CN110520498B - 具有耐化学品性的聚氨酯粘合剂 - Google Patents
具有耐化学品性的聚氨酯粘合剂 Download PDFInfo
- Publication number
- CN110520498B CN110520498B CN201880014208.5A CN201880014208A CN110520498B CN 110520498 B CN110520498 B CN 110520498B CN 201880014208 A CN201880014208 A CN 201880014208A CN 110520498 B CN110520498 B CN 110520498B
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- Prior art keywords
- pressure sensitive
- sensitive adhesive
- adhesive composition
- polyurethane
- polyol
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Abstract
本发明提供了一种压敏粘合剂组合物,该压敏粘合剂组合物包含聚氨酯聚合物,该聚氨酯聚合物包含多异氰酸酯组分与多元醇组分的反应产物。多元醇组分具有小于10的亲水亲脂平衡(HLB)。聚氨酯还包含0.5重量%至10重量%具有大于12的HLB的亲水性聚合单元,诸如聚乙二醇聚合物的反应产物。在另一个实施方案中,聚氨酯还包含侧链烯键式不饱和基团。还描述了诸如层合胶带和保护膜的制品以及用压敏粘合剂和层合胶带粘结基底的9方法。
Description
发明内容
描述了一种压敏粘合剂组合物,其包含聚氨酯聚合物,该聚氨酯聚合物包含多异氰酸酯组分与多元醇组分的反应产物。该多元醇组分具有小于10的亲水亲脂平衡(“HLB”)。
在一个实施方案中,聚氨酯还包含0.5重量%至10重量%的具有大于12的HLB的亲水性聚合单元,诸如聚乙二醇聚合物的反应产物。
在另一个实施方案中,聚氨酯包含侧链烯键式不饱和基团。
在又一个实施方案中,聚氨酯包含亲水性聚合单元和侧链烯键式不饱和基团两者。
还描述了诸如层合胶带和保护膜的制品以及用压敏粘合剂和层合胶带粘结基底的方法。
具体实施方式
聚氨酯组合物包含多异氰酸酯组分与多元醇组分的反应产物。
多元醇组分包括包含至少两个羟基末端基团的芳族和/或脂族聚酯或聚己内酯多元醇。当(例如,聚酯)多元醇平均具有2个羟基基团时,其可表征为(例如,聚酯)二醇。在其他实施方案中,(例如,聚酯)多元醇可表征为(例如,聚酯)三醇。在其他实施方案中,(例如,聚酯)多元醇可包含二醇和三醇的混合物,其中羟基基团的数目平均大于2,但小于3。其它多元醇具有4个、5个或6个羟基末端基团。聚酯多元醇可通过例如多元醇组分与酸组分之间的酯化反应而获得。酸组分的示例包括琥珀酸、甲基琥珀酸、己二酸、庚二酸、壬二酸、癸二酸、1,12-十二烷二酸、1,14-十四烷二酸、二聚酸、2-甲基-1,4-环己烷二羧酸、2-乙基-1,4-环己烷二羧酸、对苯二甲酸、间苯二甲酸、邻苯二甲酸、1,4-萘二羧酸、4,4'-联苯二羧酸以及它们的酸酐。
如本领域已知的,芳族聚酯多元醇可通过使芳族二羧酸与脂族二醇聚合来制备。在一个实施方案中,芳族二羧酸通常包含主要量的间苯二甲酸或邻苯二甲酸。聚酯多元醇可任选地由少量的其它芳族二羧酸诸如对苯二甲酸来制备。此外,聚酯多元醇可任选地由少量的脂环族二羧酸诸如1,3-环戊烷二羧酸、1,2-环己烷二羧酸、1,4-环己烷二羧酸、2,5-降冰片烷二羧酸等制备。这些二羧酸通常是酸酐的形式。
用于制备芳族或脂族(例如聚酯或聚碳酸酯)多元醇的脂族二醇通常包含直链或支链亚烷基基团诸如乙二醇、二甘醇、丙二醇、1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、1,7-庚二醇、1,8-辛二醇、1,9-壬二醇、1,10-癸二醇、2,4-二甲基-2-乙基己烷-1,3-二醇、2,2-二甲基-1,3-丙二醇(新戊二醇)、2-乙基-2-丁基-1,3-丙二醇、2-乙基-2-异丁基-1,3-丙二醇、3-甲基-1,5-戊二醇、2,2,4-三甲基-1,6-己二醇、十八烷二醇等。在典型的实施方案中,用于产生芳族或脂族聚酯多元醇的脂族二醇中的至少一种包含含有至少4个、5个或6个碳原子且通常不大于24个或不大于36个的直链或支链亚烷基基团(例如下式中的R1)。在一些实施方案中,直链或支链亚烷基基团包含不大于12个或8个碳原子。在一些实施方案中,直链亚烷基基团是优选的。
在一些实施方案中,多元醇是聚己内酯多元醇,其可通过使环状酯单体例如ε-己内酯或σ-戊内酯经受开环聚合而获得。聚己内酯多元醇包含具有5个碳原子的亚烷基基团。
在其他实施方案中,多元醇组分还可包含聚碳酸酯多元醇,其可从脂族二醇如丁二醇-(1,4)和/或己二醇-(1,6)与光气、碳酸二芳基酯诸如碳酸二苯酯或与环状碳酸酯诸如碳酸亚乙酯或丙二醇碳酸酯的反应中获得。由上述聚酯或聚内酯与光气、碳酸二芳基酯或环状碳酸酯获得的聚酯碳酸酯也是合适的。聚酯或聚碳酸酯多元醇的制备通常包括如前所述使用至少一种脂族二醇。脂族二醇和(例如芳族)聚酯或聚碳酸酯多元醇的亚烷基基团可包含疏水取代基如卤素取代基。一种说明性的聚碳酸酯多元醇以商品名“DesmophenC2200”得自拜耳材料科学公司(Bayer Materials Science LLC)。
在典型的实施方案中,单一脂族二醇用于(例如,聚酯)多元醇的制备。在该实施方案中,脂族二醇包含如前所述的包含至少4个、5个或6个碳原子的亚烷基基团。另选地,在(例如,聚酯)多元醇的制备中可使用两种或更多种脂族二醇,其中此类二醇中的至少一种包含如前所述的包含至少4个、5个或6个碳原子的亚烷基基团。当使用脂族二醇的混合物时,二醇的总量(或总R1亚烷基基团)的至少50重量%、60重量%、70重量%、80重量%、90重量%或95重量%是如前所述的包含至少4个、5个或6个碳原子的亚烷基基团。
多元醇通常是聚合物。(例如,聚酯)多元醇通常具有范围为约250至约30000的当量重量(每个羟基基团所对应的分子量)。在一些实施方案中,(例如,聚酯)多元醇的当量重量不大于20000、10000、8000、7000、6000、5000、4000、3500、3000、2500或2000;或在500和30000之间、在2000和20000之间、在2000和10000之间或在2000和4000之间。就二醇而言,(例如,聚酯)多元醇的分子量为刚才描述的当量重量的两倍。就三醇而言,(例如,聚酯)多元醇的分子量为刚刚描述的当量重量的三倍。在一些实施方案中,聚合多元醇的分子量小于4000克/摩尔、3500克/摩尔、或3000克/摩尔。
在一个实施方案中,脂族聚酯多元醇可包含含有(R1)亚烷基基团的重复单元和末端酯基或通过酯键键合的多于一个(R1)亚烷基基团和末端酯基基团。
在另一个实施方案中,脂族聚碳酸酯多元醇可包含含有(R1)亚烷基基团的重复单元和末端碳酸酯基团或通过碳酸酯键键合的多于一个(R1)亚烷基基团和末端碳酸酯基团。
在另一个实施方案中,芳族聚酯多元醇可包含重复单元,该重复单元包含通过酯键键合至(脂族二醇)的(R1)亚烷基基团的(二羧酸的)芳族(例如,邻苯二甲酸酯)基团。在该实施方案中,六元环与具有至少4个、5个或6个碳原子的亚烷基基团的比率为约1:1并且可在约1.5:1至1:1.5的范围内。
多元醇通常具有某些溶解度参数,这些参数使用在《涂层织物》1989年第19卷第53期的K.L.Hoy编写的(K.L.Hoy,J.Coated Fabrics,Volume 19,53(1989))论文中描述的基团贡献法进行计算。利用获自诺格因蒙哥马利化学软件有限公司(Norgwyn MontgomerySoftware,Inc.)(宾夕法尼亚州北威尔士(North Wales,Pa.))的程序Molecular ModelingPro Plus进行计算。
多元醇通常具有至少9.0、9.5、并且在一些实施方案中至少10(cal/cm3)1/2的总溶解度参数。多元醇的总溶解度参数通常不大于14(cal/cm3)1/2。在一些实施方案中,总溶解度参数不大于13、12.5、12、11.5或11(cal/cm3)1/2。
多元醇的氢键合溶解度参数通常为至少2.0(cal/cm3)1/2且在一些实施方案中为至少2.5(cal/cm3)1/2、3.0(cal/cm3)1/2或3.5(cal/cm3)1/2且通常不大于6(cal/cm3)1/2。在一些实施方案中,多元醇的氢键合溶解度参数不大于5.5(cal/cm3)1/2或5.0(cal/cm3)1/2。在一些实施方案中,分散溶解度参数可在约7(cal/cm3)1/2至9(cal/cm3)1/2的范围内。在一些实施方案中,分散溶解度参数可以为至少8。此外,极性溶解度参数可在约2(cal/cm3)1/2至6(cal/cm3)1/2的范围内。在一些实施方案中,极性溶解度参数可以为至少3。
下表描述了具有刚才描述的溶解度参数的例示性多元醇。
表A
