CN106916555A - 粘着剂、使用其的粘着片、偏光板粘着片及液晶单元构件 - Google Patents
粘着剂、使用其的粘着片、偏光板粘着片及液晶单元构件 Download PDFInfo
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- CN106916555A CN106916555A CN201611052481.6A CN201611052481A CN106916555A CN 106916555 A CN106916555 A CN 106916555A CN 201611052481 A CN201611052481 A CN 201611052481A CN 106916555 A CN106916555 A CN 106916555A
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- Prior art keywords
- sticker
- methyl
- compound
- acrylic acid
- copolymer
- Prior art date
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Links
- 239000000853 adhesive Substances 0.000 title claims abstract description 32
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 32
- 239000004973 liquid crystal related substance Substances 0.000 title claims abstract description 24
- 210000002858 crystal cell Anatomy 0.000 title claims abstract description 17
- 150000001875 compounds Chemical class 0.000 claims abstract description 65
- 239000000178 monomer Substances 0.000 claims abstract description 55
- 229920001577 copolymer Polymers 0.000 claims abstract description 50
- 239000004593 Epoxy Substances 0.000 claims abstract description 27
- 229910000077 silane Inorganic materials 0.000 claims abstract description 24
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 21
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 13
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 27
- 239000011521 glass Substances 0.000 claims description 21
- 239000012948 isocyanate Substances 0.000 claims description 21
- 150000002513 isocyanates Chemical class 0.000 claims description 14
- 230000003287 optical effect Effects 0.000 claims description 10
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- 238000007667 floating Methods 0.000 abstract description 6
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 28
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- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 26
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 18
- 229910052757 nitrogen Inorganic materials 0.000 description 18
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- 238000006243 chemical reaction Methods 0.000 description 15
- 239000002253 acid Substances 0.000 description 14
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 14
- 150000003254 radicals Chemical class 0.000 description 14
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 11
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- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 9
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- 238000005227 gel permeation chromatography Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 7
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- 238000000576 coating method Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
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- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 7
- 238000010030 laminating Methods 0.000 description 7
- 238000006116 polymerization reaction Methods 0.000 description 7
