CN106133098A - 粘着剂组合物和包含该粘着剂组合物的偏光板 - Google Patents
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Abstract
本发明提供粘着剂组合物及包含该粘着剂组合物的偏光板和液晶显示装置,所述粘着剂组合物包含丙烯酸系共聚物、交联剂、硅烷偶联剂和pKa值为3以下的强酸。根据本发明的粘着剂组合物具有高粘着强度和优异的耐久性。
Description
技术领域
本发明涉及粘着剂组合物和包含该粘着剂组合物的偏光板。具体地,本发明提供具有高粘着强度和优异的耐久性的粘着剂组合物、包含所述粘着剂组合物的偏光板以及具有所述偏光板的液晶显示装置。
背景技术
液晶显示装置(LCD)具有包括液晶盒和通过粘着剂层层压在液晶盒的两面上的偏光板的液晶面板。
用于将偏光板粘附于液晶盒的粘着剂应同时满足如耐热性、耐热/湿性、耐热冲击性和耐寒性的耐久性,用以解决接触误差或存在的异物的返工性,对于由偏光板的收缩应力产生的漏光的抑制性,以及在移除脱模膜以粘着偏光板时防止静电产生的抗静电特性。在这些特性中,用于实现耐久性和返工性的粘着剂的特征互相冲突。因此,不能完全满足两种物理特性。
为了提供粘着剂对基板良好的粘着性,提出了将硅烷偶联剂添加至粘着剂的技术。日本专利申请公开平4-223403号公开了一种包含如3-环氧丙氧丙基三甲氧基硅烷一样的具有环氧基的硅烷化合物的粘着剂组合物。然而,该粘着剂组合物在实际应用中粘着性和耐久性不足。
发明内容
技术问题
本发明的目的是提供一种粘着剂组合物,其包含pKa值为3以下的强酸而具有高粘着强度和优异的耐久性。
本发明的另一目的是提供包括含有粘着剂组合物的粘着剂层的偏光板。
本发明的又另一目的是提供在液晶盒的至少一个表面上具有偏光板的液晶显示装置。
技术方案
根据本发明的一个方面,提供一种粘着剂组合物,其包含丙烯酸系共聚物、交联剂、硅烷偶联剂和pKa值为3以下的强酸。
在本发明的一个实施方式中,pKa值为3以下的强酸包括草酸或对甲苯磺酸。
根据本发明的另一方面,提供包括含有粘着剂组合物的粘着剂层的偏光板。
根据本发明的又另一方面,提供在液晶盒的至少一个表面上具有偏光板的液晶显示装置。
有益效果
本发明的粘着剂组合物通过强酸的作用来提高硅烷偶联剂的活性,由此大大提高粘着强度,并且容易提供优异的耐久性。
具体实施方式
以下,更详细地描述本发明。
本发明的一个实施方式涉及粘着剂组合物,其包含丙烯酸系共聚物、交联剂、硅烷偶联剂和pKa值为3以下的强酸。
在本发明的一个实施方式中,丙烯酸系共聚物是粘着剂树脂,其可以是具有C1-12烷基的(甲基)丙烯酸酯单体与具有可交联的官能团的单体的共聚物。在此,术语“(甲基)丙烯酸酯”是指丙烯酸酯和甲基丙烯酸酯。
具有C1-12烷基的(甲基)丙烯酸酯单体的例子可包括(甲基)丙烯酸正丁酯、(甲基)丙烯酸2-丁酯、(甲基)丙烯酸叔丁酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸2-乙基丁酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸甲酯、(甲基)丙烯酸正丙酯、(甲基)丙烯酸异丙酯、(甲基)丙烯酸戊酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸异辛酯、(甲基)丙烯酸正壬酯、(甲基)丙烯酸异壬酯、(甲基)丙烯酸癸酯、(甲基)丙烯酸月桂酯等。这些单体可单独使用或组合两种以上使用。其中,优选为丙烯酸正丁酯、丙烯酸2-乙基己酯及它们的混合物。
具有C1-12烷基的(甲基)丙烯酸酯的含量基于丙烯酸系共聚物的制备中所使用的总单体100重量%,优选为80至99重量%,更优选为90至95重量%。如果(甲基)丙烯酸酯单体的含量小于80重量%,则粘着强度可能不足。如果(甲基)丙烯酸酯单体的含量大于99重量%,则凝集强度可能降低。