在一些实施方案中,刚才描述的聚酯多元醇比聚丙二醇更疏水。表征疏水性的一种方法是亲水亲脂平衡(“HLB”)。虽然已描述多种用于测定如本文中所用的化合物的HLB的方法,但除非另有说明,否则HLB指通过格里芬方法(Griffin’s method)获得的值。(参见《化妆品化学会志》1954年第5期第259页Griffin WC所著论文(Griffin WC:“Calculationof HLB Values of Non-Ionic Surfactants,”Journalof the Society of CosmeticChemists 5(1954):259))。利用获自宾夕法尼亚州北威尔士的诺格因蒙哥马利化学软件有限公司(Norgwyn Montgomery Software,Inc.(North Wales,Pa.))的软件程序MolecularModeling Pro Plus进行计算。
根据格里芬方法:HLB=20*Mh/M,其中Mh为分子的亲水性部分的分子质量,并且M为整个分子的分子质量。亲水性部分及其分子质量可通过各种技术诸如核磁共振来确定。这种计算提供在0到20标度内的数值结果,其中“0”为高度亲脂性的。因此,数值结果10被认为是亲水性和亲脂性相等。
就聚合物材料如聚合多元醇而言,格里芬方法通常用于计算单一分子或重复单元的HLB。当聚合物表面活性剂包含重复单元的混合物时,可以用各个重复单元的HLB与每个分子的重量分数乘积的总和来计算HLB。
例如,具有30个重复单元的聚丙二醇可具有10的HLB,而芳族聚酯多元醇“PH-56”具有小于10,即9的HLB。
脂族聚酯多元醇也可具有小于聚丙二醇的HLB。例如,脂族聚酯多元醇“Priplast1900”具有8的HLB。在其他实施方案中,脂族聚酯多元醇可具有小于7、6或5的HLB。例如,脂族聚酯多元醇“Priplast 1838”具有4的HLB。在一些实施方案中,脂族聚酯多元醇的HLB大于氢化聚丁二烯、蓖麻油或“Priplast 3196”。因此,HLB大于2或3。
当多元醇组分含有多元醇的混合物时,HLB可通过将每种多元醇的HLB与其重量分数乘积的总和来确定。例如,当多元醇组分包含1:1重量比的“Priplast 1900”和“Priplast1838”时,多元醇组分的HLB为4。
在一些有利的实施方案中,使用芳族聚酯多元醇,其可通过使芳族邻二羧酸或间二羧酸(酸酐)组分与脂族二醇组分反应而获得。因此,多元醇组分包含邻苯二甲酸酯或间苯二甲酸酯的聚合单元,并包含含有至少4个碳原子的亚烷基基团的聚合单元。
在一个实施方案中,聚酯多元醇(由间苯二甲酸或邻苯二甲酸制备的)具有以下结构:
其中R1独立地为包含至少4个碳原子的亚烷基基团,
n为至少2、3、4或5,并且
酯基取代基在邻位或间位键合到环。
在一些实施方案中,n不大于25、20、15或10。
当芳族聚酯多元醇包含邻酯部分或间酯部分时,聚酯多元醇往往具有低的玻璃化转变温度,例如低于0℃、5℃或10℃。此外,此类芳族聚酯多元醇往往在25℃为(无定形)粘滞液体。在一些实施方案中,芳族聚酯多元醇具有在80℃小于10,000cP或5,000cP的粘度。
衍生自邻苯二甲酸的芳族聚酯多元醇可以以商品名StepanpolTM商购自斯泰潘公司(Stepan)并具有以下结构:
当芳族聚酯多元醇衍生自异对苯二甲酸时,聚酯多元醇可具有以下结构:
在其他实施方案中,多元醇可以是(例如,C36)二聚体基聚酯多元醇。此类多元醇还可包含低浓度的芳族基团,通常为多元醇的小于1质量%。
在一些有利的实施方案中,上述芳族或脂族聚酯二醇是聚氨酯的主要或唯一羟基官能反应物和唯一多元醇。在其他实施方案中,具有前述溶解度参数的其他聚酯和/或聚己内酯二醇是聚氨酯的主要或唯一羟基官能反应物和唯一多元醇。
具有前述溶解度参数的多元醇(例如,二醇)是聚氨酯的主要多元醇,此类多元醇以多元醇组分的总量的至少50重量%、55重量%、60重量%、65重量%、70重量%、75重量%、80重量%、85重量%、90重量%、95重量%或99重量%的量存在。在一些实施方案中,芳族聚酯二醇是聚氨酯的主要多元醇并且以多元醇组分的总量的至少50重量%、55重量%、60重量%、65重量%、70重量%、75重量%、80重量%、85重量%、90重量%、95重量%或99重量%的量存在。在其他实施方案中,脂族聚酯二醇是聚氨酯的主要多元醇并且以多元醇组分的总量的至少50重量%、55重量%、60重量%、65重量%、70重量%、75重量%、80重量%、85重量%、90重量%、95重量%或99重量%的量存在。
在一些实施方案中,(即在与多异氰酸酯组分反应之前)的羟基值为至少5mgKOH/g、10mgKOH/g、25mgKOH/g、30mgKOH/g或40mg KOH/g,并且在一些实施方式不大于200mgKOH/g、150mgKOH/g、100mgKOH/g、90mgKOH/g、80mgKOH/g或70mg KOH/g。在一些实施方案中,其他多元醇的聚酯多元醇的水含量不大于多元醇的0.10重量%或0.05重量%。在一些实施方案中,聚酯多元醇或其他多元醇的加德纳色度不大于3、2或1。在一些实施方案中,聚酯多元醇或其他多元醇的酸值不大于5mgKOH/g、4mgKOH/g、3mgKOH/g、2mgKOH/g或1mg KOH/g,或者换句话说,为多元醇的不大于0.005重量%、0.004重量%、0.003重量%、0.002重量%或0.001重量%。同样,在一些实施方案中,如刚才所述,聚氨酯聚合物也包含低浓度的酸。
多元醇组分还可包含0.5重量%、1重量%、5重量%、10重量%、15重量%、20重量%、25重量%、30重量%、35重量%、40重量%、45重量%或50重量%的另一种多元醇或其他多元醇,尤其是亲水性多元醇和/或具有酸基团的多元醇。还可任选地使用充当增链剂和化学交联剂的多元醇。
在一些实施方案中,聚氨酯包含亲水性聚合单元。此类亲水性聚合单元的可表征为具有至少12、13、14、15、16、17、18、19或20的HLB。少量此类亲水性基团可改善环境老化结果,即粘合剂在65℃和90%相对湿度下老化800小时后表现出小于2%、1.5%或1%的雾度。在一些实施方案中,聚氨酯包含至少0.5重量%、1.0重量%或1.5重量%的聚合亲水性单元。聚合亲水性单元的量通常小于聚氨酯的总聚合单元的10重量%、9重量%、8重量%、7重量%、6重量%或5重量%。在一些实施方案中,聚氨酯包含不大于4重量%、3.5重量%或3重量%的聚合亲水性单元。
在一些实施方案中,聚合亲水性单元衍生自聚乙二醇聚合物。聚乙二醇聚合物可为聚乙二醇均聚物或乙二醇与共聚单体(例如,环氧丙烷)的共聚物。共聚物通常包含至少50重量%、60重量%、70重量%、80重量%或90重量%的乙二醇聚合单元。
一种合适的聚乙二醇聚合物可以以商品名YmerTMN-120从柏斯托公司(Perstorp)商购获得。此类聚合物的结构如下:
此类材料通常用作水性聚氨酯分散体的非离子分散剂。然而,目前所述的聚氨酯主要为疏水性的,并且因此不包含足够浓度的亲水性基团以使得该聚氨酯为水溶性的或水分散性的,如IPA/水耐化学品性所证实的。当聚乙二醇聚合物具有包含两个羟基的末端基团时,可将该聚合物并入聚合物主链中,使得所得的聚氨酯包含侧链聚乙二醇聚合物单元。相比之下,在两端均具有末端基团的聚乙二醇聚合物导致聚乙二醇聚合物单元存在于聚合物主链中而非侧链中。
其他可商购获得的环氧乙烷/环氧丙烷嵌段共聚物以商品名“Pluronic”得自巴斯夫公司(BASF)。
在一些实施方案中,(例如,侧链)聚合亲水性单元或聚乙二醇聚合物具有至少200g/mol、300g/mol、400g/mol或500g/mol的分子量。在一些实施方案中,聚合亲水性单元或聚乙二醇聚合物具有不大于2000g/mol或1500g/mol的分子量。
在一些实施方案中,在制备聚氨酯期间使用包含一个或多个羟基基团和一个或多个烯键式不饱和基团的化合物。该羟基基团与多异氰酸酯反应,将烯键式不饱和基团并入到聚氨酯中。在一些实施方案中,可使用具有单个羟基基团和单个烯键式不饱和基团的化合物,诸如丙烯酸羟乙酯(HEA)。在该实施方案中,异氰酸酯基团键合到聚氨酯聚合物主链,并且二异氰酸酯的相对端与该化合物的羟基基团键合,得到末端烯键式不饱和基团。在其他实施方案中,该化合物具有至少两个羟基基团和至少两个烯键式不饱和基团,诸如双酚A甘油二甲基丙烯酸酯(BAGDM)。在该实施方案中,该化合物可用作多元醇(即,二醇)且因此结合到聚氨酯主链中。烯键式不饱和基团相对于聚氨酯主链是侧链的。
在制备聚氨酯期间可使用包含一个或多个羟基基团和一个或多个烯键式不饱和基团的各种化合物。此类化合物可以是脂族的或芳族的。可得自日本大阪的长濑化学产业株式会社(Nagase ChemteX Corporation,Osaka,Japan)的其他代表性化合物包括,例如,可作为DA-212获得的环氧丙烯酸酯形式的1,6-己二醇;可作为DA-214L获得的环氧丙烯酸酯形式的1,4-己二醇。
多异氰酸酯组分可包含各种多官能异氰酸酯化合物。此类多官能异氰酸酯化合物的示例包括多官能脂族异氰酸酯化合物、多官能脂族环状异氰酸酯化合物和多官能芳族异氰酸酯化合物。
多官能脂族异氰酸酯化合物的示例包括三亚甲基二异氰酸酯、四亚甲基二异氰酸酯、六亚甲基二异氰酸酯、五亚甲基二异氰酸酯、1,2-亚丙基二异氰酸酯、1,3-亚丁基二异氰酸酯、十二亚甲基二异氰酸酯和2,4,4-三甲基六亚甲基二异氰酸酯。