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- OZAIFHULBGXAKX-UHFFFAOYSA-N 2,2'-azo-bis-isobutyronitrile Substances N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 6
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
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- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 6
- 239000005058 Isophorone diisocyanate Substances 0.000 description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 6
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
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- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 description 5
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- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 5
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 5
- 229920002554 vinyl polymer Polymers 0.000 description 5
- 229920002284 Cellulose triacetate Polymers 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 4
- 239000002202 Polyethylene glycol Substances 0.000 description 4
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 4
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- 150000001336 alkenes Chemical class 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
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- 125000003118 aryl group Chemical group 0.000 description 4
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 4
- OHJMTUPIZMNBFR-UHFFFAOYSA-N biuret Chemical compound NC(=O)NC(N)=O OHJMTUPIZMNBFR-UHFFFAOYSA-N 0.000 description 4
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- 230000000052 comparative effect Effects 0.000 description 4
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- 239000004744 fabric Substances 0.000 description 4
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- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 4
- 238000003475 lamination Methods 0.000 description 4
- 150000002978 peroxides Chemical class 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 4
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Classifications
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Abstract
本发明涉及一种粘着剂、使用其的粘着片、偏光板粘着片及液晶单元构件,粘着剂的剥离性优异,在暴露于高温环境下或高温高湿环境下后,难以产生来自被粘物的浮起或剥落。本发明的粘着剂是包含丙烯酸系共聚物(A)、交联剂(B)、硅烷偶联剂(C)以及具有环氧基或环氧基环己基的化合物(D)而成,并且共聚物(A)为至少含有含羧基的单体(a‑1)单元及含羟基的单体(a‑2)单元的共聚物,化合物(D)为下述式[I]或式[II]所表示的化合物。式中,p、q、r为整数,1≤p≤30、5≤q≤50、5≤r≤50、10≤q+r≤100;X1~X4为烷基,X5为碳数1~10的二价有机残基,Y表示环氧基或环氧基环己基。
Description
技术领域
本发明涉及一种粘着剂、粘着片、偏光板粘着片及液晶单元构件。更详细而言,涉及一种可适合用于塑料或玻璃等构件的粘着剂、粘着片、偏光板粘着片及液晶单元构件。
背景技术
电子计算机、电子钟表、手机、电视机等家庭用或业务用电化制品等多种设备中使用的液晶显示器等显示装置推进大型化,特别是液晶电视或等离子电视等的大型化显著。另外,近年来,以智能手机或平板电脑为代表的触摸面板方式的液晶显示器急速普及,今后也期待大的市场扩大。另一方面,液晶显示器也用于汽车导航等车载设备等,需要能够于高温高湿环境等严酷的车内环境下使用的耐久性。而且,液晶显示器中,使用具有多种光学功能的偏光板或相位差板等,这些构件经由粘着剂而贴附于使用玻璃或透明塑料的液晶单元等被粘物上。
所述偏光板通常是聚乙烯醇膜由三乙酰基纤维素系膜或环烯烃系膜所夹持的构成的积层体。而且,这些膜由于各自的机械特性不同,故而加热时的尺寸变化率不同,因此在放置于高温环境下的情况下,常常在所述积层体上产生翘曲。
此处,例如若将偏光板/粘着剂层/玻璃(玻璃为液晶单元的表面构件)的液晶单元用构件放置于高温环境下,则存在产生以下问题的情况:产生由偏光板的构成构件间的尺寸变化率所引起的翘曲,或在粘着剂层与玻璃的贴附界面产生气泡(发泡),或偏光板自玻璃上浮起而剥落。另外,由于翘曲,液晶单元用构件的应力分布变得不均匀,应力向液晶单元用构件的周边端部集中,结果存在产生如下问题的情况,即,自液晶单元用构件的四角或周边端部漏出光的所谓“漏光现象”。所述问题在高温高湿环境下也同样产生。