具有可交联的官能团的单体通过与交联剂化学键合来提供组合物的凝集强度或粘着强度,并且其可包括具有羟基的单体、具有羧基的单体、具有酰胺基的单体、具有叔胺基的单体等。这些单体可单独使用或组合两种以上使用。
具有羟基的单体的例子可包括(甲基)丙烯酸2-羟基乙酯、(甲基)丙烯酸2-羟基丙酯、(甲基)丙烯酸2-羟基丁酯、(甲基)丙烯酸4-羟基丁酯、(甲基)丙烯酸6-羟基己酯、2-羟基乙二醇(甲基)丙烯酸酯、2-羟基丙二醇(甲基)丙烯酸酯、具有C2-4亚烷基的羟基亚烷基二醇(甲基)丙烯酸酯等。其中,优选为(甲基)丙烯酸2-羟基乙酯。
具有羧基的单体的例子可包括:一元酸,例如(甲基)丙烯酸和巴豆酸;二元酸,例如马来酸、衣康酸和富马酸、以及它们单烷基酯;3-(甲基)丙烯酰基丙酸;具有C2-3烷基的(甲基)丙烯酸2-羟基烷基酯的琥珀酸酐开环加合物、具有C2-4亚烷基的羟基亚烷基二醇(甲基)丙烯酸酯的琥珀酸酐开环加合物、将琥珀酸酐开环加成至具有C2-3烷基的(甲基)丙烯酸2-羟基烷基酯的己内酯加合物而获得的化合物等。其中,优选为(甲基)丙烯酸。
具有酰胺基的单体的例子可包括(甲基)丙烯酰胺、N-异丙基丙烯酰胺、N-叔丁基丙烯酰胺等。其中,优选为(甲基)丙烯酰胺。
具有叔胺基的单体的例子可包括N,N-(二甲氨基)乙基(甲基)丙烯酸酯、N,N-(二乙氨基)乙基(甲基)丙烯酸酯、N,N-(二甲氨基)丙基(甲基)丙烯酸酯等。
具有可交联的官能团的单体的含量基于丙烯酸系共聚物的制备中所使用的总单体100重量%,优选为1至20重量%,更优选为1至10重量%。如果具有可交联的官能团的单体的含量小于1重量%,则凝集强度可能降低。如果具有可交联的官能团的单体的含量大于20重量%,则粘着强度可能变差。
除了上述单体以外,丙烯酸系共聚物可在不降低粘着强度的范围、例如10重量%以下、优选5重量%以下进一步含有其他单体。
共聚物可使用但不限于本领域通常已知的本体聚合、溶液聚合、乳化聚合或悬浮聚合等来制备。其中,优选为溶液聚合。此外,可使用本领域通常已知的溶剂、聚合引发剂、用于控制分子量的链转移剂等进行聚合。
丙烯酸系共聚物通过凝胶渗透色谱(GPC)测量的聚苯乙烯转换重均分子量可为50,000至2,000,000,优选为1,000,000至2,000,000。
在本发明的一个实施方式中,交联剂通过交联共聚物来提高粘着剂的凝集强度。举例而言,交联剂可包括但不限于异氰酸酯化合物、环氧化合物等。这些化合物可单独使用或组合两种以上使用。
异氰酸酯化合物的例子可包括:甲苯二异氰酸酯、二甲苯二异氰酸酯、2,4-二苯基甲烷二异氰酸酯、4,4-二苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯、四甲基二甲苯二异氰酸酯、萘二异氰酸酯等二异氰酸酯化合物;和通过1mol三羟甲基丙烷等多元醇化合物与3mol二异氰酸酯化合物反应而获得的加合物、通过3mol二异氰酸酯化合物自缩合而获得的异氰脲酸酯、通过由2mol二异氰酸酯化合物制备的二异氰酸酯脲与1mol二异氰酸酯化合物缩合而获得的缩二脲、三苯基甲烷三异氰酸酯和亚甲基双三异氰酸酯等具有三个官能团的多官能异氰酸酯化合物。
环氧化合物的例子可包括乙二醇二缩水甘油醚、二乙二醇二缩水甘油醚、聚乙二醇二缩水甘油醚、丙二醇二缩水甘油醚、三丙二醇二缩水甘油醚、聚丙二醇二缩水甘油醚、新戊二醇二缩水甘油醚、1,6-己二醇二缩水甘油醚、聚四亚甲基二醇二缩水甘油醚、甘油二缩水甘油醚、甘油三缩水甘油醚、二甘油聚缩水甘油醚、聚甘油聚缩水甘油醚、间苯二酚二缩水甘油醚、2,2-二溴新戊二醇二缩水甘油醚、三羟甲基丙烷三缩水甘油醚、季戊四醇聚缩水甘油醚、山梨醇聚缩水甘油醚、己二酸二缩水甘油酯、邻苯二甲酸二缩水甘油酯、三(缩水甘油基)异氰脲酸酯、三(环氧丙氧乙基)异氰脲酸酯、1,3-双(N,N-缩水甘油基氨基甲基)环己烷、N,N,N’,N’-四缩水甘油基-间苯二甲胺等。