多官能脂族环状异氰酸酯化合物的示例包括1,3-环戊烯二异氰酸酯、1,3-环己烷二异氰酸酯、1,4-环己烷二异氰酸酯、异佛乐酮二异氰酸酯、氢化二苯基甲烷二异氰酸酯、氢化苯二甲基二异氰酸酯、氢化甲苯二异氰酸酯、氢化四甲基二甲苯二异氰酸酯和生物基多官能脂族环状异氰酸酯诸如以商品名1410得自巴斯夫公司(BASF Corporation)的2-庚基-3,4-双(9-异氰酸根合壬基)-1-戊基环己烷。
多官能芳族异氰酸酯化合物的示例包括苯二异氰酸酯、2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、2,2'-二苯基甲烷二异氰酸酯、4,4'-二苯基甲烷二异氰酸酯、4,4'-甲苯胺二异氰酸酯、4,4'-二苯醚二异氰酸酯、4,4'-二苯基二异氰酸酯、1,5-萘二异氰酸酯和苯二甲基二异氰酸酯。
在一些实施方案中,多官能异氰酸酯包括多异氰酸酯,其作为25℃下的液体单独存在或与少量在25℃下为固体的多异氰酸酯组合。在其他实施方案中,诸如当多元醇是脂族多元醇时,多官能异氰酸酯在25℃下为固体。
在一些实施方案中,多官能异氰酸酯化合物包括脂族异氰酸酯化合物,诸如六亚甲基二异氰酸酯。在其他实施方案中,多官能异氰酸酯化合物包含邻芳族异氰酸酯化合物或间芳族异氰酸酯化合物,诸如1,4-亚甲基二苯基二异氰酸酯(MDI)、间四亚甲基二异氰酸酯(TMXDI)或它们的混合物。也可使用(例如,环状)脂族多官能异氰酸酯化合物和芳族多官能异氰酸酯化合物的混合物。
在一些实施方案中,脂族聚酯多元醇或脂族聚酯多元醇可与芳族多异氰酸酯或环状脂族多异氰酸酯一起使用。
在一些实施方案中,聚氨酯粘合剂组合物包含上述多异氰酸酯和多元醇组分的反应产物,并且还包含由下式表示的含有官能酸的化合物:(HX)2R1 A;其中A是选自-CO2 M、-OSO3 M、-SO3 M、-OPO(OM)2、-PO(OM)2的官能酸基团,其中M为H或阳离子诸如钠、钾和钙;X是O、S、NH或NR,其中R是包含1至10个或1至4个碳原子的烷基基团;并且R1是化合价为至少3的包含1至50个、1至30个、1至15个或1至7个碳原子的有机连接基团,并且任选地包含一个或多个叔氮、醚氧或酯氧原子,并且不具有含异氰酸酯反应性氢的基团。在一些实施方案中,A为-CO2 M,X为O或NH,并且R1为具有1至7个碳原子的直链或支链亚烷基。例示性的含官能酸的化合物包括二羟基羧酸、二羟基磺酸、二羟基膦酸以及它们的盐,诸如如以下示出的二羟甲基丙酸(DMPA)(或以商品名诸如多元醇HA-0135、多元醇HA-0135LV2、多元醇HC-0123和多元醇BA-0132得自GEO特种化学品公司(GEOSpecialty Chemicals,Inc.)的其衍生物):
在一些实施方案中,聚氨酯中的官能酸的量可根据每100克聚氨酯(100gPU)的官能酸基团A的毫摩尔数(mmol A)来描述。就这一点而言,聚氨酯可包括0.001mmol A/100gPU至37mmol A/100g PU、0.1mmol A/100g PU至37mmol A/100g PU、1mmol A/100g PU至37mmol A/100g PU、或1mmolA/100g PU至25mmol A/100g PU。据信在聚氨酯中掺入少量酸官能团还可改善(相对于本公开的没有酸官能团的聚氨酯)粘合性质以及材料对例如极性化学品的耐化学品性。
在一些实施方案中,聚氨酯包含至少25mol%、30mol%、35mol%、40mol%或45mol%的包含至少4个、5个或6个碳原子的亚烷基基团。在一些实施方案中,聚氨酯包含不大于65mol%或60mol%的包含至少4个、5个或6个碳原子的亚烷基基团,其中一些通过使用包含长链亚烷基基团的多异氰酸酯如己二异氰酸酯或异佛乐酮二异氰酸酯来提供。在其他实施方案中,诸如当多异氰酸酯组分主要或仅为芳族多异氰酸酯时,聚氨酯包含不大于约55mol%或50mol%的包含至少4个、5个或6个碳原子的亚烷基基团。如前所述,亚烷基基团通常具有不大于36个、24个、12个或8个碳原子。聚氨酯通过使包含芳族聚酯多元醇和/或具有前述溶解度参数的其他多元醇的多元醇组分与至少一种多官能异氰酸酯化合物反应而获得。此类组合物可任选地包含不损害聚氨酯的期望的耐热性和/或耐化学品性的其它组分。
在一些实施方案中,芳族聚酯多元醇与异氰酸酯组分反应,使得羟基当量(OH基团)相对于NCO异氰酸酯当量(NCO基团)的比率为约1:1。所得聚氨酯的羟基含量不大于约0.5重量%。
在其它实施方案中,聚氨酯聚合物可通过理想配比过剩的有机多异氰酸酯的反应来制备。NCO与OH的摩尔比通常为约1.3:1或1.2:1或1.1:1。
在该实施方案中,NCO末端基团通常还与多官能多元醇反应。合适的多官能多元醇可包括两个或更多个羟基基团,诸如例如支链己二酸二醇、三羟甲基丙烷、1,2,6-己三醇、三羟甲基乙烷、季戊四醇、二季戊四醇、三季戊四醇等。
在其它实施方案中,聚氨酯聚合物可通过理想配比过剩的多元醇的反应来制备。OH与NCO的摩尔比通常为约1.3:1或1.2:1或1.1:1。
在该实施方案中,OH末端基团通常还与多官能多异氰酸酯反应。合适的多官能多异氰酸酯可包含两个或更多个异氰酸酯基团,诸如例如来自拜耳公司(Bayer)的DesmodurN-3300、Desmodur N-3390和Desmodur N-3400。
除了氨基甲酸酯键之外,聚氨酯可含有本领域已知的其它基团,前提条件是此类另外的基团不会降低所需的耐热性和/或耐化学品性。在典型的实施方案中,聚氨酯不含(末端)甲硅烷基基团。
当使多元醇组分与异氰酸酯组分反应时,根据各自反应物的选择和催化剂的选择,反应温度通常在约60℃至约90℃的范围内。反应时间通常在约2小时至约48小时的范围内。
通常用本领域已知的催化剂来制备聚氨酯组合物。催化剂的量的范围可高达聚氨酯的约0.5重量份。在一些实施方案中,催化剂的量的范围为聚氨酯的约0.001重量%至约0.05重量%。有用的催化剂的示例包括但不限于选自锡II和IV盐的那些,诸如辛酸亚锡和二月桂酸二丁基锡以及二乙酸二丁基锡;叔胺化合物诸如三乙胺和双(二甲基氨基乙基)醚、吗啉化合物诸如β,β'-二吗啉代二***、羧酸铋、羧酸锌铋、氯化铁(III)、辛酸钾和乙酸钾。
可使用溶剂来控制聚氨酯的粘度。为此目的而添加的有用溶剂(其通常为挥发性有机化合物)的示例包括但不限于酮(例如甲基乙基酮、丙酮)、叔醇、醚、酯(例如乙酸乙酯)、酰胺、烃、氯代烃、氯碳化合物、以及它们的混合物。
通过实施例中所述的测试方法测定,所得聚氨酯通常具有至少50,000g/摩尔的分子量(Mw)。聚氨酯的分子量(Mw)通常不大于500,000g/摩尔、300,000g/摩尔,或者在一些实施方案中不大于275,000g/摩尔或250,000g/摩尔。
在一些实施方案中,聚氨酯具有在30,000克/摩尔和500,000克/摩尔之间、在50,000-300,000克/摩尔之间、或在75,000-200,000克/摩尔之间的分子量(Mw)。在交联聚氨酯的烯键式不饱和基团之后,分子量(Mw)可甚至更高并且可表现出更好的耐化学品性。在一些实施方案中,本公开的聚氨酯粘合剂可任选地包含化学交联剂。通常,可以使用任何合适的化学交联剂。示例性的化学交联剂包括共价交联剂,诸如双酰胺、环氧化物(例如,N,N,N',-四缩水甘油基-间-苯二甲胺,以商品名“TETRAD-X”得自日本三菱气体化学公司(Mitsubishi Gas Chemical Co.Inc,Japan))、三聚氰胺、多官能胺和氮丙啶(例如,亚丙基亚胺三官能聚氮丙啶,以商品名“PZ-28”得自新泽西州梅福德的聚氮丙啶公司(PolyAziridine,LLC,Medford,NJ));以及离子交联剂诸如金属氧化物和有机金属螯合剂(例如乙酰丙酮铝)。
当聚氨酯由含官能酸的化合物制备并且因此还包含酸性基团时,聚氨酯粘合剂还可包含碳二亚胺(例如,聚碳二亚胺)交联剂,诸如可从佐治亚州卡尔霍恩的斯塔尔公司(Stahl,USA,Calhoun,GA)商购获得。即使在不存在包含酸性基团的聚氨酯的情况下,此类碳二亚胺交联剂以及其他酸反应性化合物也可用作酸清除剂。这些反应涉及在碳二亚胺上加成酸(例如,羧酸)基团以形成脲键。上述其他化学交联剂也可用作酸清除剂。在一些实施方案中,粘合剂组合物还包含至少0.1重量%、0.2重量%、0.3重量%、0.4重量%或0.5重量%的碳二亚胺和/或其他酸反应性化合物。碳二亚胺和/或其他酸反应性化合物的浓度通常不大于粘合剂组合物的5重量%、4重量%、3重量%或2重量%。
聚氨酯聚合物优选在高温和高湿条件下是稳定的。然而,聚氨酯聚合物由于与水的反应而易于发生化学分解。聚氨酯聚合物的水解可产生醇和酸。酸还可催化该水解过程以加速化学分解过程。包含酸反应性化合物尤其是碳二亚胺(例如,聚碳二亚胺)和环氧化合物,可减少此类化学分解。在该实施方案中,这些材料可表征为酸捕集器。酸捕集器不仅减少酸,而且还可使水解过程中生成的那些酸基团重新交联。