另一方面,液晶显示器等的制造步骤中,当将偏光板贴合于液晶单元等光学零件上时,在贴合位置上产生偏移的情况等,贴合后经过一定时间之后将偏光板剥离,将昂贵的液晶单元进行再利用。因此,对粘着剂要求如下特性(再加工性):贴附后经过一定时间后,可将偏光板自液晶单元上再剥离。
为了解决这些问题,专利文献1中公开了如下技术:通过包含使用含芳香环的单体的丙烯酸系共聚物,来提高应力缓和性,防止漏光。但是,专利文献1中列举的使用含芳香环的单体的粘着剂在漏光评价中,存在产生白斑,并且光学特性劣化的问题。
另外,专利文献2中公开了如下技术:为了赋予再剥离性,对重量平均分子量为50万以上的高分子量丙烯酸系聚合体,掺合酸值高且重量平均分子量为0.2万~10万的低分子量丙烯酸系聚合体。但是,专利文献2记载的粘着剂存在粘着剂的干燥条件受到限制的问题。
另一方面,专利文献3中公开了如下技术:通过使用利用两种以上的单体的嵌段聚合物,来提高加热或加湿条件下的耐久性或粘着特性。但是,专利文献3记载的粘着剂存在加热或加湿条件下的透过率下降的问题。
进而,专利文献4中公开了如下技术:通过包含玻璃转移温度为-55℃以上且小于0℃的丙烯酸系共聚物、以及玻璃转移温度为0℃以上180℃以下的丙烯酸系共聚物的水分散型粘着剂,难以产生去极化,且赋予再加工性、回收再利用性。但是,专利文献4记载的粘着剂存在如下问题:由于粘着剂中使用的多种添加剂,历经长期而贴附后的再加工性不足。
另外,专利文献5中公开了如下技术:通过利用含羟基及环氧烷基的丙烯酸系共聚物、以及多官能性异氰酸酯系硬化剂,以硬化状态来构筑相互渗透网络结构,从而抑制高温高湿环境下的浮起剥落。但是,专利文献5记载的粘着剂存在如下问题:当历经长期而放置于高温高湿环境下时,产生环氧烷基的分解,从而产生浮起、剥落。
另外,专利文献6中公开了如下技术:利用含羟基及羧基的丙烯酸系共聚物以及含巯基的硅烷化合物及醇,当在长期放置于高温高湿环境下时,抑制粘着片的浮起、剥落。但是,专利文献6记载的粘着剂存在如下问题:由于使用挥发性高的硅烷化合物,故而当将粘着剂涂敷、干燥时,硅烷化合物挥发,在涂敷后的粘着剂层中未残存足够量的硅烷化合物,因此产生浮起剥落。
[现有技术文献]
[专利文献]
[专利文献1]日本专利特开2007-169329号公报
[专利文献2]日本专利特开2010-100710号公报
[专利文献3]日本专利特开2013-82772号公报
[专利文献4]日本专利特开2014-1365号公报
[专利文献5]日本专利特开2014-055299号公报
[专利文献6]日本专利特开2004-059711号公报
发明内容
[发明所欲解决的课题]
本发明所欲解决的课题是为了解决所述诸多问题,目的为提供一种粘着剂及使用其的粘着片,所述粘着剂当用于粘着片时,剥离性优异,在暴露于高温环境下或高温高湿环境下后,难以产生自被粘物上的浮起或剥落。进而目的为提供一种具有良好的粘着力,并且不会污染玻璃等被粘物的粘着剂及使用其的粘着片,所述粘着剂当用于偏光板固定用途时,漏光评价极少,即便在暴露于高温高湿环境下的情况下,也能够维持高透明性。
[解决课题的手段]
本发明为一种粘着剂,其是包含丙烯酸系共聚物(A)、交联剂(B)、硅烷偶联剂(C)以及分子内具有至少一个环氧基或环氧基环己基的化合物(D)而成,
所述粘着剂在于:所述丙烯酸系共聚物(A)为至少含有含羧基的单体(a-1)单元及含羟基的单体(a-2)单元来作为构成共聚物的单体单元的共聚物,
所述交联剂(B)包含异氰酸酯系化合物,且
所述分子内具有至少一个环氧基或环氧基环己基的化合物(D)为下述式[I]或式[II]所表示的化合物,
[化1]
(式中,p、q、r为表示重复单元的整数,1≤p≤30、5≤q≤50、5≤r≤50、10≤q+r≤100;X1~X4分别独立地表示烷基,X5表示碳数1~10的二价有机残基,Y表示环氧基或环氧基环己基)。
另外,本发明的实施方式涉及所述粘着剂,其中相对于丙烯酸系共聚物(A)100重量份,含有0.05重量份~2重量份的分子内具有至少一个环氧基或环氧基环己基的化合物(D)而成。
另外,本发明的实施方式涉及所述粘着剂,其中所述交联剂(B)为异氰酸酯系化合物。
另外,本发明的实施方式涉及所述粘着剂,其中所述硅烷偶联剂(C)为具有乙氧基的硅烷偶联剂。
另外,本发明的实施方式涉及所述粘着剂,其中相对于丙烯酸系共聚物(A)100重量份,含有0.5重量份~20重量份的交联剂(B)而成。
另外,本发明的实施方式涉及一种粘着片,其包括基材、以及包含所述粘着剂的粘着剂层而成。
另外,本发明的实施方式涉及一种偏光板粘着片,其包括偏光板、以及包含所述粘着剂的粘着剂层而成。
另外,本发明的实施方式涉及一种液晶单元构件,其包括玻璃板、包含所述粘着剂的粘着剂层、以及光学构件而成。
[发明的效果]
通过本发明,能够提供再剥离性优异,在暴露于高温环境下或高温高湿环境下后,例如在玻璃或塑料等上难以自被粘物产生浮起或剥落,可制成难以产生漏光的粘着片的粘着剂。
具体实施方式
以下,对本发明进行详细说明。此外,本说明书中,所谓(甲基)丙烯酸酯是指丙烯酸酯及甲基丙烯酸酯的总称。另外,所谓环氧基环己基是指下述式[III]所表示的基团。
[化2]
本发明的粘着剂在于包含:丙烯酸系共聚物(A)、交联剂(B)、硅烷偶联剂(C)、以及分子内具有至少一个环氧基或环氧基环己基的化合物(D)(以下有时仅记载为化合物(D))。
<丙烯酸系共聚物(A)>
本说明书中的丙烯酸系共聚物(A)为至少含有含羧基的单体(a-1)单元及含羟基的单体(a-2)单元来作为构成共聚物的单体单元的共聚物,可通过将至少含有含羧基的单体(a-1)及含羟基的单体(a-2)的单体混合物进行共聚合而获得。
含羧基的单体(a-1)是指具有羧基的单体(以下,有时略记为单体(a-1))。单体(a-1)不仅通过与交联剂的交联反应而形成聚合物网络,而且与被粘物表面形成氢键,借此有助于抑制浮起及剥落、抑制漏光。单体(a-1)优选为不具有羟基的含羧基的单体。
单体(a-1)具体而言可列举:(甲基)丙烯酸、丙烯酸对羧基苄酯、丙烯酸β-羧基乙酯、顺丁烯二酸、单乙基顺丁烯二酸、衣康酸、柠康酸、反丁烯二酸等。这些单体可单独使用或者并用两种以上。
单体(a-1)优选为在丙烯酸系共聚物中,作为构成共聚物的单体单元而包含0.1重量%~20重量%,更优选为0.5重量%~10%重量%。通过含量成为0.1重量%以上,凝聚力进一步提高。另外,通过含量成为20重量%以下,容易兼具凝聚力与应力缓和性。
含羟基的单体(a-2)是指具有羟基的单体(以下,有时略记为单体(a-2))。单体(a-2)通过与交联剂的交联反应而形成聚合物网络,借此有助于抑制浮起及剥落、抑制漏光。单体(a-2)优选为不具有羧基的含羟基的单体。
