的自由基聚合而获得的聚合物。更特别地,“聚(甲基)丙烯酸酯”理解为指具有如下的单体基础物的聚合物,所述单体基础物在至少50重量%的程度上由丙烯酸、甲基丙烯酸、丙烯酸酯和/或甲基丙烯酸酯组成,其中丙烯酸酯和/或甲基丙烯酸酯至少部分地、优选以至少30重量%的程度存在,基于所讨论的聚合物的总单体基础物。
本发明的压敏胶粘剂优选地以≥40重量%、更优选45至99重量%、特别地48至70重量%包括聚(甲基)丙烯酸酯,在各自的情况下基于压敏胶粘剂的总重量。可存在单一的聚(甲基)丙烯酸酯或多种聚(甲基)丙烯酸酯,并且当存在多种聚(甲基)丙烯酸酯时,表述“压敏胶粘剂以…重量%包括聚(甲基)丙烯酸酯”当然是指“压敏胶粘剂包括总计…重量%的聚(甲基)丙烯酸酯”。
本发明的压敏胶粘剂中的聚(甲基)丙烯酸酯的玻璃化转变温度优选<0℃、更优选在-5和-50℃之间。根据本发明通过动态扫描量热法(DSC)测定聚合物或嵌段共聚物中聚合物嵌段的玻璃化转变温度。为此,将约5mg未处理的聚合物样品称重到铝舟(体积25μl)中,并用穿孔的盖子封闭。使用来自Netzsch的DSC 204F1进行测量。采用氮气气氛进行惰化。首先将样品冷却至-150℃,然后以10K/分钟的加热速率加热至+150℃,再次冷却至-150℃。随后的第二加热曲线再次以10K/分钟运行,并记录热容的变化。玻璃化转变被认为是温谱图中的台阶。
玻璃化转变温度如下获得(参见图1):
在台阶之前和之后的测量曲线的相应线性区域在上升温度(台阶之前的区域)或下降温度(台阶之后的区域)的方向上延伸(切线①和②)。在台阶的区域中,最佳拟合线⑤与纵坐标平行,使得其与两条切线相交,特别地以形成两个相等的区域③和④(在相应的切线、最佳拟合线和测量曲线之间)的方式。由此定位的最佳拟合线与测量曲线的交点给出玻璃化转变温度。
本发明的压敏胶粘剂中的聚(甲基)丙烯酸酯优选地包括至少一种按比例共聚的官能单体,其更优选地为与环氧基团反应性的以形成共价键。最优选地,按比例共聚的官能单体(其更优选地为与环氧基团反应性的以形成共价键)包含至少一个选自以下的官能团:羧酸基团、磺酸基团、膦酸基团、羟基、酸酐基团、环氧基团和氨基;它尤其包含至少一个羧酸基团。极优选地,本发明的压敏胶粘剂中的聚(甲基)丙烯酸酯包含按比例共聚的丙烯酸和/或甲基丙烯酸。所有提到的基团具有与环氧基团的反应性,这意味着聚(甲基)丙烯酸酯有利地适于与引入的环氧化物热交联。
本发明的压敏胶粘剂中的聚(甲基)丙烯酸酯可优选地基于以下单体组成:
a)至少一种下式(1)的丙烯酸酯和/或甲基丙烯酸酯
CH2=C(RI)(COORII) (1)
其中RI=H或CH3,并且RII为具有4至18个碳原子的烷基;
b)至少一种烯属不饱和单体,其具有至少一个选自以下的官能团:羧酸基团、磺酸基团、膦酸基团、羟基、酸酐基团、环氧基团和氨基;
c)任选地可与组分(a)共聚的另外的丙烯酸酯和/或甲基丙烯酸酯和/或烯属不饱和单体。
特别有利的是选择具有45至99重量%的比例的组分(a)的单体、具有1至15重量%的比例的组分(b)的单体、以及具有0至40重量%的比例的组分(c)的单体,其中所述数字基于没有添加任何添加剂例如树脂的对于基础聚合物的单体混合物。
组分(a)的单体通常为增塑的、相对非极性的单体。更优选地,单体a)中的RII是具有4至10个碳原子的烷基或丙烯酸2-丙基庚酯或甲基丙烯酸2-丙基庚酯。式(1)的单体尤其选自丙烯酸正丁酯、甲基丙烯酸正丁酯、丙烯酸正戊酯、甲基丙烯酸正戊酯、丙烯酸正戊基酯、丙烯酸正己酯、甲基丙烯酸正己酯、丙烯酸正庚酯、丙烯酸正辛酯、甲基丙烯酸正辛酯、丙烯酸正壬酯、丙烯酸异丁酯、丙烯酸异辛酯、甲基丙烯酸异辛酯、丙烯酸2-乙基己酯、甲基丙烯酸2-乙基己酯、丙烯酸2-丙基庚酯和甲基丙烯酸2-丙基庚酯。
组分(b)的单体更优选地选自丙烯酸、甲基丙烯酸、衣康酸、马来酸、富马酸、巴豆酸、乌头酸、二甲基丙烯酸、β-丙烯酰氧基丙酸、三氯丙烯酸、乙烯基乙酸、乙烯基膦酸、马来酸酐、丙烯酸羟基乙酯、特别地丙烯酸2-羟基乙酯、丙烯酸羟基丙酯、特别地丙烯酸3-羟基丙酯、丙烯酸羟基丁酯、特别地丙烯酸4-羟基丁酯、丙烯酸羟基己酯、特别地丙烯酸6-羟基己酯、甲基丙烯酸羟基乙酯、特别地甲基丙烯酸2-羟基乙酯、甲基丙烯酸羟基丙酯、特别地甲基丙烯酸3-羟基丙酯、甲基丙烯酸羟基丁酯、特别地甲基丙烯酸4-羟基丁酯、甲基丙烯酸羟基己酯、特别地甲基丙烯酸6-羟基己酯、烯丙基醇、丙烯酸缩水甘油酯、甲基丙烯酸缩水甘油酯。
说明性的组分(c)的单体如下:
丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、丙烯酸苄基酯、甲基丙烯酸苄基酯、丙烯酸仲丁酯、丙烯酸叔丁酯、丙烯酸苯基酯、甲基丙烯酸苯基酯、丙烯酸异冰片基酯、甲基丙烯酸异冰片基酯、丙烯酸叔丁基苯基酯、甲基丙烯酸叔丁基苯基酯、甲基丙烯酸十二烷基酯、丙烯酸异癸酯、丙烯酸月桂酯、丙烯酸正十一烷基酯、丙烯酸硬脂基酯、丙烯酸十三烷基酯、丙烯酸二十二烷基酯、甲基丙烯酸环己酯、甲基丙烯酸环戊酯、丙烯酸苯氧基乙酯、甲基丙烯酸苯氧基乙酯、甲基丙烯酸2-丁氧基乙酯、丙烯酸2-丁氧基乙酯、丙烯酸3,3,5-三甲基环己酯、丙烯酸3,5-二甲基金刚烷基酯、甲基丙烯酸4-枯基苯基酯、丙烯酸氰基乙酯、甲基丙烯酸氰基乙酯、丙烯酸4-联苯基酯、甲基丙烯酸4-联苯基酯、丙烯酸2-萘基酯、甲基丙烯酸2-萘基酯、丙烯酸四氢糠基酯、丙烯酸二乙基氨基乙酯、甲基丙烯酸二乙基氨基乙酯、丙烯酸二甲基氨基乙酯、甲基丙烯酸二甲基氨基乙酯、3-甲氧基丙烯酸甲酯、丙烯酸3-甲氧基丁酯、甲基丙烯酸2-苯氧基乙酯、丁基二甘醇甲基丙烯酸酯、乙二醇丙烯酸酯、乙二醇单甲基醚丙烯酸酯、甲氧基聚乙二醇甲基丙烯酸酯350、甲氧基聚乙二醇甲基丙烯酸酯500、丙二醇单甲基丙烯酸酯、丁氧基二甘醇甲基丙烯酸酯、乙氧基三甘醇甲基丙烯酸酯、丙烯酸八氟戊酯、甲基丙烯酸八氟戊酯、甲基丙烯酸2,2,2-三氟乙酯、丙烯酸1,1,1,3,3,3-六氟异丙酯、甲基丙烯酸1,1,1,3,3,3-六氟异丙酯、甲基丙烯酸2,2,3,3,3-五氟丙酯、甲基丙烯酸2,2,3,4,4,4-六氟丁酯、丙烯酸2,2,3,3,4,4,4-七氟丁酯、甲基丙烯酸2,2,3,3,4,4,4-七氟丁酯、甲基丙烯酸2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-十五氟辛酯、二甲基氨基丙基丙烯酰胺、二甲基氨基丙基甲基丙烯酰胺、N-(1-甲基十一烷基)丙烯酰胺、N-(正丁氧基甲基)丙烯酰胺、N-(丁氧基甲基)甲基丙烯酰胺、N-(乙氧基甲基)丙烯酰胺、N-(正十八烷基)丙烯酰胺;N,N-二烷基取代的酰胺,例如N,N-二甲基丙烯酰胺和N,N-二甲基甲基丙烯酰胺;N-苄基丙烯酰胺、N-异丙基丙烯酰胺、N-叔丁基丙烯酰胺、N-叔辛基丙烯酰胺、N-羟甲基丙烯酰胺、N-羟甲基甲基丙烯酰胺、丙烯腈、甲基丙烯腈、乙烯基醚如乙烯基甲基醚、乙基乙烯基醚、乙烯基异丁基醚;乙烯基酯如乙酸乙烯酯;乙烯基卤化物、偏卤乙烯、乙烯基吡啶、4-乙烯基吡啶、N-乙烯基邻苯二甲酰亚胺、N-乙烯基内酰胺、N-乙烯基吡咯烷酮、苯乙烯、α-甲基苯乙烯和对甲基苯乙烯、α-丁基苯乙烯、4-正丁基苯乙烯、4-正癸基苯乙烯、3,4-二甲氧基苯乙烯;大分子单体如2-聚苯乙烯乙基甲基丙烯酸酯(甲基丙烯酸2-聚苯乙烯乙酯)(4000-13 000g/mol的重均分子量Mw,通过GPC测定)、聚(甲基丙烯酸甲酯)乙基甲基丙烯酸酯(甲基丙烯酸聚(甲基丙烯酸甲酯)乙酯)(2000-8000g/mol的Mw)。
组分(c)的单体也可有利地选择成使得它们包含帮助随后的辐射化学交联(例如通过电子束、UV)的官能团。合适的可共聚的光引发剂为例如苯偶姻丙烯酸酯和丙烯酸酯官能化的二苯甲酮衍生物。帮助通过电子轰击的交联的单体为例如丙烯酸四氢糠基酯、N-叔丁基丙烯酰胺和丙烯酸烯丙酯。
聚(甲基)丙烯酸酯的制备优选通过常规的自由基聚合或受控自由基聚合进行。聚(甲基)丙烯酸酯可通过如下制备:使用惯常的聚合引发剂以及任选地链转移剂使单体共聚,其通过在惯常的温度下以本体、在乳液中例如在水或液体烃中、或在溶液中的聚合。
聚(甲基)丙烯酸酯优选地通过如下制备:在溶剂中,更优选地在具有50-150℃、特别地60-120℃的沸程的溶剂中,使用0.01至5重量%、尤其是0.1至2重量%(在各自的情况下基于单体的总重量)的聚合引发剂,使单体共聚。
所有惯常的引发剂原则上是合适的。自由基源的实例是过氧化物、氢过氧化物和偶氮化合物,例如过氧化二苯甲酰、氢过氧化枯烯、过氧化环己酮、二叔丁基过氧化物、环己基磺酰基乙酰基过氧化物、过碳酸二异丙酯、过辛酸叔丁酯和苯频哪醇。优选的自由基引发剂是2,2'-偶氮双(2-甲基丁腈)(来自DuPont的67TM)或2,2'-偶氮双(2-甲基丙腈)(2,2'-偶氮二异丁腈;AIBN;来自DuPont的/>64TM)。
优选的用于制备聚(甲基)丙烯酸酯的溶剂是醇如甲醇、乙醇、正丙醇和异丙醇、正丁醇和异丁醇,尤其是异丙醇和/或异丁醇,烃如甲苯,并且特别地具有60至120℃的沸程的挥发油(溶剂油);酮,尤其是丙酮、甲乙酮、甲基异丁基酮,酯例如乙酸乙酯,以及前述溶剂的混合物。特别优选的溶剂是以2至15重量%、特别地3至10重量%的量包含异丙醇的混合物,在各情况下基于所用的溶剂混合物。
优选地,聚(甲基)丙烯酸酯的制造(聚合)之后是浓缩步骤,并且聚(甲基)丙烯酸酯的进一步处理是基本上无溶剂的。聚合物的浓缩可在不存在交联剂和促进剂物质的情况下进行。然而,也可甚至在浓缩之前向聚合物添加这些化合物类别之一,使得浓缩于是在这种/这些物质的存在下进行。
在浓缩步骤后,可将聚合物转移到配混机中。浓缩和混合也可任选地在相同(同一)反应器中进行。