除了异氰酸酯化合物、环氧化合物以外,还可进一步混合使用一种或两种以上三聚氰胺化合物。
三聚氰胺化合物的例子可包括六羟甲基三聚氰胺、六甲氧基甲基三聚氰胺、六丁氧基甲基三聚氰胺等。
交联剂的含量基于100重量份的丙烯酸系共聚物优选为0.1至15重量份、更优选为0.1至5重量份。如果交联剂的含量小于0.1重量份,则会因不充分交联而使凝集强度降低,从而导致粘着耐久性变差且损害切割特性。如果交联剂的含量大于15重量份,则会因过度交联而使残余应力无法充分缓解。
在本发明的一个实施方式中,硅烷偶联剂用于提高粘着剂对基板的粘着性,并且其可以是含有氨基、环氧基、乙酰乙酰基、聚亚烷基二醇基、丙烯酰基和烷基等官能团的烷氧基硅烷,优选为含有环氧基的硅烷偶联剂。
硅烷偶联剂的具体例子可包括乙烯基氯硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、2-(3,4-环氧环己基)乙基三甲氧基硅烷、3-环氧丙氧丙基三甲氧基硅烷、3-环氧丙氧丙基甲基二乙氧基硅烷、3-环氧丙氧丙基二乙氧基硅烷、3-环氧丙氧丙基三乙氧基硅烷、对苯乙烯基三甲氧基硅烷、3-甲基丙烯酰氧丙基三乙氧基硅烷、3-甲基丙烯酰氧丙基三甲氧基硅烷、3-甲基丙烯酰氧丙基甲基二甲氧基硅烷、3-甲基丙烯酰氧丙基甲基二乙氧基硅烷、3-丙烯酰氧丙基三甲氧基硅烷、N-2-(氨基乙基)-3-氨基丙基甲基二甲氧基硅烷、N-2-(氨基乙基)-3-氨基丙基三甲氧基硅烷、N-2-(氨基乙基)-3-氨基丙基甲基三乙氧基硅烷、3-氨基丙基三甲氧基硅烷、3-氨基丙基三乙氧基硅烷、3-三乙氧基甲硅烷基-N-(1,3-二甲基亚丁基)丙胺、N-苯基-3-氨基丙基三甲氧基硅烷、3-氯丙基三甲氧基硅烷、3-巯基丙基甲基二甲氧基硅烷、3-巯基丙基三甲氧基硅烷、双(三乙氧基甲硅烷基丙基)四硫化物、3-异氰酸丙基三乙氧基硅烷等。优选为2-(3,4-环氧环己基)乙基三甲氧基硅烷、3-环氧丙氧丙基三甲氧基硅烷、3-环氧丙氧丙基甲基二乙氧基硅烷、3-环氧丙氧丙基二乙氧基硅烷和3-环氧丙氧丙基三乙氧基硅烷等环氧系硅烷。这些化合物可单独使用或组合两种以上使用。
硅烷偶联剂的含量基于100重量份的丙烯酸系共聚物优选为0.01至2重量份,更优选为0.01至0.5重量份。如果硅烷偶联剂的含量小于0.01重量份,则增加粘着强度的效果不足而在耐热条件下引起剥离缺陷。如果硅烷偶联剂的含量大于2重量份,则增加粘着强度的效果可能变差。
在本发明的一个实施方式中,强酸可以是pKa值为3以下的任意的酸,考虑到在有机溶剂中的溶解性,优选pKa值为3以下的有机酸。强酸的具体例子可以包括草酸、硝基乙酸和氯乙酸等带有吸电子取代基的乙酸衍生物;对甲苯磺酸、苯磺酸、甲磺酸和三氟甲磺酸等有机磺酸;苯基膦酸等有机磷酸衍生物。其中,优选为草酸和对甲苯磺酸。
强酸的含量基于100重量份的丙烯酸系共聚物优选为0.001至0.1重量份。如果强酸的含量小于0.001重量份,则增加粘着强度的效果可能不足。如果强酸的含量大于0.1重量份,则可能因凝胶分率不足而使凝集强度降低。
根据本发明的一个实施方式的粘着剂组合物视需要可进一步包含增粘树脂、抗氧化剂、流平剂、表面润滑剂、染料、颜料、消泡剂、填充剂、光稳定剂及抗静电剂等添加剂,以控制粘着力、凝集力、粘度、弹性、玻璃化转变温度、抗静电特性等。
本发明的粘着剂组合物可用作粘附偏光板与液晶盒的粘着剂及表面保护膜用粘着剂。此外,粘着剂组合物也可用作以下用途的粘着剂:保护膜、反射片、用于结构的粘着剂片、用于照片的粘着剂片、用于行车道的粘着剂片、光学粘着剂产品、电子部件、一般粘着剂片产品和医用贴片。
本发明的一个实施方式涉及包括含有上述粘着剂组合物的粘着剂层的偏光板。
粘着剂层的厚度可根据其粘着强度而变化,优选为3μm至100μm,更优选为10μm至100μm。
这样的偏光板可应用于典型的液晶显示装置。具体地,偏光板可用于制造包括液晶面板的液晶显示装置,其中具有粘着剂层的偏光板层压在液晶盒的至少一面上。