单体(a-2)具体而言可列举:(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3-羟基丙酯、(甲基)丙烯酸2-羟基丁酯、(甲基)丙烯酸3-羟基丁酯、(甲基)丙烯酸4-羟基丁酯、(甲基)丙烯酸6-羟基己酯、(甲基)丙烯酸8-羟基辛酯等(甲基)丙烯酸羟基烷基酯,或聚乙二醇单(甲基)丙烯酸酯、聚丙二醇单(甲基)丙烯酸酯、1,4-环己烷二甲醇单(甲基)丙烯酸酯等二醇单(甲基)丙烯酸酯、己内酯改性(甲基)丙烯酸酯等。另外,这些单体可单独使用或者并用两种以上。
单体(a-2)优选为在丙烯酸系共聚物中,作为构成共聚物的单体单元而包含0.05重量份~10重量份,更优选为0.5重量份~5重量份。通过含量成为0.05重量份以上,凝聚力进一步提高。另外,通过含量成为10重量%以下,容易兼具凝聚力与应力缓和性。
作为构成丙烯酸系共聚物(A)的单体单元,所述以外可使用的单体可列举(甲基)丙烯酸烷基酯、此外的乙烯基系单体。(甲基)丙烯酸烷基酯例如可列举:(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸戊酯、(甲基)丙烯酸己酯、(甲基)丙烯酸环己酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸异辛酯、(甲基)丙烯酸癸酯、(甲基)丙烯酸十二烷基酯、(甲基)丙烯酸十四烷基酯、(甲基)丙烯酸十六烷基酯、(甲基)丙烯酸十八烷基酯等。这些单体中,就容易获得良好的粘着性能的方面而言,优选为(甲基)丙烯酸丁酯。这些单体可单独使用或者并用两种以上。
(甲基)丙烯酸烷基酯优选为在丙烯酸系共聚物中,作为构成共聚物的单体单元而包含70重量%~99.85重量%,更优选为85重量%~99.85%重量%。通过含量成为70重量%以上,凝聚力进一步提高。另外,通过含量成为99.85重量%以下,容易兼具凝聚力与应力缓和性。
所述其他的乙烯基系单体可列举:含有酰胺键的单体、含有环氧基的单体、含有氨基的单体、具有环氧烷单元的单体、乙酸乙烯酯、丁烯酸乙烯酯、苯乙烯、丙烯腈等,只要可进行共聚合即可,并不特别限定于这些单体。
含有酰胺键的单体例如可列举:(甲基)丙烯酰胺、N-甲基丙烯酰胺、N-异丙基丙烯酰胺、N,N-二甲基丙烯酰胺、N,N-二乙基丙烯酰胺、N,N-二甲基氨基丙基(甲基)丙烯酰胺、二丙酮丙烯酰胺、N-(羟基甲基)丙烯酰胺、N-(丁氧基甲基)丙烯酰胺等(甲基)丙烯酰胺系化合物,N-乙烯基吡咯烷酮、N-乙烯基己内酰胺、丙烯酰基吗啉等含有杂环的化合物,N-乙烯基甲酰胺、N-乙烯基乙酰胺、N-乙烯基-N-甲基乙酰胺等。
含有环氧基的单体例如可列举:(甲基)丙烯酸缩水甘油酯、(甲基)丙烯酸甲基缩水甘油酯、(甲基)丙烯酸3,4-环氧基环己基甲酯、(甲基)丙烯酸6-甲基-3,4-环氧基环己基甲酯等。
含有氨基的单体例如可列举:(甲基)丙烯酸单甲基氨基乙酯、(甲基)丙烯酸单乙基氨基乙酯、(甲基)丙烯酸单甲基氨基丙酯、(甲基)丙烯酸单乙基氨基丙酯等(甲基)丙烯酸单烷基氨基酯等。
具有环氧烷单元的单体优选为具有环氧乙烷、环氧丙烷等单元。具体而言,例如可列举:丙烯酸2-甲氧基乙酯、丙烯酸2-乙氧基乙酯、丙烯酸2-苯氧基乙酯、甲氧基聚乙二醇(甲基)丙烯酸酯、乙氧基聚乙二醇(甲基)丙烯酸酯、甲氧基聚丙二醇(甲基)丙烯酸酯、乙氧基聚丙二醇(甲基)丙烯酸酯、苯氧基聚乙二醇(甲基)丙烯酸酯、苯氧基聚丙二醇(甲基)丙烯酸酯等。
其他的乙烯基系单体可将这些单体单独使用或者并用两种以上。其他的乙烯基系单体优选为在丙烯酸系共聚物中,作为构成共聚物的单体单元而包含80重量%~99.9重量%,更优选为85重量%~99.5%重量%。通过含量成为80重量%以上,凝聚力进一步提高。另外,通过含量成为99.9重量%以下,容易兼具凝聚力与应力缓和性。
丙烯酸系共聚物(A)的重量平均分子量优选为50万~200万,更优选为70万~180万。通过在50万~200万的范围内,凝聚力等进一步提高,因此更能够抑制浮起及剥落,应力缓和性也进一步提高。另外,丙烯酸系聚合体(A)的分子量分布(表示重量平均分子量(Mw)与数量平均分子量(Mn)的比率的分子量分布(Mw/Mn))优选为2~20。通过在所述范围内,难以产生浮起及剥落,粘着力进一步提高。此外,所述重量平均分子量及数量平均分子量为利用凝胶渗透色谱(gel permeation chromatography,GPC)法来测定的聚苯乙烯换算的值。GPC的测定法的详情记载于实施例中。
丙烯酸系共聚物(A)可通过将单体混合物进行聚合而获得。聚合可为溶液聚合、块状聚合、乳化聚合、悬浮聚合等公知的聚合方法,优选为溶液聚合。溶液聚合中使用的溶媒优选为丙酮、乙酸甲酯、乙酸乙酯、甲苯、二甲苯、苯甲醚、甲基乙基酮、环己酮等。优选为聚合温度为60℃~120℃的沸点反应,聚合时间优选为5小时~12小时。
聚合引发剂优选为自由基聚合引发剂。自由基聚合引发剂若为可在聚合温度下产生自由基的化合物,则并无特别限制,可使用过氧化物及偶氮化合物等公知的化合物。
过氧化物例如可列举:二-叔丁基过氧化物、二枯基过氧化物、叔丁基枯基过氧化物、α,α′-双(叔丁基过氧化-间异丙基)苯、2,5-二(叔丁基过氧化)己炔-3等二烷基过氧化物类;
过氧化苯甲酸叔丁酯、过氧化乙酸叔丁酯、2,5-二甲基-2,5-二(苯甲酰基过氧化)己烷等过氧化酯类;
环己酮过氧化物、3,3,5-三甲基环己酮过氧化物、甲基环己酮过氧化物等酮过氧化物类;
2,2-双(4,4-二-叔丁基过氧化环己基)丙烷、1,1-双(叔丁基过氧化)3,3,5-三甲基环己烷、1,1-双(叔丁基过氧化)环己烷、正丁基-4,4-双(叔丁基过氧化)戊酸酯等过氧化缩酮类;
枯烯氢过氧化物、二异丙基苯氢过氧化物、2,5-二甲基环己烷-2,5-二氢过氧化物等氢过氧化物类;
苯甲酰基过氧化物、癸酰基过氧化物、月桂酰基过氧化物、2,4-二氯苯甲酰基过氧化物等二酰基过氧化物类;
双(叔丁基环己基)过氧化二碳酸酯等过氧化二碳酸酯类等有机过氧化物、或者这些化合物的混合物。
偶氮化合物例如可使用:2,2′-偶氮双异丁腈(2,2′-azobisisobutyronitrile,略称:AIBN)、2,2′-偶氮双(2-甲基丁腈)等2,2′-偶氮双丁腈类;
2,2′-偶氮双(4-甲氧基-2,4-二甲基戊腈)、2,2′-偶氮双(2,4-二甲基戊腈)等2,2′-偶氮双戊腈类;
2,2′-偶氮双(2-羟基甲基丙腈)等2,2′-偶氮双丙腈类;
1,1′-偶氮双(环己烷-1-甲腈)等1,1′-偶氮双-1-烷烃腈类等。
聚合引发剂可单独使用或者并用两种以上。聚合引发剂优选为相对于所述单体混合物100重量份而使用0.01重量份~10重量份,更优选为0.1重量份~2重量份。
<交联剂(B)>
继而,对交联剂(B)进行说明。交联剂通过与丙烯酸系聚合体进行交联反应,形成树脂网络,而获得如下效果:抑制浮起及剥落,抑制漏光,以及在暴露于高温高湿环境下的情况下也可维持高透明性。
交联剂(B)中可列举:异氰酸酯系化合物、环氧化合物、氮丙啶化合物、含酸酐基的化合物、碳二酰亚胺化合物、含有N-羟甲基的化合物以及金属螯合物化合物等。这些化合物中,优选为将异氰酸酯系化合物作为必需。其中,交联剂(B)为除了硅烷偶联剂(C)以及分子内具有至少一个环氧基或环氧基环己基的化合物(D)以外者。
