CN105462526A - 一种粘合剂组合物 - Google Patents
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Abstract
本发明公开了一种粘合剂组合物,由以下成分(A)、成分(B)、成分(C)和成分(D)组成:(A)以下的单体成分(a1)、(a2)和(a3)共聚而成的重均分子量Mw为210万~250万,且共聚物的分子量分布(Mw/Mn)为15~25的丙烯酸类聚合物;(a1)85~95重量%(甲基)丙烯酸烷氧基烷基酯,所述(甲基)丙烯酸烷氧基烷基酯选自(甲基)丙烯酸甲氧基乙酯和(甲基)丙烯酸乙氧基乙酯,(a2)0.5-5重量%含羧基的单体,所述含羧基的单体选自(甲基)丙烯酸、马来酸、富马酸,(a3)1~10重量%含羟基的单体,所述含羟基的单体选自2-羟基乙基(甲基)丙烯酸酯、4-羟基丁基(甲基)丙烯酸酯、2-羟基丙基(甲基)丙烯酸酯、2-羟基丁基(甲基)丙烯酸酯;(B)相对于100重量份丙烯酸类聚合物0.5~5重量份异氰酸酯类交联剂;(C)相对于100重量份丙烯酸类聚合物0.5~1.0重量份硅烷偶联剂;(D)相对于100重量份丙烯酸类聚合物0.1~0.5重量份交联促进剂。所述粘合剂组合物可用于光学构件中。
Description
技术领域
本发明属于粘合剂材料技术领域,具体涉及一种粘合剂组合物。
背景技术
在液晶单元上贴附所述光学薄膜时,通常可以使用粘合剂。另外,在光学薄膜和液晶元件、还有光学薄膜之间的粘接中,通常为了减少光损失,使用粘合剂粘附各个材料。在这种情况下,由于具有在使光学薄膜固着时不需要经过干燥工序等优点,因此通常使用的是粘合剂作为粘合剂层预先被设置在光学薄膜的一侧上的粘合型光学薄膜。
适用所述粘合型光学薄膜的液晶显示装置等的图像显示装置被用在各种环境下。所以,所述粘合型光学薄膜被希望具有在高温环境下的耐热性、在高湿环境下的耐湿性等耐久性。作为改善该耐久性的方法,提出了使用由含氨基及/或酰胺基的(甲基)丙烯酸系单体作为0.3~10重量%的共聚合成分的(甲基)丙烯酸系树脂构成的粘合剂,作为在偏振光薄膜与液晶单元的玻璃基板之间的粘合剂。
另一方面,近年来,图像显示装置被希望薄型化,粘合型光学薄膜也被希望薄型化。随着这种薄型化的要求,粘合型光学薄膜的粘合剂层也被需要薄型化。但是,如果薄型化粘合剂层,则变得难以满足耐久性。即使在使用所述专利文献1(日本)特开平6—108025号公报中记载的粘合剂的情况下,如果粘合剂层变薄,也变得难以满足耐久性。
因此,需要提供一种用于光学薄膜的粘合剂组合物,在具有良好粘合力的同时,具有需要的耐热、耐湿性,并且不易产生气泡、有效地防止发生漏光。
发明内容
本发明的目的在于提供一种粘合剂组合物,用于光学薄膜时在具有良好粘合力的同时,具有提高的耐热、耐湿性,并且不易发泡、有效地防止发生漏光。
本发明的技术方案如下:
一种粘合剂组合物,其特征在于,由以下成分(A)、成分(B)、成分(C)和成分(D)组成:
(A)以下的单体成分(a1)、(a2)和(a3)共聚而成的重均分子量Mw为210万~250万,且共聚物的分子量分布(Mw/Mn)为15~25的丙烯酸类聚合物;
(a1)85~95重量%(甲基)丙烯酸烷氧基烷基酯,所述(甲基)丙烯酸烷氧基烷基酯选自(甲基)丙烯酸甲氧基乙酯和(甲基)丙烯酸乙氧基乙酯,
(a2)0.5-5重量%含羧基的单体,所述含羧基的单体选自(甲基)丙烯酸、马来酸、富马酸,
(a3)1~10重量%含羟基的单体,所述含羟基的单体选自2-羟基乙基(甲基)丙烯酸酯、4-羟基丁基(甲基)丙烯酸酯、2-羟基丙基(甲基)丙烯酸酯、2-羟基丁基(甲基)丙烯酸酯;
(B)相对于100重量份丙烯酸类聚合物0.5~5重量份异氰酸酯类交联剂;
(C)相对于100重量份丙烯酸类聚合物0.5~1.0重量份硅烷偶联剂;
(D)相对于100重量份丙烯酸类聚合物0.1~0.5重量份交联促进剂。其中,所述异氰酸酯类交联剂选自甲苯二异氰酸酯、氯苯二异氰酸酯、六亚甲基二异氰酸酯、四亚甲基二异氰酸酯、异佛尔酮二异氰酸酯、二苯基甲烷二异氰酸酯;
所述丙烯酸类聚合物(A)的重均分子量Mw为220-230万,优选为220万;
所述丙烯酸类聚合物(A)的分子量分布为20-25;
所述硅烷偶联剂选自3-环氧丙氧基丙基三甲氧基硅烷、3-环氧丙氧基丙基三乙氧基硅烷、3-丙烯酰氧基丙基三甲氧基硅烷、3-氯丙基三甲氧基硅烷;
所述交联促进剂选自环烷酸钴、二乙酸二丁锡、四正丁基锡、氢氧化三甲基锡、二月桂酸二丁锡;
上述粘合剂组合物在制备光学薄膜中的用途。