因此,本发明的一个实施方式涉及在液晶盒的至少一面上具有偏光板的液晶显示装置。
以下,通过实施例、比较例和实验例来进一步说明本发明,其不应理解为限制本发明的范围。
制备例1:丙烯酸系共聚物的制备
向安装有冷却装置且流有氮气流的1L反应器添加由85重量份的丙烯酸正丁酯(BA)、7重量份的丙烯酸甲酯(MA)和5重量份的丙烯酸2-羟基乙酯和3重量份的丙烯酸组成的单体混合物,然后添加100重量份的乙酸乙酯(EAc)作为溶剂。之后,用氮气净化1小时以移除氧,随后将温度维持在62℃。将混合物均匀搅拌后,向其添加0.07重量份的偶氮二异丁腈(AIBN)作为反应引发剂,并且使所得混合物反应8小时,以获得重均分子量为约1,000,000的丙烯酸系共聚物。
实施例1至12及比较例1至4:附粘着剂的偏光板的制备
将表1列出的组分混合以获得粘着剂组合物(单位:重量份)。
将由此获得的粘着剂组合物以固化后的厚度为25μm的方式涂布在涂覆有硅脱模剂的膜上,并在100℃下干燥1分钟以形成粘着剂层。在其上,层压另一脱模膜以获得粘着剂片。
从上面制备的粘着剂片剥离脱模膜后,将粘着剂层粘附于厚度185μm的包含TAC保护膜的碘系偏光板以制备附粘着剂的偏光板。
[表1]
丙烯酸系共聚物 | 交联剂 | 硅烷偶联剂 | 强酸 | |
实施例1 | 制备例1(100) | Coronate-L(0.5) | KBM-403(0.5) | C-1(0.001) |
实施例2 | 制备例1(100) | Coronate-L(0.5) | KBM-403(0.5) | C-1(0.01) |
实施例3 | 制备例1(100) | Coronate-L(0.5) | KBM-403(0.5) | C-1(0.1) |
实施例4 | 制备例1(100) | Coronate-L(0.5) | KBM-403(0.5) | C-2(0.001) |
实施例5 | 制备例1(100) | Coronate-L(0.5) | KBM-403(0.5) | C-2(0.01) |
实施例6 | 制备例1(100) | Coronate-L(0.5) | KBM-403(0.5) | C-2(0.1) |
实施例7 | 制备例1(100) | Coronate-L(0.5) | KBM-403(0.5) | C-2(0.15) |
实施例8 | 制备例1(100) | Coronate-L(0.5) | KBM-4803(0.5) | C-2(0.001) |
实施例9 | 制备例1(100) | Coronate-L(0.5) | KBM-403(0.1) | C-2(0.001) |
实施例10 | 制备例1(100) | Coronate-L(0.5) | KBM-403(0.01) | C-2(0.001) |
实施例11 | 制备例1(100) | Coronate-L(0.5) | KBM-403(2.5) | C-2(0.001) |
实施例12 | 制备例1(100) | D110N(0.5) | KBM-403(0.5) | C-2(0.001) |
比较例1 | 制备例1(100) | Coronate-L(0.5) | KBM-403(0.5) | - |
比较例2 | 制备例1(100) | Coronate-L(0.5) | KBM-4803(0.5) | - |
比较例3 | 制备例1(100) | Coronate-L(0.5) | KBM-403(0.5) | C-3(0.1) |
比较例4 | 制备例1(100) | Coronate-L(0.5) | KBM-403(0.5) | C-4(0.1) |
交联剂:Coronate-L(TDI/TMP加合物,日本聚氨酯工业(Nippon PolyurethaneIndustry))
D110N(二甲苯二异氰酸酯(XDI)的加合物,三井化学有限公司(MitsuiChemicals,Inc.))