所述异氰酸酯系化合物具体而言为具有2个以上的异氰酸酯基的异氰酸酯单体,具体而言优选为:芳香族聚异氰酸酯、脂肪族聚异氰酸酯、芳香脂肪族聚异氰酸酯、脂环族聚异氰酸酯等异氰酸酯单体,以及缩二脲体、脲酸酯体及加合物。
芳香族聚异氰酸酯例如可列举:1,3-苯二异氰酸酯、4,4′-二苯基二异氰酸酯、1,4-苯二异氰酸酯、4,4′-二苯基甲烷二异氰酸酯、2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、4,4′-甲苯胺二异氰酸酯、2,4,6-三异氰酸酯甲苯、1,3,5-三异氰酸酯苯、联茴香胺二异氰酸酯、4,4′-二苯基醚二异氰酸酯、4,4′,4″-三苯基甲烷三异氰酸酯等。
脂肪族聚异氰酸酯例如可列举: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(hexamethylene diisocyanate,别名:HMDI)、五亚甲基二异氰酸酯、1,2-亚丙基二异氰酸酯、2,3-亚丁基二异氰酸酯、1,3-亚丁基二异氰酸酯、十二亚甲基二异氰酸酯、2,4,4-三甲基六亚甲基二异氰酸酯等。
芳香脂肪族聚异氰酸酯例如可列举:ω,ω′-二异氰酸酯-1,3-二甲基苯、ω,ω′-二异氰酸酯-1,4-二甲基苯、ω,ω′-二异氰酸酯-1,4-二乙基苯、1,4-四甲基苯二甲基二异氰酸酯、1,3-四甲基苯二甲基二异氰酸酯等。
脂环族聚异氰酸酯例如可列举:3-异氰酸酯基甲基-3,5,5-三甲基环己基异氰酸酯(别名:IPDI,异佛尔酮二异氰酸酯(isophorone diisocyanate))、1,3-环戊烷二异氰酸酯、1,3-环己烷二异氰酸酯、1,4-环己烷二异氰酸酯、甲基-2,4-环己烷二异氰酸酯、甲基-2,6-环己烷二异氰酸酯、4,4′-亚甲基双(环己基异氰酸酯)、1,4-双(异氰酸酯基甲基)环己烷等。
缩二脲体是指异氰酸酯单体进行自缩合而成的具有缩二脲键的自缩合物。具体而言,例如可列举六亚甲基二异氰酸酯的缩二脲体等。
脲酸酯体是指异氰酸酯单体的三聚物,例如可列举:六亚甲基二异氰酸酯的三聚物、异佛尔酮二异氰酸酯的三聚物、甲苯二异氰酸酯的三聚物等。
加合物是指异氰酸酯单体与二官能以上的含活性氢的低分子化合物进行反应而成的二官能以上的异氰酸酯化合物,例如可列举:使三羟甲基丙烷与六亚甲基二异氰酸酯进行反应而成的化合物、使三羟甲基丙烷与甲苯二异氰酸酯进行反应而成的化合物、使三羟甲基丙烷与苯二甲基二异氰酸酯进行反应而成的化合物、使三羟甲基丙烷与异佛尔酮二异氰酸酯进行反应而成的化合物、使1,6-己二醇与六亚甲基二异氰酸酯进行反应而成的化合物等。
二官能以上的含活性氢的低分子化合物例如可列举:乙二醇、丙二醇、二乙二醇、丁二醇、1,6-己二醇、3-甲基-1,5-戊二醇、3,3′-二羟甲基庚烷、2-甲基-1,8-辛二醇、3,3′-二羟甲基庚烷、2-丁基-2-乙基-1,3-丙二醇、聚氧乙二醇(环氧乙烷的加成摩尔数为10以下)、聚氧丙二醇(环氧丙烷的加成摩尔数为10以下)、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、1,8-辛二醇、1,9-壬二醇、新戊二醇、丁基乙基戊二醇、2-乙基-1,3-己二醇、环己二醇、环己烷二甲醇,三环癸烷二甲醇、环戊二烯二甲醇、二聚物二醇等脂肪族或脂环族二醇类;
1,3-双(2-羟基乙氧基)苯、1,2-双(2-羟基乙氧基)苯、1,4-双(2-羟基乙氧基)苯、4,4′-亚甲基二苯酚、4,4′-(2-亚降冰片基)二苯酚、4,4′-二羟基联苯酚、邻二羟基苯、间二羟基苯、及对二羟基苯、4,4′-亚异丙基苯酚,或者双酚A或双酚F等使双酚类中加成环氧乙烷、环氧丙烷等环氧烷而成的双酚类等芳香族二醇类;
1,1,1-三羟甲基丙烷、1,1,1-三羟甲基丁烷、1,1,1-三羟甲基戊烷、1,1,1-三羟甲基己烷、1,1,1-三羟甲基庚烷、1,1,1-三羟甲基辛烷、1,1,1-三羟甲基壬烷、1,1,1-三羟甲基癸烷、1,1,1-三羟甲基十一烷、1,1,1-三羟甲基十二烷、1,1,1-三羟甲基十三烷、1,1,1-三羟甲基十四烷、1,1,1-三羟甲基十五烷、1,1,1-三羟甲基十六烷、1,1,1-三羟甲基十七烷、1,1,1-三羟甲基十八烷、1,1,1-三羟甲基十九烷、1,1,1-三羟甲基-仲丁烷、1,1,1-三羟甲基-叔戊烷、1,1,1-三羟甲基-叔壬烷、1,1,1-三羟甲基-叔十三烷、1,1,1-三羟甲基-叔十七烷、1,1,1-三羟甲基-2-甲基-己烷、1,1,1-三羟甲基-3-甲基-己烷、1,1,1-三羟甲基-2-乙基-己烷、1,1,1-三羟甲基-3-乙基-己烷、1,1,1-三羟甲基异十七烷等三羟甲基分支烷烃类,三羟甲基丁烯、三羟甲基庚烯、三羟甲基戊烯、三羟甲基己烯、三羟甲基庚烯、三羟甲基辛烯、三羟甲基癸烯、三羟甲基十二烯、三羟甲基十三烯、三羟甲基十五烯、三羟甲基十六烯、三羟甲基十七烯、三羟甲基十八烯、1,2,6-丁三醇、1,2,4-丁三醇、甘油等三官能多元醇类;
季戊四醇、二季戊四醇、山梨糖醇、木糖醇等四官能以上的多元醇类;
乙二胺、丙二胺、丁二胺、戊二胺、己二胺、庚二胺、辛二胺、壬二胺、二氨基二环己基甲烷、3-氨基甲基-3,5,5-三甲基环己胺、1,3-双(氨基甲基)环己烷、三亚乙基四胺、二亚乙基三胺、三氨基丙烷等脂肪族多胺类;
苯二胺、甲苯二胺、二氨基二苯基甲烷、二氨基二苯基醚等芳香族多胺类;
乙二硫醇、丙二硫醇、丁二硫醇、戊二硫醇、己二硫醇、庚二硫醇、辛二硫醇、壬二硫醇、二巯基二环己基甲烷、3-巯基甲基-3,5,5-三甲基环己基硫醇、1,3-双(巯基甲基)环己烷、1,4-双(3-巯基丁酰氧)丁烷、季戊四醇四(3-巯基丁酸酯)等多硫醇类。这些多官能含活性氢的低分子化合物可单独使用或者并用两种以上。
就形成充分的交联结构的观点而言,异氰酸酯系硬化剂优选为三官能的异氰酸酯化合物,更优选为作为异氰酸酯单体与三官能的含活性氢的低分子化合物的反应物的加合物。具体而言优选为:六亚甲基二异氰酸酯的三羟甲基丙烷加合物、甲苯二异氰酸酯的三羟甲基丙烷加合物、异佛尔酮二异氰酸酯的三羟甲基丙烷加合物、异佛尔酮二异氰酸酯的脲酸酯体、苯二甲基二异氰酸酯的三羟甲基丙烷加合物,尤其优选为:甲苯二异氰酸酯的三羟甲基丙烷的加合物、苯二甲基二异氰酸酯的三羟甲基丙烷加合物等芳香脂肪族系聚异氰酸酯化合物。这些聚异氰酸酯化合物可单独使用或者并用两种以上。
环氧化合物例如可列举:双酚A-表氯醇型的环氧系树脂、乙二醇二缩水甘油醚、聚乙二醇二缩水甘油醚、甘油二缩水甘油醚、甘油三缩水甘油醚、1,6-己二醇二缩水甘油醚、三羟甲基丙烷三缩水甘油醚、二缩水甘油基苯胺、N,N,N′,N′-四缩水甘油基-间苯二甲基二胺、1,3-双(N,N′-二缩水甘油基氨基甲基)环己烷、N,N,N′,N′-四缩水甘油基氨基苯基甲烷等。
氮丙啶化合物例如可列举:N,N′-二苯基甲烷-4,4′-双(1-氮丙啶羰基化物)、N,N′-甲苯-2,4-双(1-氮丙啶羰基化物)、双间苯二甲酰基-1-(2-甲基氮丙啶)、三-1-氮丙啶基氧化膦、N,N′-六亚甲基-1,6-双(1-氮丙啶羰基化物)、2,2′-双羟基甲基丁醇-三[3-(1-氮丙啶基)丙酸酯]、三羟甲基丙烷三-β-氮丙啶基丙酸酯、四羟甲基甲烷三-β-氮丙啶基丙酸酯、三-2,4,6-(1-氮丙啶基)-1,3,5-三嗪、4,4′-双(亚乙基亚氨基羰基氨基)二苯基甲烷等。