聚丙烯酸酯的重均分子量Mw优选地在20 000-2 000 000g/mol的范围内;非常优选地在100 000-1 500 000g/mol的范围内,特别优选地在150 000-1 000 000g/mol的范围内。为此,如下可为有利的:在合适的聚合链转移剂如硫醇、卤素化合物和/或醇的存在下进行聚合,以建立所需的平均分子量。
本文中的数均摩尔质量Mn和重均摩尔质量Mw数字涉及通过凝胶渗透色谱(GPC)的测定,其本身是已知的。对100μl的经澄清过滤的样品(样品浓度4g/l)进行测定。使用的洗脱剂是具有0.1体积%的三氟乙酸的四氢呋喃。在25℃下进行测量。
使用的预柱是如下的柱:PSS-SDV型,5μm,8.0mm*50mm(此处及下面的陈述按照以下顺序:类型,颗粒尺寸,孔隙度,内径*长度;/>=10-10m)。使用如下的柱的组合进行分离:PSS-SDV型,5μm,/>以及/>和/>各自具有8.0mm×300mm(来自PolymerStandards Service的柱;借助于Shodex RI71差示折射仪进行检测)。流速为1.0ml/分钟。在聚(甲基)丙烯酸酯的情况下,针对PMMA标准物进行校准(聚甲基丙烯酸甲酯校准),否则(树脂、弹性体)针对PS标准物进行校准(聚苯乙烯校准)。
聚(甲基)丙烯酸酯优选地具有30至90、更优选地40至70的在甲苯(1%溶液,21℃)中测量的K值。Fikentscher的K值是聚合物的分子量和粘度的量度。
该方法的原理基于通过毛细管粘度法测定相对溶液粘度。为此,通过摇动30分钟使测试物质溶解在甲苯中,以得到1%溶液。在Vogel-Ossag粘度计中在25℃下测量流动时间,并将其用于测定相对于纯溶剂的粘度的样品溶液的相对粘度。根据Fikentscher[P.E.Hinkamp,Polymer,1967,8,381],可从表格读取K值(K=1000k)。
本发明的压敏胶粘剂中的聚(甲基)丙烯酸酯优选地具有PD<4的多分散性,并因此具有相对窄的分子量分布。尽管具有相对低的分子量,但基于此的胶粘剂在交联后具有特别良好的剪切强度。此外,相对低的多分散性使从熔体加工更容易,因为与具有大体上相同的应用性质的更宽分布的聚(甲基)丙烯酸酯相比,流动粘度更低。具有窄分布的聚(甲基)丙烯酸酯可有利地通过阴离子聚合或通过受控自由基聚合方法制备,后者是特别合适的。也可经由N-氧基制备相应的聚(甲基)丙烯酸酯。此外,有利地可将原子转移自由基聚合(ATRP)用于合成窄分布的聚(甲基)丙烯酸酯,优选地使用单官能或双官能的仲或叔卤化物作为引发剂,且Cu、Ni、Fe、Pd、Pt、Ru、Os、Rh、Co、Ir、Ag或Au的络合物用于所述卤化物的提取(abstraction)。RAFT聚合也是合适的。
本发明的压敏胶粘剂中的聚(甲基)丙烯酸酯优选地通过其中存在的官能团与热交联剂的连接反应(特别地以加成或取代反应的形式)交联。可以使用如下的任何热交联剂:其
-既保证足够长的加工时间,使得在加工操作、特别是挤出操作期间没有凝胶化,
-又导致聚合物在低于加工温度的温度下、特别是在室温下快速后交联至所需的交联水平。
一种可能的实例是如下的组合:包含羧基、氨基和/或羟基的聚合物,以及作为交联剂的异氰酸酯、更特别地脂族异氰酸酯或封端异氰酸酯,实例是用胺失活的三聚异氰酸酯。特别地,合适的异氰酸酯为如下的三聚衍生物:MDI[4,4’-亚甲基二(苯基异氰酸酯)]、HDI[六亚甲基二异氰酸酯,1,6-亚己基二异氰酸酯]和IPDI[异佛尔酮二异氰酸酯,5-异氰酸基-1-异氰酸基甲基-1,3,3-三甲基环己烷],实例为产品N3600和XP2410(各自来自Bayer AG:脂族多异氰酸酯,低粘度HDI三聚体)。同样合适的是微粉化的三聚IPDI的表面失活的分散体BUEJ/>(现在为/>)(Bayer AG)。
优选以0.1至5重量%、特别地以0.2至1重量%使用热交联剂,基于待交联的聚合物的总量。
通过络合剂(也称为螯合物)的交联也是可能的。优选的络合剂的实例是乙酰丙酮铝。
本发明的压敏胶粘剂中的聚(甲基)丙烯酸酯优选地通过一种或多种环氧化物或通过一种或多种含有环氧基团的物质交联。含有环氧基团的物质更特别地是多官能环氧化物,即具有至少两个环氧基团的那些;因此,总体结果是带有官能团的聚(甲基)丙烯酸酯的单元的间接连接。含环氧基团的物质可为芳族或脂族化合物。