当聚氨酯还包含如上所述的烯键式不饱和(例如,(甲基)丙烯酸酯)基团时,聚氨酯粘合剂还可包含多(甲基)丙烯酸酯交联剂,诸如氨基甲酸酯(甲基)丙烯酸酯低聚物。氨基甲酸酯(甲基)丙烯酸酯低聚物可商购获得;例如,以商品名“CN 900系列”得自沙多玛公司(Sartomer)。低聚氨基甲酸酯(甲基)丙烯酸酯也可通过式OCN-R-NCO的亚烷基或芳族二异氰酸酯与多元醇的初始反应来制备。最常见的是,多元醇为式HO-R4-OH的二醇,其中R3为C2-100亚烷基基团或亚芳基基团,并且R4为C2-100亚烷基基团或烷氧基基团。然后,中间产物为聚氨基甲酸酯二醇二异氰酸酯,其随后能经历与(甲基)丙烯酸羟烷基酯的反应。合适的二异氰酸酯包括亚烷基二异氰酸酯,诸如2,2,4-三甲基亚己基二异氰酸酯。根据供应商的报告,多种氨基甲酸酯(甲基)丙烯酸酯低聚物的物理特性阐述如下:
报告的拉伸强度、伸长率和玻璃化转变温度(Tg)特性基于由此类氨基甲酸酯(甲基)丙烯酸酯低聚物制备的均聚物。在一些实施方案中,氨基甲酸酯(甲基)丙烯酸酯低聚物具有低于室温(25℃)的Tg。在一些实施方案中,氨基甲酸酯(甲基)丙烯酸酯低聚物的Tg低于0℃、-5℃或-10℃。该Tg通常为至少-50℃。当氨基甲酸酯(甲基)丙烯酸酯低聚物具有低于室温(25℃)的Tg时,可在交联之后保持高温下的剥离粘合力。在一些实施方案中,氨基甲酸酯(甲基)丙烯酸酯低聚物的拉伸强度小于5,000psi;4,000psi;3,000psi或2,000psi。拉伸强度通常为至少50psi、100psi或150psi。在一些实施方案中,氨基甲酸酯(甲基)丙烯酸酯低聚物的伸长率为至少25%或50%,并且通常不大于500%或400%。在一些实施方案中,氨基甲酸酯(甲基)丙烯酸酯低聚物的粘度可为低的,在60℃下在1000cps至5,000cps的范围内。在其他实施方案中,氨基甲酸酯(甲基)丙烯酸酯低聚物的粘度可为适度的,在60℃下在大于5,000cps至25,000cps的范围内。在其他实施方案中,氨基甲酸酯(甲基)丙烯酸酯低聚物的粘度在60℃下可在大于25,000cps至50,000cps的范围内;60,000cps;70,000cps或80,000cps。在一些实施方案中,使用两种或更多种氨基甲酸酯(甲基)丙烯酸酯低聚物的组合。在一个实施方案中,第一氨基甲酸酯(甲基)丙烯酸酯低聚物具有如前所述的低于25℃的Tg,并且第二氨基甲酸酯(甲基)丙烯酸酯低聚物具有更高的Tg(例如,在至少50℃或75℃至100℃或更高的范围内)。在一些实施方案中,氨基甲酸酯(甲基)丙烯酸酯低聚物优选为脂族的。
在一些实施方案中,可将多(甲基)丙烯酸酯交联剂表征为亲水***联剂。包含亲水性多(甲基)丙烯酸酯交联剂,可在更严格的测试条件下提供良好的耐化学品性(例如,等级“5”),诸如由后文的实施例13和14所示。在一些实施方案中,亲水***联剂可具有大于12的HLB。此类交联剂通常包含两个或三个(甲基)丙烯酸酯基团和亚烷基氧重复单元。亚烷基重复单元通常具有式–[L-O]n-,其中L为直链或支链亚烷基。所述多(甲基)丙烯酸酯交联剂通常包含至少三个或四个邻接的亚烷基氧重复单元。在一些实施方案中,多(甲基)丙烯酸酯交联剂包含至少5个、6个、7个、8个、9个或10个邻接的亚烷基氧重复单元。在一些实施例中,邻接的亚烷基氧重复单元的数量不大于30或25或20或15。
在一些实施方案中,交联剂仅包含亚乙基氧重复单元。在其他实施方案中,交联剂仅包含亚丙基氧重复单元。在其他实施方案中,交联剂仅包含亚丁基氧重复单元。在其他实施方案中,交联剂可包含此类亚烷基氧重复单元的各种组合。例如,多(甲基)丙烯酸酯交联剂可包含亚乙基氧重复单元和亚丙基氧重复单元二者的组合。
在一些实施方案中,多(甲基)丙烯酸酯交联剂可以是脂族的且可由下述通式表示:
其中R1为H或甲基,R2为三价有机残基,L独立地为直链或支链C2至C6亚烷基,并且n为3至30。
在一些实施方案中,R2为包含至少3个、4个、5个或6个碳原子并且通常不大于12个碳原子的烃残基。在一些实施方案中,R为烃残基,其任选地还包含一个或多个氧、硫或氮原子。
聚乙二醇二丙烯酸酯和聚丙二醇二丙烯酸酯通常包含分子的混合物,其中n平均在上述范围内。
在一些实施方案中,采用包含4至5个邻接的亚烷基氧重复单元诸如亚乙基氧重复单元、亚丙基氧重复单元或它们的混合物的三(甲基)丙烯酸酯单体。邻接的亚烷基氧重复单元的数量可不大于15或14或13,并且在一些实施方案中,不大于12或9或10。代表性的单体包括乙氧基化三羟甲基丙烷三(甲基)丙烯酸酯单体,所述丙烯酸酯具有下式:
其中n、m或o中的至少一者为3或4。n+m+o的和通常为至少5、6、7、8、9或10,并且在一些实施方案中不大于30。
此类式的一种代表性单体(其中n、m和o之和为约15)可以商品名“SR9035”得自沙多玛公司(Sartomer)。此类式的另一种代表性单体(其中n、m和o之和为约20)可以商品名“SR415”得自沙多玛公司(Sartomer)。
在其他实施方案中,多(甲基)丙烯酸酯交联剂可表征为芳族的,诸如在乙氧基化双酚二丙烯酸酯交联剂的情况下。
各种可商购获得的多(甲基)丙烯酸酯交联剂描述于下表中。
所包含的交联剂的量取决于熟知的因素,诸如所需的交联度以及交联剂在具体体系中的相对效力。使用化学交联剂交联聚氨酯可使用任何常规技术诸如热引发来引发。在一些实施方案中,本公开的聚氨酯粘合剂可包括基于聚氨酯的总重量计0.1重量%至5重量%或0.1重量%至1重量%的双酰胺交联剂。另选地或另外地,在一些实施方案中,本公开的聚氨酯粘合剂可包括基于聚氨酯的总重量计0.1重量%至5重量%或0.1重量%至2重量%的乙酰丙酮铝交联剂。据信加入化学交联剂还可增强粘合剂的剪切和内聚强度,以及抗化学和高温蠕变性。
作为化学交联的替代或者除了化学交联之外,还包含烯键式不饱和基团和/或多(甲基)丙烯酸酯交联剂的本公开的聚氨酯可通过使聚氨酯经受γ、电子束或紫外辐射(具有或不具有光引发剂)辐射来交联。在该实施方案中,聚氨酯可不含化学交联剂(或它们的残基)。
在一些实施方案中,本文所述的聚氨酯粘合剂包含0.1重量%至2重量%、3重量%、4重量%、5重量%、6重量%、7重量%、8重量%、9重量%或10重量%的多(甲基)丙烯酸酯交联剂,诸如氨基甲酸酯(甲基)丙烯酸酯低聚物和/或上述亲水性多官能(甲基)丙烯酸酯单体。
交联可增加聚氨酯粘合剂的凝胶含量(如根据实施例中所述的测试方法测定)。例如,在不存在(例如,多(甲基)丙烯酸酯)交联剂的情况下,凝胶含量可在5%至10%的范围内。然而,当存在(例如,多(甲基)丙烯酸酯交联剂)时,凝胶含量通常在大于10%、15%、20%、25%、30%、35%、40%、45%或50%至60%或70%的范围内。
在一些实施方案中,压敏粘合剂包含溶解于非水性有机溶剂中的本文所述的聚氨酯聚合物。有机溶剂含量的范围通常为约2重量%至98重量%。所谓的非水性,是指液体介质含有少于3重量%、2重量%或1重量%的水。
除了聚氨酯之外,压敏粘合剂组合物可任选地包含一种或多种添加剂,诸如(例如无机氧化物)填料(诸如(例如热解法)二氧化硅和玻璃泡)、增粘剂、粘合促进剂、增塑剂、(例如化学)发泡剂、触变剂、紫外稳定剂、抗氧化剂、抗静电剂、着色剂、抗冲击助剂、阻燃剂(例如硼酸锌)等。
在一些实施方案中,压敏粘合剂组合物包含增粘剂和/或增塑剂以调节粘合力。在该实施方案中,粘合剂组合物的增粘剂和/或增塑剂的总量通常为总粘合剂组合物的不大于50重量%、40重量%、30重量%、20重量%、15重量%、10重量%或5重量%固体。在其它实施方案中,压敏粘合剂组合物包含很少或不含(即零)增粘剂和/或增塑剂。在该实施方案中,粘合剂组合物包含不大于4重量%、3重量%、2重量%、1重量%、0.5重量%、0.1重量%或0.05重量%的增粘剂和/或增塑剂。
当粘合剂组合物包含很少或不含增粘剂和/或增塑剂时,压敏粘合剂性质(例如粘性、剥离粘合力)通常由聚氨酯的R1基团(例如芳族或脂族聚酯多元醇或聚碳酸酯多元醇)提供。尽管无意于受理论的束缚,可通过使用较长的支链亚烷基基团和/或通过减少交联来增加粘性和剥离粘合力。相反,通过使用较短的支链亚烷基基团或通过增加交联可降低粘性和剥离粘合力。也可通过加入具有更长或更短的亚烷基基团的其它脂族多元醇来调节粘合力。
当期望压敏粘合剂组合物是透明的时,粘合剂通常不含具有大于100nm的粒度的填料,该填料可能降低粘合剂组合物的透明度。在该实施方案中,粘合剂组合物的填料的总量不大于粘合剂组合物的10重量%、9重量%、8重量%、7重量%、6重量%、5重量%、4重量%、3重量%或2重量%固体。在一些有利的实施方案中,粘合剂组合物包含不大于1重量%、0.5重量%、0.1重量%或0.05重量%的填料。
然而,在其它实施方案中,压敏粘合剂可包含更高量的无机氧化物填料,诸如热解法二氧化硅。
在一些实施方案中,压敏粘合剂包含着色剂,诸如包括二氧化钛和炭黑的颜料和染料。此类颜料和染料的浓度范围可为总组合物的至多约20重量%。
包含无机氧化物诸如(例如热解法)二氧化硅和二氧化钛可增加粘合剂组合物的拉伸强度。
可通过使用常规涂覆技术将聚氨酯组合物涂覆在背衬或剥离衬垫上来形成层合胶带。例如,可通过诸如辊涂、流涂、浸涂、旋涂、喷涂、刮涂和模涂的方法来施加这些组合物。涂层厚度可变化。组合物可具有用于后续涂覆的任何期望的浓度,但是通常为有机溶剂中的至少20重量%或25重量%的聚氨酯聚合物固体。在一些实施方案中,涂层包含大于约60重量%的固体聚氨酯。所需浓度可通过进一步稀释涂料组合物或通过部分干燥来实现。涂层厚度可根据压敏粘合剂层的期望厚度而变化。