碳二酰亚胺化合物可列举:通过在碳二酰亚胺化催化剂的存在下,使二异氰酸酯化合物进行脱羧(decarboxylation)缩合反应而生成的高分子量聚碳二酰亚胺。此种高分子量聚碳二酰亚胺可列举日清纺绩股份有限公司的卡博迪莱特(Carbodilite)系列。其中,卡博迪莱特(Carbodilite)V-01、03、05、07、09与有机溶剂的相容性优异,故而优选。
含酸酐基的化合物为具有2个以上的羧酸酐基的化合物,并无特别限定,优选为:四羧酸二酐、六羧酸三酐、六羧酸二酐、顺丁烯二酸酐共聚合树脂等。此外,反应中可经由脱水反应而成为酐的聚羧酸、聚羧酸酯、聚羧酸半酯等包含于本发明的“含酸酐基的化合物”中。
四羧酸二酐例如可列举:均苯四甲酸酐、二苯甲酮四羧酸二酐、联苯基四羧酸二酐、氧双邻苯二甲酸二酐、二苯基砜四羧酸二酐、二苯基硫醚四羧酸二酐、丁烷四羧酸二酐、苝四羧酸二酐、萘四羧酸二酐等。
金属螯合物化合物例如可列举:铝、铁、铜、锌、锡、钛、镍、锑、镁、钒、铬及锆等多价金属,与乙酰基丙酮或乙酰乙酸乙酯的配位化合物等。具体而言可列举:乙基乙酰乙酸·二异丙醇铝、三乙酰基丙酮酸铝、双乙基乙酰乙酸·单乙酰基丙酮酸铝、烷基乙酰乙酸·二异丙醇铝。
这些交联剂可单独使用或者并用两种以上。这些交联剂中,就兼具基材密合性与再剥离性的观点而言,优选为聚异氰酸酯系化合物。
交联剂(B)优选为相对于丙烯酸系共聚物100重量份而含有0.1重量份~25重量份,更优选为含有0.5重量份~20重量份。若为所述范围内,则容易兼具凝聚力与应力缓和性。
<硅烷偶联剂(C)>
本发明的粘着剂包含硅烷偶联剂。通过使用硅烷偶联剂,可抑制在暴露于高温环境下或者高温高湿环境下的情况下的浮起或剥落。
本说明书中的硅烷偶联剂例如可列举:3-(甲基)丙烯酰氧基丙基三甲氧基硅烷、3-(甲基)丙烯酰氧基丙基三乙氧基硅烷、3-(甲基)丙烯酰氧基丙基三丙氧基硅烷、3-(甲基)丙烯酰氧基丙基三丁氧基硅烷、3-(甲基)丙烯酰氧基丙基甲基二甲氧基硅烷、3-(甲基)丙烯酰氧基丙基甲基二乙氧基硅烷等具有(甲基)丙烯酰氧基的烷氧基硅烷化合物;
乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基三异丙氧基硅烷、乙烯基三丁氧基硅烷、乙烯基甲基二甲氧基硅烷、乙烯基甲基二乙氧基硅烷等具有乙烯基的烷氧基硅烷化合物;
3-氨基丙基三甲氧基硅烷、3-氨基丙基三乙氧基硅烷、3-氨基丙基三丙氧基硅烷、3-氨基丙基甲基二甲氧基硅烷、3-氨基丙基甲基二乙氧基硅烷、N-(2-氨基乙基)-3-氨基丙基三甲氧基硅烷、N-(2-氨基乙基)-3-氨基丙基三乙氧基硅烷、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-氨基丙基甲基二乙氧基硅烷、N-苯基-3-氨基丙基三甲氧基硅烷等具有氨基的烷氧基硅烷化合物;
3-巯基丙基三甲氧基硅烷、3-巯基丙基三乙氧基硅烷、3-巯基丙基三丙氧基硅烷、3-巯基丙基甲基二甲氧基硅烷、3-巯基丙基甲基二乙氧基硅烷等具有巯基的烷氧基硅烷化合物;
3-缩水甘油氧基丙基三甲氧基硅烷、3-缩水甘油氧基丙基三乙氧基硅烷、3-缩水甘油氧基丙基三丙氧基硅烷、3-缩水甘油氧基丙基三丁氧基硅烷、3-缩水甘油氧基丙基甲基二甲氧基硅烷、3-缩水甘油氧基丙基甲基二乙氧基硅烷、2-(3,4-环氧基环己基)乙基三甲氧基硅烷等具有环氧基的烷氧基硅烷化合物;
四甲氧基硅烷、四乙氧基硅烷、四丙氧基硅烷、四丁氧基硅烷等四烷氧基硅烷化合物;
3-氯丙基三甲氧基硅烷、正己基三甲氧基硅烷、正己基三乙氧基硅烷、正癸基三甲氧基硅烷、正癸基三乙氧基硅烷、苯乙烯基三甲氧基硅烷、苯基三甲氧基硅烷、二苯基二甲氧基硅烷、3-三乙氧基硅烷基-N-(1,3-二甲基亚丁基)丙基胺、1,3,5-三(3-三甲氧基硅烷基丙基)异氰脲酸酯、3-异氰酸酯基丙基三甲氧基硅烷、3-异氰酸酯基丙基三乙氧基硅烷、六甲基二硅氮烷、分子内具有烷氧基硅烷基的硅酮树脂等。
硅烷偶联剂可单独使用或者并用两种以上。这些硅烷偶联剂中,就兼具基材密合性与再剥离性的观点而言,优选为具有乙氧基的硅烷偶联剂。硅烷偶联剂优选为相对于丙烯酸系共聚物(A)100重量份而使用0.01重量份~2重量份,更优选为0.05重量份~1重量份的范围。
<分子内具有至少一个环氧基或环氧基环己基的化合物(D)>
本说明书中的分子内具有至少一个环氧基或环氧基环己基的化合物(D)通过与基材表面形成共价键、氢键而有助于抑制浮起及剥落、抑制漏光。
化合物(D)为式[I]或式[II]所表示的化合物,p为1≤p≤30的范围内的整数,优选为1≤p≤30的范围内的整数,更优选为5≤p≤20的范围内的整数。
所述式[II]中,X1~X4分别独立地表示烷基,烷基可列举甲基、乙基、丙基、丁基、戊基、己基等。其中,优选为甲基、乙基、丙基、丁基,更优选为甲基。
X5为碳数1~10的二价有机残基,可列举:亚甲基、1,2-亚乙基、1,3-亚丙基、1,4-亚丁基、1,5-亚戊基、1,6-亚己基、1,7-亚庚基、1,8-亚辛基、1,9-亚壬基、1,10-亚癸基等直链亚烷基,1,1-亚乙基、1,2-亚丙基、1,1-亚丙基、1-甲基-1,3-亚丁基、2-甲基-1,3-亚丁基、1,2-二甲基-1,2-亚丁基、1,1-亚丁基、乙基-1,2-亚乙基等分支状亚烷基等。这些亚烷基中,优选为直链亚烷基,更优选为亚甲基、1,2-亚乙基、1,3-亚丙基、1,4-亚丁基。
Y表示环氧基或环氧基环己基。其中,更优选为环氧基环己基。
q为5≤q≤50的范围内的整数,优选为10≤q≤50的范围内的整数,更优选为10≤q≤40的范围内的整数。
r为5≤r≤50的范围内的整数,优选为10≤r≤50的范围内的整数,更优选为10≤r≤40的范围内的整数。
q+r为10≤q+r≤100的范围内的整数,优选为10≤q+r≤80的范围内的整数,更优选为20≤q+r≤80的范围内的整数。
化合物(D)中,所述式[I]所表示的化合物具体而言可列举:丹纳考尔(Denacol)EX810、丹纳考尔(Denacol)EX811、丹纳考尔(Denacol)EX850、丹纳考尔(Denacol)EX851、丹纳考尔(Denacol)EX821、丹纳考尔(Denacol)EX830、丹纳考尔(Denacol)EX832、丹纳考尔(Denacol)EX841、丹纳考尔(Denacol)EX861“长濑化成(Nagase ChemteX)股份有限公司制造”等。
化合物(D)中,所述式[II]所表示的化合物具体而言可列举:KR-516、X-41-1810、X-40-2651、X-40-9296、KR-513、KR-511(均为信越化学工业公司制造)等。
化合物(D)优选为相对于丙烯酸系共聚物(A)100重量份而含有0.01重量份~10重量份,更优选为含有0.05重量份~5重量份,尤其优选为0.05重量份~2重量份。通过含量成为0.01重量份以上,可获得充分的基材密合性。若含量为所述范围内,则容易兼具基材密合性与再剥离性。