特别适合的多官能环氧化物为表氯醇的低聚物,多羟基醇(特别地乙二醇、丙二醇和丁二醇、聚二醇、硫二甘醇、甘油、季戊四醇、山梨糖醇、聚乙烯醇、聚烯丙醇等)的环氧醚;多羟基酚(特别地间苯二酚、对苯二酚、双(4-羟基苯基)甲烷、双(4-羟基-3-甲基苯基)甲烷、双(4-羟基-3,5-二溴苯基)甲烷、双(4-羟基-3,5-二氟苯基)甲烷、1,1-双(4-羟基苯基)乙烷、2,2-双(4-羟基苯基)丙烷、2,2-双(4-羟基-3-甲基苯基)丙烷、2,2-双(4-羟基-3-氯苯基)丙烷、2,2-双(4-羟基-3,5-二氯苯基)丙烷、2,2-双(4-羟基-3,5-二氯苯基)丙烷、双(4-羟基苯基)苯基甲烷、双(4-羟基苯基)二苯基甲烷、双(4-羟基苯基)-4'-甲基苯基甲烷、1,1-双(4-羟基苯基)-2,2,2-三氯乙烷、双(4-羟基苯基)-(4-氯苯基)甲烷、1,1-双(4-羟基苯基)环己烷、双(4-羟基苯基)环己基甲烷、4,4'-二羟基联苯、2,2'-二羟基联苯、4,4'-二羟基二苯基砜、及其羟基乙基醚)的环氧醚;苯酚-甲醛缩合产物如酚醇和酚醛树脂等;含S的环氧化物和含N的环氧化物,例如N,N-二缩水甘油基苯胺和N,N'-二甲基二缩水甘油基-4,4-二氨基二苯基甲烷;以及通过惯常方法由不饱和醇的单不饱和羧酸酯或多不饱和羧酸制备的环氧化物;缩水甘油酯,和聚缩水甘油酯,其可通过不饱和酸的缩水甘油酯的聚合或共聚或其它酸性化合物例如氰尿酸、二缩水甘油基硫醚、或环状三亚甲基三砜或其衍生物获得。
非常合适的醚的实例是1,4-丁二醇二缩水甘油醚、聚甘油-3缩水甘油醚、环己烷二甲醇二缩水甘油醚、甘油三缩水甘油醚、新戊二醇二缩水甘油醚、季戊四醇四缩水甘油醚、1,6-己二醇二缩水甘油醚、聚丙二醇二缩水甘油醚、三羟甲基丙烷三缩水甘油醚、季戊四醇四缩水甘油醚、双酚A二缩水甘油醚和双酚F二缩水甘油醚。
其他优选的环氧化物是脂环族环氧化物,例如3,4-环氧基环己基甲基3,4-环氧基环己烷羧酸酯(UVACure1500)。
更优选地,聚(甲基)丙烯酸酯借助于交联剂-促进剂体系(“交联体系”)交联,以获得对加工寿命、交联动力学和交联度的更好的控制。交联剂-促进剂体系优选地包括至少一种含环氧基团的物质作为交联剂、和至少一种如下的物质作为促进剂:其在低于待交联的聚合物的熔融温度的温度下对于借助于含环氧基团的化合物的交联反应具有促进作用。
根据本发明使用的促进剂更优选地为胺。这些在形式的意义上应被视为氨的取代产物;在下式中,取代基由“R”表示并且特别地包括烷基和/或芳基。特别优选的是,使用与待交联的聚合物仅发生低水平反应(如果有的话)的那些胺。
原则上,选择的促进剂可为伯胺(NRH2)、仲胺(NR2H)或叔胺(NR3),以及当然还有具有多个伯胺和/或仲胺和/或叔胺基团的那些。特别优选的促进剂是叔胺,例如三乙胺、三亚乙基二胺、苄基二甲基胺、二甲基氨基甲基苯酚、2,4,6-三(N,N-二甲基氨基甲基)苯酚和N,N'-双(3-(二甲基氨基)丙基)脲。另外的优选的促进剂是多官能胺如二胺、三胺和/或四胺,例如二亚乙基三胺、三亚乙基四胺和三甲基六亚甲基二胺。
另外的优选的促进剂的是氨基醇,特别地仲氨基醇和/或叔氨基醇,其中,在每分子多个胺官能团的情况下,优选地至少一个胺官能团且更优选地全部胺官能团为仲的和/或叔的。特别优选的该种类的促进剂是三乙醇胺、N,N-双(2-羟基丙基)乙醇胺、N-甲基二乙醇胺、N-乙基二乙醇胺、2-氨基环己醇、双(2-羟基环己基)甲基胺、2-(二异丙基氨基)乙醇、2-(二丁基氨基)乙醇、N-丁基二乙醇胺、N-丁基乙醇胺、2-[双(2-羟基乙基)氨基]-2-(羟甲基)-1,3-丙二醇、1-[双(2-羟基乙基)氨基]-2-丙醇、三异丙醇胺、2-(二甲基氨基)乙醇、2-(二乙基氨基)乙醇、2-(2-二甲基氨基乙氧基)乙醇、N,N,N'-三甲基-N'-羟基乙基双氨基乙基醚、N,N,N'-三甲基氨基乙基乙醇胺和N,N,N'-三甲基氨基丙基乙醇胺。
另外的合适的促进剂为吡啶、咪唑例如2-甲基咪唑、和1,8-二氮杂双环[5.4.0]十一-7-烯。也可使用脂环族多胺作为促进剂。还合适的是基于磷的促进剂如膦和/或化合物,例如三苯基膦或四苯基/>四苯基硼酸盐。
也可使用季铵化合物作为促进剂;实例是氢氧化四丁基铵、溴化十六烷基三甲基铵和苯扎氯铵。
在本发明的PSA中,丙烯腈-丁二烯橡胶优选以分散在聚(甲基)丙烯酸酯中的形式存在。因此,聚(甲基)丙烯酸酯和丙烯腈-丁二烯橡胶优选地各自为均相。优选地选择PSA中存在的聚(甲基)丙烯酸酯和丙烯腈-丁二烯橡胶,使得在23℃下它们不彼此混溶至均匀的程度。因此,至少在微观上和至少在室温下,本发明的PSA优选地具有至少两相形态。更优选地,聚(甲基)丙烯酸酯和丙烯腈-丁二烯橡胶在0℃至50℃、更特别地-30℃至80℃的温度范围内不彼此均匀混溶,并且因此在这些温度范围内,PSA至少在微观上呈至少两相形式。
对于本说明书而言,当如下的时候,组分被定义为“不彼此均匀混溶”:即使在紧密(中间)混合后,至少在微观上,至少两个稳定相的形成是物理和/或化学地可检测的,其中一个相富含一种组分并且第二相富含另一种组分时。在这方面,在没有多相特性的相反发展的情况下,一种组分在另一种组分中的可忽略不计的量的存在被认为是无关紧要的。因此,聚(甲基)丙烯酸酯相可包含少量的丙烯腈-丁二烯橡胶,和/或丙烯腈-丁二烯-橡胶相可包含少量的聚(甲基)丙烯酸酯组分,只要这些量不是影响相分离的实质(显著)量。