压敏粘合剂层的厚度范围通常为至少10微米、15微米、20微米、或25微米(1密耳)至500微米(20密耳)厚度。在一些实施方案中,压敏粘合剂层的厚度不大于400微米、300微米、200微米、或100微米。压敏粘合剂可涂覆成单层或多层。
可使用常规涂覆技术将压敏粘合剂组合物涂覆在多种柔性和非柔性背衬材料上以产生单面涂覆或双面涂覆的压敏粘合带。该胶带还可包含剥离材料或剥离衬垫。例如,在单面胶带的情况下,背衬表面的与设置粘合剂之处相反的一侧通常涂覆有合适的剥离材料。剥离材料是已知的,并且包括诸如例如硅氧烷、聚乙烯、聚氨基甲酸酯、聚丙烯酸类等材料。对于双面胶带,将第二层粘合剂设置在背衬表面的相反表面上。第二层也可包含如本文所述的聚氨酯压敏粘合剂或不同的粘合剂组合物。
柔性基底在本文中被定义为常规用作胶带背衬或可为任何其它柔性材料的任何材料。示例包括但不限于聚合物膜、织造或非织造织物;金属箔、泡沫(例如,聚丙烯酸类、聚乙烯、聚氨酯、氯丁橡胶)、以及它们的组合(例如,金属化聚合物膜)。聚合物膜包括例如聚丙烯(例如双轴取向的)、聚乙烯(例如高密度或低密度)、聚氯乙烯、聚氨酯、聚酯(聚对苯二甲酸乙二醇酯)、聚碳酸酯、聚(甲基)丙烯酸甲酯(PMMA)、聚乙烯醇缩丁醛、聚酰亚胺、聚酰胺、含氟聚合物、乙酸纤维素、三乙酸纤维素以及乙基纤维素等。织造或非织造织物可包含合成或天然材料诸如纤维素(例如,组织)、棉、尼龙、人造丝、玻璃、陶瓷材料等等的纤维或长丝。
基底可通过本文所述的压敏粘合剂或层合胶带粘结。基底可包括与刚刚描述的用于背衬的相同的材料。
一种粘结方法包括提供第一基底并使第一基底的表面与压敏粘合剂(例如层合胶带或保护膜)接触。在该实施方案中,压敏粘合剂的相反表面通常临时被剥离衬垫覆盖。
在其它实施方案中,该方法还包括使压敏粘合剂的相反表面与第二基底接触。第一基底和第二基底可由如前所述的各种材料诸如金属、无机材料、有机聚合物材料或它们的组合构成。
在一些粘结方法中,基底、压敏粘合剂或它们的组合可被加热以降低储能模量(G'),并且从而增加(例如剥离)粘合力。基底和/或压敏粘合剂可被加热到至多30℃、或35℃、或40℃、或45℃、或50℃、或55℃、或60℃、或65℃或70℃的温度。在一些实施方案中,借助于在环境温度(例如25℃)下的初始剥离粘合力将一个或多个基底与粘结到该一个或多个基底的粘合剂一起在烘箱中加热至期望的温度。在其它实施方案中,基底和/或压敏粘合剂借助于热风枪加热。
当聚氨酯还包含烯键式不饱和基团时,该烯键式不饱和基团可聚合(例如,通过辐射固化),从而交联聚氨酯或交联剂的烯键式不饱和基团。这可在将压敏粘合剂的相反表面与第二基底接触之前和/或在将压敏粘合剂的相反表面与第二基底接触之后发生。
当压敏粘合剂还包含在使用期间聚合(例如,通过辐射固化)的未交联的烯键式不饱和基团时;压敏粘合剂、层合胶带或保护膜一般被包装在不透明(例如,黑色)容器中,以防止可由于暴露于(例如,可见)光而导致的过早交联。
本文所述的透明粘合剂组合物也可设置在透明膜上以用作可移除的或永久性表面保护膜。在一些实施方案中,压敏粘合剂和透明膜具有至少90%的可见光透射率。
本文所述的压敏粘合剂、层合胶带和保护膜适用于电子、电器、汽车和一般工业产品的领域。在一些实施方案中,压敏粘合剂和层合胶带可用于可结合到家用电器、汽车、计算机(例如平板电脑)和各种手持式装置(例如电话)中的(例如照明的)显示器中。
本发明所公开的粘合剂组合物可在环境温度(25℃)下层合至固体基底,并提供良好的高温/湿度稳定性和耐化学品性。本发明所公开的粘合剂组合物的优异的耐油(例如油酸)性和耐醇性使其对于包括汽车、航空航天、电子产品和电器市场在内的各种应用具有很大的吸引力,在这些应用中在高温/湿度和化学环境下保持粘合剂粘结强度很重要。
在一些实施方案中,本文描述的压敏粘合剂和层合胶带适于粘结诸如液晶显示器(“LCD”)和发光二极管(“LED”)显示器的照明显示装置的内部部件或外部部件,诸如移动电话(包括智能手机)、可穿戴(例如手腕)装置、汽车导航***、全球定位***、测深仪、计算机监视器、笔记本电脑和平板电脑显示器。
在一些实施方案中,压敏粘合剂或层合胶带可表现出低水平的对(例如,浮法)玻璃或不锈钢的粘合力。例如,在65℃和90%相对湿度下的72小时停留时间后,在300毫米/分钟的剥离速率下,室温180°剥离值可在至少0.5N/dm、1N/dm、2N/dm、3N/dm、4N/dm、5N/dm、10N/dm或15N/dm至20N/dm的范围内(如在实施例中的测试方法中进一步描述的)。在其他实施方案中,压敏粘合剂或层合胶带的180°剥离值(例如,可热粘结的)可更高,例如在至少25N/dm、50N/dm、75N/dm、100N/dm、125N/dm至220N/dm的范围内。
在一些实施方案中,压敏粘合剂或层合胶带在暴露于升高的温度和湿度之后,诸如在65℃和90%相对湿度下的72小时停留时间后,可表现出相同的更高水平的与玻璃或不锈钢的粘合力。在一些实施方案中,粘合力的增加不大于300%、250%、200%、150%、100%、90%、80%或70%(如通过从老化剥离值中减去24小时室温值,除以24小时室温值并乘以100%所确定的)。在其他实施方案中,压敏粘合剂或层合胶带在暴露于升高的温度和湿度之后,诸如在85℃和90%相对湿度下的72小时停留时间后,可表现出更低水平的对玻璃或不锈钢的粘合力。
在一些实施方案中,压敏粘合剂或层合胶带在70℃下72小时后不溶解在油酸和/或70%异丙醇水性溶液中。
在一些实施方案中,如可通过动态力学分析(如在实施例中进一步描述的)测量的,压敏粘合剂组合物具有小于1MPa、0.9MPa、0.8MPa、0.7MPa、0.6MPa或0.5MPa的在25℃和1赫兹的频率下的储能模量G'。储能模量随着温度的升高而降低。在一些实施方案中,压敏粘合剂组合物具有小于0.6或0.5的在35℃和1赫兹的频率下的储能模量G'。在一些实施方案中,压敏粘合剂组合物具有小于0.5或0.4的在45℃和1赫兹的频率下的储能模量G'。在一些实施方案中,压敏粘合剂组合物具有小于0.4或0.3的在55℃和1赫兹的频率下的储能模量G'。在一些实施方案中,压敏粘合剂组合物具有小于0.3或0.2的在65℃和1赫兹的频率下的储能模量G'。压敏粘合剂具有小于0.3的在低于70℃、或65℃、或60℃、或55℃、或50℃、或45℃的温度下在1赫兹的频率下的储能模量G'。
压敏粘合剂具有如可通过动态力学分析测量的低于25℃的玻璃化转变温度。在一些实施方案中,玻璃化转变温度低于20℃或15℃。在一些实施方案中,玻璃化转变温度高于0℃。在一些实施方案中,玻璃化转变温度低于0℃、-10℃、-20℃、-30℃或-40℃。
在一些实施方案中,本公开的聚氨酯可用作底漆。在这些实施方案中,聚氨酯可在有机溶剂(例如,MEK)或溶剂混合物中形成为稀溶液(例如,2重量%至20重量%固体)。将该溶液施加到基底并干燥。然后可将压敏粘合剂施加到经干燥的底漆。压敏粘合剂可以是如本文所述的聚氨酯压敏粘合剂。另选地,压敏粘合剂可以是不同的压敏粘合剂,诸如不同的聚氨酯或不同的丙烯酸类粘合剂。作为上述多异氰酸酯、多元醇和含官能酸的化合物的反应产物的本公开聚氨酯可特别适于用作底漆。
实施例
通过下列实施例进一步示出了本公开的优点和实施方案,但这些实施例中所表述的具体材料及其量以及其它条件和细节不应当被解释为对本发明的不当限制。除非另外指明,否则在这些实施例中,所有百分比、比例和比率均按重量计。
除非另外指明或显而易见,否则所有材料都可从例如威斯康星州密尔沃基的西格玛-奥德里奇化学公司(Sigma-Aldrich Chemical Company;Milwaukee,WI)商购获得,或是本领域技术人员已知的。
这些缩写用于以下实施例中:g=克,hr=小时,kg=千克,min=分钟,mol=摩尔;cm=厘米,mm=毫米,mL=毫升,L=升,MPa=兆帕,并且wt=重量。
材料
测试方法
用于测定聚氨酯分子量的方法
使用凝胶渗透色谱法(GPC)对化合物的分子量分布进行表征。GPC仪器(其购自美国马萨诸塞州米尔福德的沃特世公司(Waters Corporation(Milford,MA,USA)))包括高压液相色谱泵(型号1515HPLC)、自动进样器(型号717)、紫外检测器(型号2487)和折射率检测器(型号2410)。该色谱图配备有购自美国加利福尼亚州帕罗奥图的瓦里安有限公司(Varian Inc.(Palo Alto,CA,USA))的两个5微米PL gel MIXED-D色谱柱。聚合物溶液的样品通过如下方式来制备:将干燥的聚合物样品以1.0%(重量/体积)的浓度溶于四氢呋喃中,然后将溶液过滤通过购自美国宾夕法尼亚州西彻斯特的VWR国际有限公司(VWRInternational(West Chester,PA,USA))的0.2微米聚四氟乙烯过滤器。将所得样品注入到GPC中,并以1毫升/分钟的速率洗脱通过保持在35℃的柱。将***用聚苯乙烯标准物校准,使用线性最小二乘法分析来建立标准品校准曲线。根据该标准品校准曲线计算每个样品的重均分子量(Mw)和多分散性指数(用重均分子量除以数均分子量(Mn))。
用于测定初始剥离粘合强度的方法