本发明的粘着剂中,若为不损及本发明效果的范围,则也可调配作为任意成分的各种树脂、油、软化剂、染料、颜料、抗氧化剂、紫外线吸收剂、耐候稳定剂、塑化剂、填充剂、抗老化剂及抗静电剂等。
本发明的粘着剂除了适合作为光学构件用粘着剂以外,也可非常有用地用作:各种塑料片、一般标签、片、涂料、弹性壁材、涂膜防水材、地板材、粘着性赋予剂、粘着剂、积层结构体用粘着剂、密封剂、成形材料、表面改质用涂布剂、粘合剂(磁性记录介质、墨水粘合剂、铸件粘合剂、烧结砖(burnt brick)粘合剂、接枝材、微胶囊、玻璃纤维上浆(glassfibre sizing)等)、氨基甲酸酯发泡体(硬质、半硬质、软质)、氨基甲酸酯反应射出成型(Reaction Injection Molding,RIM)、紫外线(ultraviolet,UV)、电子束(electron beam,EB)硬化树脂、高固体涂料(high solid paint)、热硬化型弹性体、微蜂窝(microcellular)、纤维加工剂、塑化剂、吸音材料、阻尼材料、表面活性剂、凝胶涂布剂、人工大理石用树脂、人工大理石用耐冲击性赋予剂、墨水用树脂、膜(层压粘着剂、保护膜等)、夹层玻璃(laminated glass)用树脂、反应性稀释剂、各种成形材料、弹性纤维、人工皮革、合成皮革等原料,另外,也可用作各种树脂添加剂及其原料等。
<粘着片>
本发明的粘着片包括基材、以及包含本发明的粘着剂的粘着剂层。粘着片例如是通过在基材上涂敷粘着剂并干燥,形成粘着剂层而获得。另外,通过在剥离性片涂敷粘着剂并干燥而形成粘着剂层,贴合基材而获得所述粘着片。此外,粘着剂层只要设置于基材的至少一面即可。另外,本发明中,片、膜及带为同义语。另外,当然在粘着剂层的不与基材接触的面上贴合剥离性片。
当涂敷粘着剂时,可添加适当的液状介质,例如:甲苯、二甲苯、己烷、庚烷等烃系溶剂;乙酸乙酯、乙酸丁酯等酯系溶剂;丙酮、甲基乙基酮等酮系溶剂;二氯甲烷、氯仿等卤化烃系溶剂;二***、甲氧基甲苯、二噁烷等醚系溶剂,其他的烃系溶剂等有机溶剂,来调整粘度。另外,也可对粘着剂进行加热而使粘度下降。其中,水或醇等由于会阻碍丙烯酸系共聚物(B)与聚异氰酸酯化合物的交联反应,故而优选为避免使用。
基材例如可列举:玻璃纸、塑料、橡胶、发泡体、布、橡胶布(rubberized cloth)、树脂含浸布、玻璃板、木材等。基材可为板状,也可为膜状。另外,基材也优选为单独或者积层有多个基材的构成。
塑料例如可列举:聚乙烯醇或三乙酰基纤维素、聚丙烯、聚乙烯、聚环烯烃、亚乙基-乙酸乙烯酯共聚物等聚烯烃系树脂,聚对苯二甲酸乙二酯,聚对苯二甲酸丁二酯,聚萘二甲酸乙二酯等聚酯系树脂,聚碳酸酯系树脂、聚降冰片烯系树脂、聚芳酯系树脂(polyarylate resin,PAR:双酚A与邻苯二甲酸的共聚合树脂)、聚丙烯酸系树脂、聚苯硫醚树脂、聚苯乙烯树脂、聚酰胺系树脂、聚酰亚胺系树脂、环氧系树脂(使含环氧基的树脂与多胺或羧酸酐进行反应而成的树脂)等。
本发明中,粘着剂可利用公知的方法来涂敷。例如可列举:迈耶棒(Meyer bar)、敷料器(applicator)、毛刷、喷射、辊、凹版涂布机、模式涂布机、唇式涂布机、缺角轮涂布机、刮刀涂布机、反向涂布机、旋转涂布机等。对干燥方法并无特别限制,可列举利用热风干燥、红外线或减压法的方法。干燥条件通常可为60℃~160℃左右的热风加热。
粘着剂层的厚度优选为0.1μm~300μm,更优选为1μm~100μm。在不满0.1μm的情况下,有时无法获得充分的粘着力,且即便超过300μm,粘着力等性能也不会进一步提高的情况多。
本发明的粘着片可适合用于光学构件的贴合。即优选为在基材上使用光学构件。光学构件具体而言可列举:偏光板、相位差膜、椭圆偏光膜、抗反射膜、亮度提高膜等。
在基材上使用光学构件的本发明的粘着片也优选为贴附于液晶单元的玻璃构件上而用作液晶单元构件。在所述光学构件为偏光板的情况下,当放置于高温环境及高温高湿环境下时,粘着剂层由于应力缓和性良好,故而也能够抑制由偏光板的翘曲所引起的漏光。
本发明的粘着片可优选用于液晶显示器、等离子显示器、触摸面板、电极周边构件等各种电子学相关的构件或保护膜、建材或车辆的窗玻璃等玻璃构件,但也可用于聚烯烃、丙烯腈丁二烯苯乙烯(acrylonitrile butadiene styrene,ABS)、丙烯酸等塑料,纸板,木材,合板(plywood),不锈钢、铝等金属。
[实施例]
以下,通过实施例对本发明进行详细说明,但本发明并不限定于这些实施例。例中,所谓“份”是指“重量份”,所谓“%”是指“重量%”。
<丙烯酸系共聚物(A)的合成>
<合成例1>
在具备搅拌机、温度计、回流冷却管、滴加装置、氮导入管的反应容器(以下,有时仅称为“反应容器”)中,投入99.4份的丙烯酸丁酯、0.5份的丙烯酸、0.1份的丙烯酸2-羟基乙酯、100份的乙酸乙酯、0.025份的2,2′-偶氮双异丁腈(AIBN)后,将反应容器内的空气以氮气进行置换。继而,在氮气环境下一边搅拌,一边加热至80℃,开始反应。进而,使反应溶液在回流温度下反应7小时。反应结束后,进行冷却,以乙酸乙酯加以稀释而获得不挥发成分为30%、粘度为3000mPa·s的共聚物溶液。另外,使用GPC来测定丙烯酸系共聚物的重量平均分子量(Mw),结果,重量平均分子量为100万。将所获得的共聚物设为共聚物(A-1)。
<合成例2~合成例20>
除了分别变更为表1及表2所示的原料及量来代替合成例1中使用的原料以外,利用与合成例1相同的方法来分别合成丙烯酸系共聚物(A-2)~丙烯酸系共聚物(A-20)。将所获得的各丙烯酸系共聚物的重量平均分子量示于表1及表2中。
<重量平均分子量(Mw)的测定>
重量平均分子量(Mw)是使用岛津制作所公司制造的GPC“LC-GPC***”来进行测定,根据作为标准物质的聚苯乙烯的换算值来决定。以下示出测定条件。
装置名:岛津制作所公司制造,LC-GPC***“普罗米内斯(Prominence)”
管柱:将4根东曹公司制造的GMHXL、1根东曹公司制造的HXL-H串联连结。
流动相溶媒:四氢呋喃(tetrahydrofuran,THF)
流量:1.0mL/min
管柱温度:40℃
(实施例1)
调配作为丙烯酸系共聚物(A)的合成例1中获得的共聚物溶液(溶液中的丙烯酸系共聚物(A-1)成为100份的量)、1份作为交联剂(B)的甲苯二异氰酸酯的三羟甲基丙烷的加合物、0.1份作为硅烷偶联剂(C)的3-缩水甘油氧基丙基三乙氧基硅烷、1份作为化合物(D)的表5所示的化合物(D-1),进而,调配不挥发成分成为20%的量的乙酸乙酯,从而获得粘着剂。
以干燥后的厚度成为25μm的方式,将所述粘着剂涂敷于厚度为38μm的聚对苯二甲酸乙二酯制剥离性片(赛拉皮尔(Cerapeel)MF;东丽膜(Toray Film)加工公司制造)上,在100℃下干燥2分钟,借此形成粘着剂层。继而,在该粘着剂层上,贴合将聚乙烯醇(polyvinyl alcohol,PVA)系偏光元件的两面以三乙酰基纤维素系膜(triacetylcellulose,以下称为“TAC膜”)夹持而成的积层结构的偏光板(HLC2-5618:三立(SANRITZ)制造)的单面,获得包含所谓“剥离膜/粘着剂层/TAC膜/PVA/TAC膜”的构成的粘着片。继而,使所获得的粘着片在温度为35℃、相对湿度为55%的条件下熟化1周,获得积层体。