特别地,可实现相分离,使得富含丙烯腈-丁二烯橡胶(换句话说,基本上由丙烯腈-丁二烯-橡胶形成)的离散域(“畴”)存在于富含聚(甲基)丙烯酸酯(换句话说,基本上由聚(甲基)丙烯酸酯形成)的连续基体中。用于相分离的一种合适的分析系统是例如扫描电子显微镜法。替代地,相分离也可为例如通过如下可检测的:在动态扫描量热法(DSC)或动态力学分析(DMA)中具有彼此独立的两个玻璃化转变温度的不同相。当其可通过所述分析方法的至少一种清楚地显示时,根据本发明存在相分离。
本发明的PSA以1至49重量%、优选最高达10至45重量%、更优选20至40重量%包括至少一种丙烯腈-丁二烯橡胶。基于PSA的总重量。当存在两种或多种丙烯腈-丁二烯橡胶时,“PSA以…重量%包括至少一种丙烯腈-丁二烯胶”当然意味着“PSA以总计…重量%包括丙烯腈-丁二烯橡胶”。
丙烯腈-丁二烯橡胶(缩写代码NBR,源自“丁腈橡胶”)表示通过以约52:48至10:90的质量比例使丙烯腈和1,3-丁二烯共聚而获得的合成橡胶。NBR制造几乎专门地在水性乳液中进行。得到的乳液原样使用(NBR胶乳)或加工成固体橡胶。
在聚合背景中,原则上在所谓的冷聚合和热聚合进行区分。冷聚合惯常地在5至15℃的温度下进行,并且与通常在30至40℃下进行的热聚合相比,冷聚合导致较少数量的支链。
NBR橡胶可从许多制造商例如Nitriflex、Zeon、LG Chemicals和Lanxess商购获得。合适的NBR是可商购获得的,例如以商品名Nipol、特别是Nipol DN401L、Nipol N917和Nipol 1001CG,以及Zetpol、更特别地Zetpol 2001、Zetpol 2001EP、Zetpol 4310和Zetpol4310EP,来自Zeon。
羧基化的NBR等级是通过丙烯腈和丁二烯与少量(甲基)丙烯酸在乳液中的三元共聚而形成的。在NBR中C,C双键的选择性氢化导致氢化的丁腈橡胶(H-NBR)。硫化使用惯常的硫交联剂、过氧化物或通过高能辐射进行。合适的羧基化的NBR等级例如可以商品名KrynacX160和Krynac X750从Arlanceo商购购得。
在一种优选的实施方式中,所述至少一种丙烯腈-丁二烯橡胶是氢化或部分氢化的丙烯腈-丁二烯橡胶。
在另一优选的实施方式中,所述至少一种丙烯腈-丁二烯橡胶是羧基化的。
在另一实施方式中,所述至少一种丙烯腈-丁二烯橡胶是羧基化的且氢化或部分氢化的丙烯腈-丁二烯橡胶。
除羧基化或氢化的NBR橡胶外,还有液体NBR橡胶。在聚合过程中,通过添加聚合链转移剂,这些在分子量方面受限,且因此作为液体橡胶获得。
本发明的PSA不仅可包括一种或多种固体丙烯腈-丁二烯橡胶,还可包括至少一种液体丙烯腈-丁二烯橡胶。
液体丙烯腈-丁二烯橡胶的分数优选地为至多20重量%、更优选在1和15重量%之间、更优选在2和10重量%之间,基于丙烯腈-丁二烯橡胶的总重量。
相对于固体橡胶区分液体橡胶的因素是,它们具有<40℃的软化点。低聚和聚合化合物(例如树脂)的软化点TE的数字涉及根据DIN EN 1427:2007的环球法,其中适当应用测定(调查低聚物或聚合物样品,而不是沥青,其中程序在其它方面保持);测量在甘油浴中进行。
在一种优选的实施方式中,所述至少一种丙烯腈-丁二烯橡胶具有10至60重量%、优选15至50重量%的丙烯腈分数,基于丙烯腈-丁二烯共聚物橡胶的总重量。
在一种优选的实施方式中,根据DIN 53523-2:1991-05测量的,所述至少一种丙烯腈-丁二烯橡胶在100℃下具有至少19、优选20至100的门尼(Mooney)粘度。
本发明的PSA优选地包括至少一种增粘剂,其也可称为剥离粘附促进剂或增粘树脂,其特别地与聚(甲基)丙烯酸酯和/或丙烯腈-丁二烯橡胶相容。根据技术人员的一般理解,“增粘剂”是如下的低聚物或聚合物树脂:与不含增粘剂的在其它方面相同的PSA相比,其提高PSA的粘附性(剥离粘附性)。
“与聚(甲基)丙烯酸酯相容的增粘剂”是如下的增粘剂:与纯的聚(甲基)丙烯酸酯相比,其改变在彻底混合聚(甲基)丙烯酸酯和增粘剂后获得的体系的玻璃化转变温度,其中也仅一个Tg可分配给聚(甲基)丙烯酸酯和增粘剂的混合物。与聚(甲基)丙烯酸酯不相容的增粘剂将导致在彻底混合聚(甲基)丙烯酸酯和增粘剂后获得的体系中的两个Tg,其中一个Tg可分配给聚(甲基)丙烯酸酯,并且另一个可分配给树脂畴。本文中Tg的测定借助于DSC(差示扫描量热法)量热地进行。
与聚(甲基)丙烯酸酯相容的增粘剂优选地具有低于-30℃、更优选至多-70℃、最优选低于-50℃的DACP和/或优选地低于40℃、更优选至多30℃、更特别地24至28℃的MMAP。关于测定DACP和MMAP值,参考C.Donker,PSTC Annual Technical Seminar,Proceedings,第149-164页,2001年5月。
特别优选地,与聚(甲基)丙烯酸酯相容的增粘剂选自(甲基)丙烯酸酯树脂、松香衍生物和含芳族化合物的烃树脂,更优选富芳族化合物烃树脂;更特别地,选自(甲基)丙烯酸酯树脂和芳族烃树脂。特别优选地,与聚(甲基)丙烯酸酯相容的增粘剂是(甲基)丙烯酸酯树脂。这特别地使得可改善对极性粘合基材的粘附性。本发明的PSA还可包括两种或更多种增粘剂的混合物。在松香衍生物中,优选松香酯。