硅烷偶联剂:KBM-403(信越(Shin-Etsu))
KBM-4803(信越(Shin-Etsu))
C-1:草酸(pKa=2.83)
C-2:对甲苯磺酸(pKa<0)
C-3:苯甲酸(pKa=3.77)
C-4:十三酸(pKa=4.75)
实验例1:粘着强度和耐热性的评价
使用以下方法测量在实施例和比较例中制备的附粘着剂的偏光板的物理特性,并且将结果示于表2中。
(1)粘着强度
将附粘着剂的偏光板切割为25mm×100mm的大小。在剥离脱模膜后,将偏光板以0.25MPa层压在玻璃基板上,并在50℃、490pa和20分钟的条件下进行高压釜处理以获得样品。
将上述样品在25℃、50%RH下静置24小时,使用万能测试机(UTM,英斯特朗(Instron))测量以10m/min的剥离速率和180°的剥离角进行剥离时的样品的粘着强度。该测量在25℃、50%RH下进行。
(2)耐热性
在从附粘着剂的偏光板剥离脱模膜后,将所述板层压在玻璃(康宁有限公司(Corning Inc.))上,随后进行高压釜处理。在85℃下静置300小时后,观察到气泡或剥离的发生。
<评价标准>
×:至少3个气泡或剥离
Δ:不多于2个气泡或剥离
○:无气泡或剥离
[表2]
粘着强度(N/25mm) | 耐热性 | |
实施例1 | 8.7 | ○ |
实施例2 | 12.8 | ○ |
实施例3 | 21.5 | ○ |
实施例4 | 19.8 | ○ |
实施例5 | 22.0 | ○ |
实施例6 | 21.2 | ○ |
实施例7 | 20.0 | ○ |
实施例8 | 15.7 | ○ |
实施例9 | 18.2 | ○ |
实施例10 | 12.8 | ○ |
实施例11 | 6.9 | Δ |
实施例12 | 22.3 | ○ |
比较例1 | 3.1 | × |
比较例2 | 2.0 | × |
比较例3 | 3.2 | × |
比较例4 | 3.5 | × |
如表2所示,与仅使用硅烷偶联剂的比较例1和2的偏光板和使用弱酸的比较例3和4的偏光板相比,根据本发明的使用强酸的实施例1至12的偏光板,显示出显著优异的粘着强度和耐热性。
尽管示出并描述了本发明的具体实施方式,但本领域技术人员应该理解,本发明并不意欲限制于优选的实施方式,并且对于本领域技术人员显而易见的是,在不背离本发明的精神和范围的情况下可进行多种改变和修改。
因此,本发明的范围由随附的权利要求及其等效内容来限定。
Claims (8)
1.一种粘着剂组合物,其包含丙烯酸系共聚物、交联剂、硅烷偶联剂和pKa值为3以下的强酸。
2.如权利要求1所述的粘着剂组合物,其中,所述硅烷偶联剂的含量基于100重量份的丙烯酸系共聚物为0.01至2重量份。
3.如权利要求1所述的粘着剂组合物,其中,所述pKa值为3以下的强酸是有机酸。
4.如权利要求1所述的粘着剂组合物,其中,所述pKa值为3以下的强酸是乙酸衍生物、有机磺酸或有机磷酸衍生物。
5.如权利要求1所述的粘着剂组合物,其中,所述pKa值为3以下的强酸是草酸或对甲苯磺酸。
6.如权利要求1所述的粘着剂组合物,其中,所述pKa值为3以下的强酸的含量基于100重量份的丙烯酸系共聚物为0.001至0.1重量份。
7.一种偏光板,其包括包含权利要求1至6中的任一项所述的粘着剂组合物的粘着剂层。
8.一种液晶显示装置,其在液晶盒的至少一面上的具有权利要求7所述的偏光板。
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- 2015-03-26 TW TW104109826A patent/TW201536881A/zh unknown
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Also Published As
Publication number | Publication date |
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KR20150111635A (ko) | 2015-10-06 |
KR102149235B1 (ko) | 2020-08-28 |
WO2015147498A1 (ko) | 2015-10-01 |
US20170101561A1 (en) | 2017-04-13 |
TW201536881A (zh) | 2015-10-01 |
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