通过移除易剥离衬垫(通常为RF02N)并且将涂底漆的2密耳(50微米)PET膜层合在粘合剂上,然后将测试条裁切为25.6mm×12.7mm来制备粘合带样品测试条。针对每种粘合剂类型/面板制备两个复制品。移除强粘接衬垫之后,然后沿浮法玻璃基底的长度粘附暴露的粘合剂表面,并卷动5次。在室温(25℃)下在50%相对湿度(RH)下调理24小时后,将测试样品在65℃和90%RH下停留72小时,然后在粘合力测试之前返回道恒定温度(25℃)的室达24小时。使用配备有1000N负荷传感器的张力试验机(MTS Insight,购自明尼苏达州伊甸草原的MTS***公司(MTS Systems,Corporation,Eden Prairie,MN))来评估剥离粘合强度,在测试过程中使用300mm/分钟的夹头速度,以180°的角度,其中试样固定在底部夹具中并且尾部固定在顶部夹具中。
用于耐化学品性测试的方法
通过从每个制备的粘合剂转移胶带样品上切割0.5英寸×0.5英寸(1.27cm×1.27cm)的测试条来制备样品。对于实施例1-12,将剥离衬垫从粘合剂转移胶带的两侧移除,并将该胶带粘附在两个载玻片之间(使得对应于胶带的厚度的边缘暴露)。将通过粘合剂转移胶带粘附的载玻片留出,在室温(RT,约23℃)下停留15分钟,并置于培养皿中。对于实施例13-14,移除一侧上的剥离衬垫,并将测试条附接(粘贴)到玻璃培养皿的底部。移除测试条的第二暴露表面上的剥离衬垫(使得顶表面和边缘暴露)。将含有所附接样品测试条的培养皿留出,以在室温(RT,约23℃)下停留15分钟。然后将样品(带有粘合剂或测试条的载玻片)在70℃下在油酸、香蕉船牌防晒剂、或重量比为75:25(IPA:H2O)的异丙醇(IPA)和水的混合物中浸没72小时。使用以下准则对粘合剂样品对油酸或IPA:H2O混合物的抗性进行评级并报告。如果在72小时后没有出现溶胀、变色或气泡,则将样品评级为“5”;当样品在边缘区域周围具有轻微雾度而本体仍为澄清时,评级为“3”;如果在样品上观察到溶胀、变色和气泡,则将其评级为“1”。
雾度测量方法
使用亨特联合实验室(弗吉尼亚州的雷斯顿)(HunterLab(Reston,VA))的UltrascanPro仪器以透射模式进行雾度测量。将样品切成大约5cm长×10cm长。移除载体衬垫中的一个并将样品层合到一块1mm厚的透明玻璃板。然后移除另一个衬垫,并且将样品放入UltrascanPro中,以测量通过样品和玻璃组件的透射率。
凝胶含量测试方法
将已知重量的待测干粘合剂置于预先称重的筛网篮上。将聚合物和筛网浸没于乙酸乙酯中,并且使其浸泡24小时。浸泡后,用更干净的溶剂洗涤筛网上的任何残余聚合物,并且在70℃下干燥20分钟。干燥后,再次称量样品以获得保留在筛网上的聚合物的重量。重复这一步骤,直至获得稳定的干重。凝胶含量计算为浸泡后保留在筛网上的聚合物的重量除以聚合物的初始重量的比率,再乘以100。
环境老化测试方法
为了制备环境老化样品,首先剥离易剥离衬垫(RF02N),并且用2密耳厚的PET膜代替。然后将样品切成2英寸x4英寸尺寸的片,并且移除那些粘合剂片的强粘接衬垫(诸如J9),并且将样品层合在载玻片上。在室温下停留24小时后,将样品转移至85℃和85%湿度的烘箱持续一段时间。如果发现任何以下观察结果,例如,粘合剂膜变得模糊(超过1%)、形成气泡、以及如果粘合剂由于重力而从其初始位置滑落(所谓滑动)、以及从PET/玻璃的边缘渗出,则我们将其记录为失效。
比较例A(CExA)
向配备有机械搅拌器、冷凝器和氮气入口的树脂反应容器中加入50.0g羟基封端的聚酯PH-56(羟基值为56mg KOH/g)和10.0g MEK。将溶液加热至至多75℃,然后在搅拌下加入2.8g 1重量%的DBTDA在MEK中的溶液和6.256g MODUR MLQ。反应2小时后,加入20g的MEK以稀释该体系(即,降低该体系的粘度)。然后,将温度保持在75℃下持续约10小时,或直到通过FT-IR观察不到游离的NCO基团为止。最后,加入26.5g MEK以将固体含量调节为50重量%,得到澄清且透明的聚氨酯PSA溶液。如上述通过GPC测定,CExA的Mw和多分散度分别为85K和1.98。
将溶液刮涂在剥离衬垫(RF02N)上,在刀与剥离衬垫之间具有0.4mm间隙,以形成粘合剂涂层。将涂层在70℃烘箱中干燥1小时,然后将强粘接剥离衬垫(RF52N)层合在粘合剂表面上。这一PU粘合剂的干燥厚度为约120微米。
实施例1(Ex1)
向配备有机械搅拌器、冷凝器、热电偶和氮气入口的树脂反应容器中加入100.0g羟基封端的聚酯PH-56(羟基值为57mg KOH/g)、1.0g DMPA-0135LV2、1.0g YMER N120和30.0g MEK。在搅拌下将溶液加热至70℃,然后加入0.05g DBTDA和9.23g DESMODUR H。然后,将温度保持在80±2℃,直至反应完成。在反应期间,将所需量的MEK加入到体系中以稀释该体系(即降低该体系的粘度)。当不存在异氰酸酯基团时,反应完成,通过使用FT-IR监测在约2274cm-1处的NCO峰的消失来监测反应。最后,获得固体含量为40重量%的澄清粘稠溶液。如上所述获得GPC数据:Mn=60858,Mw=148224,Mp=96178且Pd=2.43。
将溶液刮涂在剥离衬垫(RF02N)上,在刀与剥离衬垫之间具有0.4mm间隙,以形成粘合剂涂层。将涂层在70℃烘箱中干燥1小时,然后将强粘接剥离衬垫(RF52N)层合在粘合剂表面上。这一PU粘合剂的干燥厚度为约100微米。
实施例2(Ex2)
向配备有机械搅拌器、冷凝器、热电偶和氮气入口的树脂反应容器中加入106.0g羟基封端的聚酯PH-56(羟基值为57mg KOH/g)、1.8g YMER N120和30.0g MEK。在搅拌下将溶液加热至70℃,然后加入0.05g DBTDA和9.39g DESMODUR H。然后,将温度保持在80±2℃,直至反应完成。在反应期间,将所需量的MEK加入到体系中以稀释该体系(即降低该体系的粘度)。当不存在异氰酸酯基团时,反应完成,通过使用FT-IR监测在约2274cm-1处的NCO峰的消失来监测反应。最后,获得固体含量为40重量%的澄清粘稠溶液。如上所述测定GPC数据:Mn=53233,Mw=106654,Mp=89260且Pd=2.0。
将溶液刮涂在剥离衬垫(RF02N)上,在刀与剥离衬垫之间具有0.4mm间隙,以形成粘合剂涂层。将涂层在70℃烘箱中干燥1小时,然后将强粘接剥离衬垫(RF52N)层合在粘合剂表面上。这一PU粘合剂的干燥厚度为约100微米。
实施例3(Ex3)
向配备有机械搅拌器、冷凝器、热电偶和氮气入口的树脂反应容器中加入100.0g羟基封端的聚酯PH-56(羟基值为57mg KOH/g)、0.29gDMPA、5.18g YMER N120和30.0g MEK。在搅拌下将溶液加热至70℃,然后加入0.06g DBTDA和9.44g DESMODUR H。然后,将温度保持在80±2℃,直至反应完成。在反应期间,将所需量的MEK加入到体系中以稀释该体系(即降低该体系的粘度)。当不存在异氰酸酯基团时,反应完成,通过使用FT-IR监测在约2274cm-1处的NCO峰的消失来监测反应。最后,获得固体含量为40重量%的澄清粘稠溶液。如上所述测定GPC数据:Mn=42072,Mw=81940,Mp=68480且Pd=1.95。
将溶液刮涂在剥离衬垫(RF02N)上,在刀与剥离衬垫之间具有0.4mm间隙,以形成粘合剂涂层。将涂层在70℃烘箱中干燥1小时,然后将强粘接剥离衬垫(RF52N)层合在粘合剂表面上。这一PU粘合剂的干燥厚度为约100微米。
实施例4(Ex4)
向配备有机械搅拌器、冷凝器、热电偶和氮气入口的树脂反应容器中加入100.0gPRIPLAST 1838(羟基值为56mg KOH/g)、2.9g YMER N120、30.0g MEK和0.29g BAGDM和0.04g丁基化羟基甲苯。在搅拌下将溶液加热至80℃,然后加入0.06g DBTDA和13.05gTMXDI。然后,将温度保持在80±2℃,直至反应完成。在反应期间,将所需量的MEK加入到体系中以稀释该体系(即降低该体系的粘度)。当不存在异氰酸酯基团时,反应完成,通过使用FT-IR监测在约2274cm-1处的NCO峰的消失来监测反应。最后,获得固体含量为40重量%的澄清粘稠溶液。如上所述测定GPC数据:Mn=21036,Mw=110502,Mp=31589且Pd=5.25。
通过混合100g的上述聚氨酯聚合物溶液、0.05g的KBM-403、0.12g的IRGACURE 184和0.5g的XR-5580来制备涂覆溶液。将所得溶液在辊上再混合1小时,得到均匀的涂覆溶液。
将溶液刮涂在剥离衬垫(RF02N)上,在刀与剥离衬垫之间具有0.4mm间隙,以形成粘合剂涂层。将涂层在70℃烘箱中干燥1小时,然后将强粘接剥离衬垫(J9)层合在粘合剂表面上。然后将粘合剂暴露于所具有的光谱输出为300nm-400nm且最大值在351nm处的低强度紫外线辐射(总能量为1J/cm2)持续约10分钟。所得PU粘合剂的干燥厚度为约120微米。
实施例5(Ex5)