本发明的PSA优选地以总计5至25重量%、更优选以总计8至18重量%包括与聚(甲基)丙烯酸酯相容的增粘剂,在各自的情况下基于PSA的总重量。
本发明的压敏胶粘剂优选地包括
40-98重量%的至少一种聚(甲基)丙烯酸酯,
1-49重量%的至少一种丙烯腈-丁二烯橡胶,和
1-30重量%的至少一种增粘剂,
在各自的情况下基于PSA的总重量。更优选地,所述至少一种聚(甲基)丙烯酸酯和至少一种增粘剂的重量%的总和为至少55重量%、更特别地至少60重量%,在各自的情况下基于PSA的总重量。
更特别地,本发明的压敏胶粘剂包括
48-70重量%的至少一种聚(甲基)丙烯酸酯,
20-40重量%的至少一种丙烯腈-丁二烯橡胶,和
5-25重量%的至少一种增粘剂,
在各自的情况下基于PSA的总重量。
取决于本发明的PSA的使用领域和期望的性质,其可包括另外的组分和/或添加剂,在各自的情况下单独地或与一种或多种其他添加剂或组分组合。下面描述优选的实施方式。
本发明的PSA可进一步包括至少一种基于聚氨酯和/或硅酮的填料。通常,本领域已知的所有基于聚氨酯和硅酮的填料是合适的,但PSA优选地包括至少一种固体聚合物珠形式的基于聚氨酯和/或硅酮的填料,更特别地具有4至30μm直径的那些。
在PSA的制造过程中,这类固体聚合物珠可例如以在分散介质如EVA中的约50%母料的形式使用。
替代选地或另外地,本发明的PSA可包括,例如,不同于基于聚氨酯和/或硅酮的填料的粉末和粒料形式的填料,更特别地包括磨料和增强填料;染料;以及颜料,例如白垩(CaCO3)、二氧化钛、氧化锌和/或炭黑。
用于本发明PSA的合适添加剂另外地(独立于其他添加剂选择)为不可膨胀的中空聚合物珠或实心聚合物珠、中空玻璃珠、实心玻璃珠、中空陶瓷珠、实心陶瓷珠和/或实心碳珠(“碳微球”)。
根据一种优选的实施方式,本发明的PSA是发泡的。发泡优选地通过微球的引入和随后的膨胀来进行。在一种优选的实施方式中,本发明的PSA包括至少一种增粘剂和/或多个(种)微球。
“微球”是如下的中空微珠:其在它们的基态下是弹性的并因此可膨胀的,其具有热塑性聚合物壳。这些珠填充有低沸点液体或液化气体。所用的壳材料特别地包括聚丙烯腈、PVDC、PVC或聚丙烯酸酯。合适的低沸点液体特别地为如下的烃:低级烷烃例如异丁烷或异戊烷,其在压力下作为液化气体被包封在聚合物壳内。
通过微球的暴露、更特别地通过热暴露,导致聚合物外壳软化。同时,壳内存在的液态发泡气体经历转变为其气态。在该过程中,微球不可逆地且三维地膨胀。当内部压力与外部压力匹配时,膨胀结束。由于聚合物壳被保留,结果为闭孔泡沫体。
许多类型的微球是可商购获得的,主要在其尺寸(在未膨胀状态下6-45μm直径)和其膨胀所需的起始温度(75℃至220℃)方面不同。可商购获得的微球的一个实例是来自Akzo Nobel的DU等级(DU=干燥未膨胀的)。
未膨胀的微球等级还为以具有约40-45重量%的固含量或微球含量的水性分散体的形式、以及聚合物结合的微球(母料)(例如以约65重量%的微球浓度在乙烯-乙酸乙烯酯中)的形式可获得的。与DU等级一样,不仅微球分散体而且母料适合用于制造本发明的发泡的PSA。
本发明的发泡的PSA也可使用所谓的预膨胀的微球产生。在该组别的情况下,膨胀甚至在引入聚合物基体之前发生。预膨胀的微球是可商购获得的,例如,以牌号或以类型牌号“Expancel xxx DE”(DE=干燥膨胀的)得自Akzo Nobel。
优选地,在本发明中,由微球形成的所有空腔的至少90%具有10至200μm、更优选15至200μm的最大直径。“最大直径”是指在空间中在任何方向上的微球的最大尺度。
直径是基于500倍放大的扫描电子显微镜(SEM)中的低温断裂边缘测定的。各单独的微球的直径图解地确定。
在使用微球进行发泡的情况下,微球可以母料(批次,batch)、糊剂或者未延展的或延展的(未膨胀的或膨胀的)粉末的形式提供至配制物(组成物)。它们也可以悬浮在溶剂中的形式存在。
根据本发明的一种优选的实施方式的胶粘剂中的微球的分数为在大于0重量%和10重量%之间、更特别地在0.25重量%和5重量%之间、更特别地在0.5重量%和1.5重量%之间,在各自的情况下基于胶粘剂的总组成。
本发明的发泡的PSA的绝对密度优选地为350至1200kg/m3、更优选地600至1000kg/m3、更特别地750至950kg/m3。相对密度描述本发明的发泡的PSA的密度与具有相同配方的本发明的未发泡的PSA的密度之比。本发明的PSA的相对密度为优选地0.35至0.99、更优选地0.45至0.97、更特别地0.50至0.90。