(实施例2~实施例34、比较例1~比较例10)
除了分别变更为表3及表4所示的材料及调配量来代替实施例1中使用的材料以外,以与实施例1相同的方式分别获得粘着剂。进而,以与实施例1相同的方式分别获得粘着片及积层体。
将所使用的化合物(D)的详情示于表5中。
利用以下方法,对所获得的积层体进行评价。
(1)耐热性及耐湿热性评价
将所述获得的积层体切割为宽160mm、纵120mm的大小。继而,自切割出的积层体上剥落剥离性片,使用层压机来贴附于无碱玻璃板上。继而,将贴附有该积层体的玻璃板在50℃、5气压的条件的高压釜内保持20分钟,使各构件密合,借此获得测定试样。对于该测定试样评价耐热性,来作为高温环境下的耐性评价。即,将测定试样在85℃下放置500小时后,以目视来观察发泡、浮起、剥落的有无。
另外,对于测定试样评价耐湿热性,来作为高温高湿环境下的耐性评价。即,将测定试样在60℃、相对湿度95%下放置500小时后,以目视来观察发泡、浮起、剥落的有无。耐热性及耐湿热性均基于以下的基准来进行评价。
◎:完全未确认到发泡、浮起、剥落,良好。
○:虽确认到0.5mm以下的发泡、浮起、剥落的任一种,但在实用上无问题。
×:全面地存在发泡、浮起、剥落,无法使用。
(2)漏光评价
将所述获得的积层体切割为宽160mm、纵120mm的大小。继而,自切割出的积层体上剥落剥离性片,在无碱玻璃板的两面,将各为2片的积层体以其偏光板的吸收轴正交的方式,使用层压机来贴附而获得压接物。继而,使压接物在50℃、5气压的条件的高压釜内保持20分钟,使各构件密合,借此获得测定试样。将该测定试样在85℃下放置500小时后,以目视来观察当使光透过偏光板时的漏光。漏光性是基于以下的基准来进行评价。
◎:无白斑,良好。
○:虽在极少的一部分上确认到白斑,但未确认到全面的白斑,在实用上无问题。
×:全面地存在白斑,无法使用。
(3)再剥离性评价
将所述获得的积层体切割为宽160mm、纵120mm的大小。继而,自切割出的积层体上剥落剥离性片,使用层压机来贴附于无碱玻璃板上。继而,使其在50℃、5气压的条件的高压釜内保持20分钟,使各构件密合,借此获得测定试样。将该测定试样在85℃下放置3小时后,在23℃、相对湿度50%的环境下,使用拉伸试验机(艾安德(Orientec)公司制造的“滕喜龙(Tensilon)”),来进行在180°方向上以300mm/min的速度进行拉伸的剥离试验。继而,以目视来观察剥离后的玻璃表面的模糊,基于以下的基准进行评价。
○:未确认到残胶、模糊,良好。
×:确认到残胶、模糊,无法实用。
(4)粘着力评价
将所获得的积层体切割为宽25mm、纵100mm的大小。继而,自切割出的积层体上剥落剥离性片,使用层压机来贴附于无碱玻璃板上。继而,使其在50℃、5气压的条件的高压釜内保持20分钟,使各构件密合,借此获得测定试样。将该测定试样在23℃下放置1天后,在23℃、相对湿度50%的环境下,使用拉伸试验机(艾安德(Orientec)公司制造的“滕喜龙(Tensilon)”),以剥离速度为300mm/min、剥离角度为180°的条件来测定粘着力(贴合1天后的粘着力)。另外,将所述测定试样在23℃下放置14天后,利用同样的方法来测定粘着力(贴合14天后的粘着力)。
根据表6、表7及表8的结果,如实施例1~实施例34所示,本发明的粘着剂的高温环境及高温高湿环境下的耐久性、漏光性、以及再剥离性优异。另一方面,比较例1~比较例10无法全部满足所述特性。
[表6]
[表7]
[表8]
Claims (8)
1.一种粘着剂,其是包含丙烯酸系共聚物(A)、交联剂(B)、硅烷偶联剂(C)以及分子内具有至少一个环氧基或环氧基环己基的化合物(D)而成,所述粘着剂的特征在于:
所述丙烯酸系共聚物(A)为至少含有含羧基的单体(a-1)单元及含羟基的单体(a-2)单元来作为构成共聚物的单体单元的共聚物,
所述交联剂(B)包含异氰酸酯系化合物,并且
所述分子内具有至少一个环氧基或环氧基环己基的化合物(D)是由下述式[I]或式[II]所表示的化合物,
式中,p、q、r为表示重复单元的整数,1≤p≤30、5≤q≤50、5≤r≤50、10≤q+r≤100;X1~X4分别独立地表示烷基,X5表示碳数1~10的二价有机残基,Y表示环氧基或环氧基环己基。
2.根据权利要求1所述的粘着剂,其特征在于:相对于所述丙烯酸系共聚物(A)100重量份,含有0.05重量份~2重量份的所述分子内具有至少一个环氧基或环氧基环己基的化合物(D)而成。
3.根据权利要求1或2所述的粘着剂,其特征在于:所述交联剂(B)为异氰酸酯系化合物。
4.根据权利要求1或2所述的粘着剂,其特征在于:所述硅烷偶联剂(C)为具有乙氧基的硅烷偶联剂。
5.根据权利要求1或2所述的粘着剂,其特征在于:相对于所述丙烯酸系共聚物(A)100重量份,含有0.5重量份~20重量份的所述交联剂(B)而成。
6.一种粘着片,其特征在于,包括以下构件而成:基材、以及包含根据权利要求1至5中任一项所述的粘着剂的粘着剂层。
7.一种偏光板粘着片,其特征在于,包括以下构件而成:偏光板、以及包含根据权利要求1至5中任一项所述的粘着剂的粘着剂层。
8.一种液晶单元构件,其特征在于,包括以下构件而成:玻璃板、包含根据权利要求1至5中任一项所述的粘着剂的粘着剂层、以及光学构件。
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CN102051146A (zh) * | 2009-10-27 | 2011-05-11 | 琳得科株式会社 | 水分散型丙烯酸系粘着剂组合物和粘着片及其制备方法 |
JP2013224431A (ja) * | 2013-05-20 | 2013-10-31 | Toyo Ink Sc Holdings Co Ltd | 光学用粘着剤および光学用粘着シート |
JP2014234419A (ja) * | 2013-05-31 | 2014-12-15 | 日本カーバイド工業株式会社 | 光学部材用粘着剤組成物及び光学フィルム |
Cited By (2)
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CN112210325A (zh) * | 2019-07-10 | 2021-01-12 | 日东电工(上海松江)有限公司 | 粘合剂组合物 |
CN112210325B (zh) * | 2019-07-10 | 2023-11-17 | 日东电工(上海松江)有限公司 | 粘合剂组合物 |
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JP2017095597A (ja) | 2017-06-01 |
KR20170061070A (ko) | 2017-06-02 |
TWI707017B (zh) | 2020-10-11 |
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