向配备有机械搅拌器、冷凝器、热电偶和氮气入口的树脂反应容器中加入100.0gPRIPLAST 1838(羟基值为56mg KOH/g)、100g PRIPLAST 1900(羟基值为57mg KOH/g)、6.0gYMER N120、30.0g MEK、0.59g BAGDM和0.072g丁基化羟基甲苯。在搅拌下将溶液加热至80℃,然后加入0.06gK-DBTDA和30.99g TMXDI。然后,将温度保持在80±2℃,直至通过FT-IR观察不到NCO峰强度。然后,加入1.75g 2-甲基-1,3-丙二醇以用于扩链。在反应期间,将所需量的MEK加入到体系中以稀释该体系(即降低该体系的粘度)。当不存在异氰酸酯基团时,反应完成,通过使用FT-IR监测在约2274cm-1处的NCO峰的消失来监测反应。最后,获得固体含量为40重量%的澄清粘稠溶液。如上所述测定GPC数据:Mn=29000,Mw=94173,Mp=41792且Pd=3.35。
通过混合100g的上述聚氨酯聚合物溶液、0.05g的KBM-403、0.12g的IRGACURE 184和0.5g的XR-5580来制备涂覆溶液。将所得溶液在辊上再混合1小时,得到均匀的涂覆溶液。
将溶液刮涂在剥离衬垫(RF02N)上,在刀与剥离衬垫之间具有0.4mm间隙,以形成粘合剂涂层。将涂层在70℃烘箱中干燥1小时,然后将强粘接剥离衬垫(J9)层合在粘合剂表面上。然后将粘合剂暴露于所具有的光谱输出为300nm-400nm且最大值在351nm处的低强度紫外线辐射(总能量为1J/cm2)持续约10分钟。所得PU粘合剂的干燥厚度为约120微米。
实施例6(Ex6)
向配备有机械搅拌器、冷凝器、热电偶和氮气入口的树脂反应容器中加入205gPRIPLAST 1838(羟基值为56mg KOH/g)、5.9g YMER N120、0.59g BAGM和50.0g MEK。在搅拌下将溶液加热至80℃,然后加入0.12g K-KAT XC B221和27.84g DESMODUR W。然后,将温度保持在80±2℃以获得含有丙烯酸酯的聚氨酯。在反应期间,将所需量的MEK加入到体系中以稀释该体系(即降低该体系的粘度)。当不存在异氰酸酯基团时,反应完成,通过使用FT-IR监测在约2274cm-1处的NCO峰的消失来监测反应。最后,获得固体含量为50重量%的澄清粘稠溶液。如上所述测定GPC数据:Mn=23323,Mw=123304,Mp=40131且Pd=5.28。
通过混合100g的上述聚氨酯聚合物溶液、0.05g的KBM-403和0.12g的IRGACURE184来制备涂覆溶液。将所得溶液在辊上再混合1小时,得到均匀的涂覆溶液。
将溶液刮涂在剥离衬垫(RF02N)上,在刀与剥离衬垫之间具有0.4mm间隙,以形成粘合剂涂层。将涂层在70℃烘箱中干燥1小时,然后将强粘接剥离衬垫(J9)层合在粘合剂表面上。然后将粘合剂暴露于所具有的光谱输出为300nm-400nm且最大值在351nm处的低强度紫外线辐射(总能量为1J/cm2)持续约10分钟。所得PU粘合剂的干燥厚度为约120微米。
下表1汇总了用于制备Ex1-Ex6和CExA聚氨酯聚合物溶液的组分的量。
表1.
使用上述方法测试Ex1-Ex6和CExA样品的雾度。在雾度测试之前,使样品经受在65℃下在90%RH下的环境老化持续预定时间段。下表2汇总了Ex1-Ex6和CExA样品的雾度数据。
表2.
*N/M表示未测量
使用上述方法测试Ex1-Ex6和CExA样品的剥离粘合强度和耐化学品性。下表3汇总了Ex1-Ex6和CExA样品的剥离粘合强度和耐化学品性数据。
表3:
实施例7(Ex 7)
在8盎司棕色广口瓶中,将100g如实施例6中所述的聚氨酯聚合物溶液(50重量%固体,MEK中)、0.6g Irgacure 184(MEK中,10重量%)、0.5gKBM-403(MEK中,10重量%)和1.0g XR-5580(50重量%,直接使用)混合在一起。将混合物密封并在滚筒搅拌器上放置过夜。
实施例8(Ex 8)
在8盎司棕色广口瓶中,将80g如实施例6中所述的聚氨酯聚合物溶液、0.8gIrgacure 184(MEK中,10重量%)、0.4g KBM-403(MEK中,10重量%)、4.0g CN9782(MEK中,50重量%固体)和0.8g XR-5580(50重量%,直接使用)混合在一起。将混合物密封并在滚筒搅拌器上放置过夜。
实施例9(Ex 9)
在8盎司棕色广口瓶中,将80g如实施例6中所述的聚氨酯聚合物溶液、0.8gIrgacure 184(MEK中,10重量%)、0.4g KBM-403(MEK中,10重量%)、1.6g CN983(MEK中,50重量%)、4.0g CN9782(50重量%固体,MEK中)和0.8g XR-5580(50重量%,直接使用)混合在一起。将混合物密封并在滚筒搅拌器上放置过夜。
实施例10(Ex 10)
在8盎司棕色广口瓶中,将80g如实施例6中所述的聚氨酯聚合物溶液、0.8gIrgacure 184(10重量%,MEK中)、0.4g KBM-403(10重量%,MEK中)、4.0g CN9178(50重量%固体,MEK中)和0.8g XR-5580(50重量%,直接使用)混合在一起。将混合物密封并在滚筒搅拌器上放置过夜。
将实施例7-10的溶液刮涂在剥离衬垫(RF02N)上,在刀与剥离衬垫之间具有0.4mm间隙,以形成粘合剂涂层。将涂层在70℃烘箱中干燥1小时,然后将强粘接剥离衬垫(J9)层合在粘合剂表面上。这一PU粘合剂的干燥厚度为约100微米。将层合的粘合带在氮气下以100%功率(H灯泡)和25fpm在Light HammerTM6高功率6英寸UV固化***(前身为马里兰州盖瑟斯堡的融合UV***公司(Fusion UV Systems,Inc.,Gaithersburg,MD),现为贺利氏特种光源融合UV公司(Heraeus Noblelight Fusion UV Inc.))中UV固化1次。根据先前所述的测试方法测试初始剥离粘合强度,不同的是在50%RH和室温(25℃)下调理24小时后测试样品,并且在环境老化(在85℃和85%RH下停留24小时)后再测试,然后返回到室温持续24小时,之后进行粘附测试。粘合剂性质列在表4中。
表4:
实施例11(EX 11)
向配备有机械搅拌器、冷凝器、热电偶和氮气入口的树脂反应容器中加入160.0gPRIPLAST 1838(羟基值为56mg KOH/g)、40g PRIPLAST1900(羟基值为57mg KOH/g)、6.0gYMER N120、30.0g MEK、0.74g BAGDM和0.0s72g丁基化羟基甲苯。在搅拌下将溶液加热至80℃,然后加入0.12gDBTDA和30.60g TMXDI。然后,将温度保持在80±2℃,直至通过FT-IR观察不到NCO峰强度变化。然后,加入1.5g 2-甲基-1,3-丙二醇以用于扩链。在反应期间,将所需量的MEK加入到体系中以稀释该体系(即降低该体系的粘度)。当不存在异氰酸酯基团时,反应完成,通过使用FT-IR监测在约2274cm-1处的NCO峰的消失来监测反应。最后,获得固体含量为45重量%的澄清粘稠溶液。如上所述测定GPC数据:Mn=34249,Mw=173596且Pd=4.98。
在8盎司棕色广口瓶中,将88.9g上述制备的聚氨酯聚合物(45重量%固体,MEK中)、0.8g Irgacure 184(10重量%,MEK中)、0.4g A-174(10重量%,MEK中)、4.0g CN9178(50重量%固体,MEK中)和1.0g XR-5580(50重量%,直接使用)混合在一起。将混合物密封并在滚筒搅拌器上放置过夜。
实施例12(EX 12)
在8盎司棕色广口瓶中,将88.9g如实施例11中所述制备的聚氨酯聚合物、0.8gIrgacure 184(10重量%,MEK中)、0.4g A-174(10重量%,MEK中)、4.0g CN9178(50重量%固体,MEK中)和2.0g XR-5580(50重量%,直接使用)混合在一起。将混合物密封并在滚筒搅拌器上放置过夜。
实施例13(EX 13)
在8盎司棕色广口瓶中,将88.9g如实施例11中所述制备的聚氨酯聚合物、0.8gIrgacure 184(10重量%,MEK中)、0.4g A-174(10重量%,MEK中)、4.0g CN9178(50重量%固体,MEK中)和3.2g XR-5580(50重量%,直接使用)混合在一起。将混合物密封并在滚筒搅拌器上放置过夜。
将实施例11-13的溶液涂布到剥离衬垫上,并且以与实施例7-10所述相同的方式固化。使样品经受环境老化测试。结果在表5中列出。
表5
在5加仑桶中,加入4000g根据实施例12制备的聚氨酯聚合物(45重量%固体,MEK中)、180g CN9178(50重量%固体,MEK中)、50.2g Irgacure184(10重量%,MEK中)、18g A-174(10重量%,MEK中)和90g XR-5580(50重量%固体,直接使用),再加入额外的368g MEK,将最终溶液在滚筒搅拌器上放置过夜,得到具有40.4%固体的均匀涂覆溶液。过滤该粘合剂溶液,并以16rpm、20rpm和24rpm的流速泵送至20.4cm(8英寸)宽的狭槽型涂布模头中。狭槽式涂布模头将20.4cm宽的涂层均匀地分布到RF02N易剥离衬垫移动纤维网上的以5英尺/分钟移动的基底上。接着,在穿过间隙干燥器和烘箱干燥器后干燥涂层。涂层干燥后,将强粘接涂层衬垫(J9)层合在粘合剂涂层上。使位于RF02N衬垫与J9衬垫之间的粘合剂穿过配备有VPS/1600灯的UV室,该灯可从融合UV***公司(Fusion UV Systems Inc.)购得并使用以100%功率操作的H灯泡。用氮气吹扫该UV室。氮气的流速被固定在11scfm(311升/分钟)。粘合剂涂层厚度分别测量为100微米(16rpm流速)、125微米(20rpm流速)和150微米(24rpm流速)。如下所述测量样品的剥离粘合力、凝胶含量和耐化学品性:
表6:
表7
实施例14(EX 14)
向配备有机械搅拌器、冷凝器、热电偶和氮气入口的树脂反应容器中加入150gPriplast 1901(羟基值为55mg KOH/g)、6.0g Ymer N120、0.74g BAGM和50.0g MEK。在搅拌下将溶液加热至80℃,然后加入0.12g DBTDA和28.78g TMXDI。将温度保持在80±2℃,以获得具有所需NCO含量的含丙烯酸酯的聚氨酯预聚物。然后分别加入50.9g Priplast 3180(羟基值为58.9mg KOH/g)和1.0g 2-甲基-1,3-丙二醇。在反应期间,将所需量的MEK加入到所述体系中以稀释粘度。当不存在异氰酸酯基团时,反应完成,通过使用FT-IR监测在约2274cm-1处的NCO峰的消失来监测反应。最后,获得固体含量为50重量%的澄清粘稠溶液。GPC数据为:Mn=37829,Mw=127887,Mp=55072且Pd=3.38
在8盎司棕色广口瓶中,将100g上述聚氨酯聚合物溶液、3.0g TPO-L(10重量%,MEK中)、0.5g KBM-403(10重量%,MEK中)、1.9g SR415和1.5g XR 5580(50重量%,直接使用)混合在一起。将混合物密封并在滚筒搅拌器上放置过夜。
将实施例14的溶液刮涂在剥离衬垫(RF02N)上,在刀与剥离衬垫之间具有0.4mm间隙,以形成粘合剂涂层。将涂层在70℃烘箱中干燥30分钟,然后将剥离衬垫(J9)层合在粘合剂表面上。粘合剂的干燥厚度为约100微米。将层合的粘合带在氮气下以100%功率(H灯泡)和25fpm在Light HammerTM6高功率6英寸UV固化***(前身为马里兰州盖瑟斯堡的融合UV***公司(Fusion UV Systems,Inc.,Gaithersburg,MD),现为贺利氏特种光源融合UV公司(Heraeus Noblelight Fusion UV Inc.))中UV固化1次。粘合剂的耐化学品性报告于表8中。
表8
Claims (33)
1.一种压敏粘合剂组合物,所述压敏粘合剂组合物包含聚氨酯聚合物,所述聚氨酯聚合物包含多异氰酸酯组分与多元醇组分的反应产物;其中所述多元醇组分包括
至少50重量%的所述多元醇组分包括具有小于10的亲水亲脂平衡的多元醇组分;并且
所述聚氨酯包含0.5重量%至10重量%的、衍生自聚乙二醇聚合物的、分子量大于500g/摩尔的、具有大于12的亲水亲脂平衡的亲水性聚合单元。
2.根据权利要求1所述的压敏粘合剂组合物,其中所述多元醇组分包括聚合的聚酯多元醇、聚合的聚己内酯多元醇,或它们的混合物。
3.根据权利要求1所述的压敏粘合剂组合物,其中所述多元醇组分、多异氰酸酯组分或它们的组合包含至少一个六元环结构。
4.根据权利要求1所述的压敏粘合剂组合物,其中所述多元醇组分、多异氰酸酯组分或它们的组合包含具有至少4个、5个或6个碳原子的亚烷基基团。
5.根据权利要求1所述的压敏粘合剂组合物,其中所述多元醇组分包括无定形聚合的多元醇。
6.根据权利要求1所述的压敏粘合剂组合物,其中所述多异氰酸酯组分包括在25℃下为液体的多异氰酸酯。
7.根据权利要求1所述的压敏粘合剂组合物,其中所述多元醇组分包含邻苯二甲酸酯或间苯二甲酸酯的重复单元和含有至少4个、5个或6个碳原子的亚烷基基团。
8.根据权利要求1所述的压敏粘合剂组合物,其中所述多元醇组分包括基于C36的聚酯多元醇。
9.根据权利要求1所述的压敏粘合剂组合物,其中所述聚氨酯聚合物还包含烯键式不饱和基团。
10.根据权利要求9所述的压敏粘合剂组合物,其中所述烯键式不饱和基团的至少一部分是侧链的。
11.根据权利要求10所述的压敏粘合剂组合物,其中所述烯键式不饱和基团为包含至少两个羟基基团和至少两个烯键式不饱和基团的单体的反应产物。
12.根据权利要求1所述的压敏粘合剂组合物,其中所述聚氨酯聚合物还包含含官能酸的化合物的反应产物。
13.根据权利要求12所述的压敏粘合剂组合物,其中所述含官能酸的化合物由通式(HX)2R1 A表示;其中A是选自-CO2 M、-OSO3 M、-SO3 M、-OPO(OM)2、-PO(OM)2的官能酸基团,其中M为H或阳离子;X是O、S、NH或NR,其中R是包含1至4个碳原子的烷基基团;并且R1是具有至少3的化合价且包含1至50个碳原子的有机连接基团,任选地包含一个或多个叔氮、醚氧或酯氧原子且不含含异氰酸酯反应性氢的基团。
14.根据权利要求13所述的压敏粘合剂组合物,其中A为-CO2 M,X为O或NH,并且R1为具有1至7个碳原子的亚烷基。
15.根据权利要求13所述的压敏粘合剂组合物,其中所述聚氨酯包括0.001mmol A/100g PU至37mmol A/100g PU。
16.根据权利要求9所述的压敏粘合剂组合物,其中在使所述聚氨酯的任何烯键式不饱和基团交联之前,所述聚氨酯具有在75,000g/mol至200,000g/mol范围内的重均分子量。
17.根据权利要求1所述的压敏粘合剂组合物,其中所述压敏粘合剂组合物还包含交联剂、酸反应性化合物、或它们的组合。
18.根据权利要求17所述的压敏粘合剂组合物,其中所述交联剂为多(甲基)丙烯酸酯交联剂。
19.根据权利要求17所述的压敏粘合剂组合物,其中所述交联剂为氨基甲酸酯(甲基)丙烯酸酯低聚物。
20.根据权利要求17所述的压敏粘合剂组合物,其中所述交联剂包含亚烷基氧重复单元。
21.根据权利要求1所述的压敏粘合剂组合物,其中所述压敏粘合剂组合物具有在65℃和90%相对湿度下的72小时停留时间之后,在室温下在300mm/分钟的剥离速率下至少15N/dm至200N/dm的对玻璃的180°剥离力。
22.根据权利要求1所述的压敏粘合剂组合物,其中所述压敏粘合剂组合物具有在70℃下在72小时后在油酸或70%异丙醇水性溶液中3-5的耐化学品性等级。
23.一种层合胶带,所述层合胶带包括:
基底;和
根据权利要求1所述的压敏粘合剂组合物的层,所述层设置在所述基底的主表面上。
24.根据权利要求23所述的层合胶带,其中所述基底是背衬或剥离衬垫。
25.根据权利要求23所述的层合胶带,其中所述压敏粘合剂组合物设置在所述基底的两个主表面上。
26.一种保护膜,所述保护膜包括:
膜;和
根据权利要求1所述的压敏粘合剂组合物的层,所述层设置在所述膜的主表面上。
27.根据权利要求26所述的保护膜,其中所述膜和压敏粘合剂组合物是透明的,并且所述压敏粘合剂组合物具有小于2%的雾度。
28.一种粘结方法,所述方法包括:
提供第一基底;
使所述第一基底的表面与根据权利要求1所述的压敏粘合剂组合物接触。
29.根据权利要求28所述的方法,所述方法还包括使所述压敏粘合剂组合物的相反表面与第二基底接触。
30.根据权利要求29所述的方法,其中所述第一基底和所述第二基底由无机材料、有机聚合物材料,或它们的组合构成。
31.根据权利要求29所述的方法,其中所述第一基底和所述第二基底由金属构成。
32.根据权利要求28所述的方法,其中所述聚氨酯聚合物还包含烯键式不饱和基团,其中将所述压敏粘合剂组合物辐射固化以使所述烯键式不饱和基团交联。
33.一种照明显示装置,所述照明显示装置包括用根据权利要求1所述的压敏粘合剂组合物粘结的部件。
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CN114851661B (zh) * | 2022-04-29 | 2024-06-07 | 宁波腾燊科技发展有限公司 | 一种用于风机叶片前缘保护的复合膜及其生产方法 |
CN115044317B (zh) * | 2022-06-29 | 2024-05-28 | 湖北祥源高新科技有限公司 | 一种双面自粘结聚氨酯泡棉的制备方法和产品 |
TWI836831B (zh) * | 2022-12-30 | 2024-03-21 | 臺灣永光化學工業股份有限公司 | 濕氣固化型熱熔膠組成物及其用途 |
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US20200056072A1 (en) | 2020-02-20 |
CN110520498A (zh) | 2019-11-29 |
EP3589713A1 (en) | 2020-01-08 |
WO2018160350A1 (en) | 2018-09-07 |
EP3589713A4 (en) | 2020-12-30 |
JP7101183B2 (ja) | 2022-07-14 |
JP2020512435A (ja) | 2020-04-23 |
US11629273B2 (en) | 2023-04-18 |
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