本发明的PSA可进一步包括:低可燃性填料,例如多磷酸铵;导电填料,例如导电炭黑、碳纤维和/或覆银珠;导热材料,例如氮化硼、氧化铝、碳化硅;铁磁性添加剂,例如铁(III)氧化物;有机可再生原料,例如木粉;有机和/或无机纳米颗粒;纤维、配混剂、老化抑制剂、光稳定剂和/或抗臭氧剂。
本发明的PSA任选地包括一种或多种增塑剂。可添加的增塑剂的实例包括(甲基)丙烯酸酯低聚物、邻苯二甲酸盐(酯)、烃油、环己烷二羧酸酯、水溶性增塑剂、增塑树脂、磷酸盐(酯)或多磷酸盐(酯)。
本发明的PSA优选地包括二氧化硅、更优选地沉淀二氧化硅、更特别地用二甲基二氯硅烷表面改性的沉淀二氧化硅。使用该添加剂,可有利地建立PSA的热剪切强度。
幅材形式的本发明的PSA的厚度为优选地50至1500μm、更优选地70至1200μm、更特别地100至800μm、例如150μm至500μm或200μm至400μm。
本发明的PSA可采取压敏胶粘剂膜的形式。这可通过本领域技术人员已知的惯常涂覆方法来实现。在这种情况下,PSA(包括添加剂)以在合适的溶剂中的溶液的形式可通过例如网版(半调)辊施加(halftone roll application)、逗号棒涂布、多辊涂布或在印刷过程中涂布到载体膜或剥离膜上,之后可在干燥通道或干燥箱中除去溶剂。替代地,载体膜或剥离膜也可在无溶剂工艺中涂覆。为此,将丙烯腈-丁二烯橡胶和聚(甲基)丙烯酸酯在挤出机中加热并熔化。可在挤出机中进行另外的的操作步骤,例如与所描述的添加剂混合、过滤或脱气。然后通过压延机将熔体涂覆到载体膜或剥离膜上。
本发明的另外的主题是本发明的PSA用于粘合电子设备的部件、特别地显示器、或汽车中或汽车上的部件、更特别地用于粘合汽车中的电子部件以及用于粘合汽车的清漆饰面上的装饰条或标志的用途。特别地,在电子设备的高价值个体部件(例如显示器)的粘合的情况下,例如,以上已经概述的重新定位部件的可能性是特别有利的。使用本发明PSA的粘合可手动地或以自动方式进行。
最后,本发明的另外的主题是包括至少一个根据本发明的压敏胶粘剂的层的胶带。
实施例
NBR的表征
一般实验说明:压敏胶粘剂的制造
聚丙烯酸酯1的制造:
向常规用于自由基聚合的反应器充入72.0kg丙烯酸2-乙基己酯、20.0kg丙烯酸甲酯、8.0kg丙烯酸和66.6kg丙酮/异丙醇(94:6)。在氮气通过反应器45分钟后,在搅拌下,将反应器加热至58℃,并加入溶解在500g丙酮中的50g AIBN。然后将外部加热浴加热至75℃,并在该外部温度下持续进行反应。1小时后,加入另外的溶解在500g丙酮中的50g AIBN,并且4小时后,用10kg丙酮/异丙醇混合物(94:6)稀释反应混合物。
在5小时后并且再次在7小时后,用在各自的情况下溶解在500g丙酮中的在各自的情况下150g过氧二碳酸双(4-叔丁基环己基)酯再引发反应。在22小时的反应时间后,终止聚合反应,并将体系冷却至室温。产物具有55.8%的固含量,并被干燥。
聚丙烯酸酯2的制造:
向常规用于自由基聚合的300l反应器充入47kg丙烯酸正丁酯、20kg丙烯酸甲酯、30kg丙烯酸2-苯氧基乙酯、3kg丙烯酸和72.4kg挥发油/丙酮(70:30)。在氮气通过反应器45分钟后,在搅拌下,将反应器加热至58℃,并加入50g67(2,2'-偶氮双(2-甲基丁腈))。然后将夹套温度加热至75℃,并在该外部温度下持续进行反应。1小时的反应时间后,加入10g/>67。在3小时后,用20kg挥发油/丙酮(70:30)进行稀释,并在6小时后用10kg挥发油/丙酮(70:30)进行稀释。为了减少残留的引发剂,在5.5小时和7小时各自后加入0.15kg/>16(过氧二碳酸二(4-叔丁基环己基)酯)。在24小时的反应时间后,终断反应,并将体系冷却至室温。将溶液调节至38重量%的固含量。/>
制造方法,对比例1:
在具有双西格玛捏合钩的捏合设备中,将压敏胶粘剂作为基于溶剂的配混物均质化。使用的溶剂是丁酮(甲乙酮,2-丁酮)。通过水冷来冷却捏合设备。在第一步骤中,首先在23℃下用相同量的丁酮对固体丙烯腈-丁二烯橡胶进行预溶胀12小时。如所知的,该预配料然后被捏合2小时。随后,再次,在两步中加入上述选择量的丁酮和任选地液体NBR橡胶,在各自的情况下捏合10分钟。随后将增粘树脂作为固含量50%的在丁酮中的溶液加入,然后再均匀捏合20分钟。通过添加丁酮将最终的固含量调节至30重量%。
制造方法,对比例2:
将小球形式的SIS3421通过固体计量系统在行星辊式挤出机中熔化。随后添加在单螺杆挤出机中预熔化和浓缩的聚丙烯酸酯,丙烯酸酯树脂/>DM55,微球(/>920DU40)。还向混合物加入交联剂(/>1500)。将熔体混合并通过双辊压延机在两个剥离膜(硅化的PET膜)之间成形为厚度200μm的层。
一般的制造方法,符合本发明的实施例:
将小球形式的丙烯腈橡胶DN401L通过固体计量系统在行星辊式挤出机中熔化。随后添加在单螺杆挤出机中预熔化和浓缩的聚丙烯酸酯,丙烯酸酯树脂/>DM55,和/或芳族树脂/>AR100,微球(/>920DU40)。还向混合物加入交联剂(1500)。将熔体混合并通过双辊压延机在两个剥离膜(硅化的PET膜)之间成形为厚度200μm的层。
得到的胶粘剂的层的组成如下:
测试方法
测试1:活化=对塑料的瞬时剥离粘附性
在23℃+/-1℃温度和50%+/-5%相对湿度的测试条件下进行对塑料的剥离粘附性的测定,所用的塑料基材为表面粗糙度1μm的30%玻璃纤维增强的PBT的板。
为了在测量之前进行清洁和调节,首先用乙醇擦拭测试板,然后在空气中静置5分钟以使溶剂蒸发。然后,在单层胶带的背向测试基材的一侧用36μm经蚀刻的PET膜加衬,以防止在测量过程中的试样拉伸。然后将测试试样辊压到塑料基材上。为此,使用2kg橡胶辊以10m/分钟的滚动速度来回辊压胶带两次。将辊压胶带后,立即以180°的角度将胶带从塑料基材剥离,并用Zwick拉伸试验机测量实现这一点所需的力。测量结果以N/cm报告,并从三次单独测量取平均值。
落塔测试方法(抗穿透力)
从所调查的胶带上切下框架形状的方形样品(面积180mm2;边框宽度2.0mm)。
对照测量:
将样品粘附在已经用丙酮清洁的钢框架上。在胶带的另一侧上,粘附用丙酮清洁的钢窗。以如下方式进行钢框架、胶带框架和钢窗的粘合:使得几何中心和对角线各自相互重叠(角对角)。使粘合件经历62N的压力10s,并在23℃/50%相对湿度调节的情况下储存72小时。随后将样品在65℃下再储存72小时。从储存取出样品后,将测试试样在23℃/50%r.H下调节2小时。
在油酸中浸渍后的测量:
按照对照测量准备样品。在23℃/50%r.H.下调节72小时后,安置样品使得它躺在钢窗上。由于已经粘合的钢框架,此刻存在空腔,向其中引入0.7ml油酸。然后将样品储存在密封容器中在65℃ 72小时。在72小时后,通过用棉花吸取油酸来清洁样品并在23℃/50%r.H.下再次调节样品2小时。
为了进行测量,将测试试样插入仪表化跌落设备的样品架中,使得组件为水平的,其中钢窗朝下。测量通过仪器自动进行,使用5kg的装载重量和20cm的跌落高度。由装载重量引入的动能通过在窗口和框架之间的胶带的断裂来破坏胶粘粘合,并且通过压电传感器每μs记录力。相应地,相关软件给出测量后的力/时间进程的图,并由此可测定最大力F最大。在矩形冲击几何体冲击窗之前不久,使用两个光束测定下落重物的速度。假设所引入的能量相对于胶粘粘合的抗冲击性是大的,则使用力进程、分离所用的时间和下落重物的速度来确定在完全分离之前由粘合执行的功,即分离功。研究各样品的五个测试试样;最终的抗冲击性结果由这五个样品的分离功(以J计的能量)或最大力(以N计的F最大)的平均值组成。
在70℃的静态剪切测试
将尺寸13x 20mm的胶粘剂转移带在没有气泡的情况下粘合到已经用丙酮清洁的钢板。胶带的背面用铝箔加衬。使用2kg钢辊以10m/分钟的速度将粘合件总共辊压4次。将测试试样悬挂在与加热柜组合的剪切试验测量站上。以5N进行加载。当粘合失效或规定的测试时间到期时,认为测试结束。结果以分钟报告,并且是3次单独测量的中值。
表1:发明实施例和对比例的性质
根据本发明的实施例不仅表现出对化学品(油酸作为实例)的良好耐受性,而且表现出高剪切强度。
对比例1,纯NBR带,表现出不足的剪切强度。
对比例2,Ac聚合物和SIS的共混物,表现出不足的耐化学性。
Claims (11)
1.压敏胶粘剂,包括
-至少一种聚(甲基)丙烯酸酯;和
-至少一种丙烯腈-丁二烯橡胶,其中
所述至少一种丙烯腈-丁二烯橡胶以1至49重量%存在,基于压敏胶粘剂的总重量。
2.如权利要求1所述的压敏胶粘剂,其中所述至少一种丙烯腈-丁二烯橡胶具有10至60重量%的丙烯腈分数,基于丙烯腈-丁二烯橡胶的总重量。
3.如权利要求1或2所述的压敏胶粘剂,其中所述至少一种丙烯腈-丁二烯橡胶是氢化或部分氢化的丙烯腈-丁二烯橡胶。
4.如前述权利要求中任一项所述的压敏胶粘剂,其中根据DIN ISO289-1:2018-12测量的,所述至少一种丙烯腈-丁二烯橡胶在100℃下具有至少19、优选20至100的门尼粘度。
5.如前述权利要求中任一项所述的压敏胶粘剂,其中所述压敏胶粘剂是幅材形式的压敏胶粘剂。
6.如前述权利要求中任一项所述的压敏胶粘剂,其中所述压敏粘合剂包含≥40重量%的聚(甲基)丙烯酸酯,基于压敏粘合剂的总重量。
7.如前述权利要求中任一项所述的压敏胶粘剂,其中所述压敏胶粘剂是发泡的压敏胶粘剂。
8.如前述权利要求中任一项所述的压敏胶粘剂,其中所述压敏胶粘剂包括至少一种增粘剂和/或多个微球。
9.用于制造如权利要求1至8中任一项所述的压敏胶粘剂的方法,其中所述制造包括通过配混和挤出设备,并且所述方法是连续工艺。
10.如权利要求1至8中任一项所述的压敏胶粘剂用于粘合电子设备的部件或汽车中的部件的用途。
11.胶带,包括至少一个如权利要求1至8中任一项所述的压敏胶粘剂的层。
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