一种光学构件,在光学薄膜的至少一面设置了上述粘合剂组合物得到的粘合剂层。
本发明的光学构件用粘合剂中使用的所述丙烯酸类聚合物可以通过溶液聚合法、本体聚合法、乳液聚合法和悬浮聚合法等目前公知的聚合法来制造。所述丙烯酸类聚合物制备中,由于采用了比(甲基)丙烯酸烷基酯单体多含烷氧基的(甲基)丙烯酸烷氧基烷基酯单体,并结合具有基于凝胶渗透色谱法(GPC)的重均分子量(Mw)为210万~250万,较好是220-230万的特征,使得制备的丙烯酸类聚合物在具有良好耐久性(耐热、耐湿等)同时,具有满足需要的粘合性能。Mw如果不足210万,则耐热、耐湿性能不足,受热时粘合剂容易发生高温条件下的发泡,Mw如果大于250万,则粘合剂的贴合性、粘合力下降。
另外,所述丙烯酸类聚合物需要重均分子量(Mw)和数均分子量(Mn)的比值(Mw/Mn)为15~25,是分子量分布广、具有低拉伸弹性模量的聚合物。由于其拉伸弹性模量低,发挥良好的应力缓和性,有效地防止显示偏差。如果所述比值(Mw/Mn)过大,则低分子量聚合物增加,容易产生发泡;如果所述比值(Mw/Mn)过小,则应力缓和性下降,在粘贴面积大的情况下,容易发生漏光。
另外,本发明的组合物中不使用具有氨基的化合物组分,例如制备共聚物时具有氨基的单体、具有氨基的硅烷偶联剂和交联促进剂,因为具有氨基的化合物,在加热时容易产生具有刺激性气味的氨气,导致操作环境恶化,影响工人健康。故本发明的粘合剂具有更加环保的优点。
具体实施方式
以下通过具体实施方式对本发明的技术方案进行进一步的说明和描述。
制造例1
在具备搅拌机、回流冷凝器、温度计和氮气导入管的反应装置中加入分别示于表1的重量份的共聚性单体和乙酸乙酯,加入0.5份偶氮二异丁腈,将反应容器内的空气以氮气置换。接着,在氮气气氛下,搅拌的同时升温至60℃后,使其反应1.5小时后,继续加入0.2份偶氮二异丁腈,升温至80℃,使其反应1小时,接着再添加0.3份偶氮二异丁腈,使其反应3.5小时。反应结束后,用乙酸乙酯稀释,获得(甲基)丙烯酸类聚合物溶液。
制造例2-9
除用于聚合的原料不同外,其余制备过程与制造例1相同。
以上个制造例制成的(甲基)丙烯酸类聚合物的由GPC测定得到的重均分子量(Mw)以及聚合物的重均分子量除以数均分子量而得的值(Mw/Mn)的数值示于表1。
<GPC测定条件>
测定装置:HLC-8120GPC
GPC柱构成:以下的5连柱(1)TSK-GELHXL-H(保护柱),(2)TSK-GELG7000HXL,(3)TSK-GELGMHXL,(4)TSK-GELGMHL,(5)TSK-GELG2500HXL
样品浓度:用四氢呋喃稀释至1.0mg/cm3
流动相溶剂:四氢呋喃
流量:1.0cm3/分钟
柱温:40℃
表1:
实施例1
相对于100重量份由制造例1得到的(甲基)丙烯酸类聚合物溶液中的(甲基)丙烯酸类聚合物(固体成分),添加2重量份甲苯二异氰酸酯交联剂、0.7重量份3-环氧丙氧基丙基三甲氧基硅烷,以及0.1重量份二月桂酸二丁锡,获得粘合剂组合物的溶液。
通过将该粘合剂组合物的溶液涂布于经硅酮剥离处理的聚酯膜PET的表面并使其干燥,获得具有厚30μm的粘合剂层的粘合片。将该粘合片贴合在偏振片上并进行转印,制作带有粘合剂层的偏振板。
实施例2-5以及比较例1-5的制备方法同实施例1,不同的是分别使用制造例2-10的(甲基)丙烯酸类聚合物替代实施例1中的制造例1的(甲基)丙烯酸类聚合物。
60℃/48小时后的粘接力的测定
将上述样品裁断成25mm宽度,用2kg辊以一个往复将其压接在厚0.7mm的无碱玻璃上,从而进行贴附,在50℃、0.5MPa的高压釜中处理15分钟,接着,在60℃下放置48小时。对用抗张力试验机以剥离角度180°、剥离速度300mm/min剥脱该样品时的粘接力(N/25mm)进行测定。
耐久性测试
将上述样品切断成320mm×240mm,将其贴附在厚度0.7mm的无碱玻璃上,利用50℃、0.5MPa的高压锅处理15分钟,使上述样品与无碱玻璃完全密接。对于已实施该处理的样品,在90℃、100℃、60℃/90%RH的条件下实施500小时处理,然后以下述基准目视评价发泡、剥离、浮起的状态。
○:没有发泡、剥离。
△:确认有对辨识性不造成影响的发泡(最大直径不到100μm)。
×:确认有发泡(最大直径为100μm以上)、剥离。
防漏光性的评价方法
将2块光学构件用层压机辊粘合,使它们在无碱玻璃板的正反面相互呈正交尼科尔位,再在调整至50℃、5大气压的高压釜中保持20分钟,制成试验片。
将制成的试验片在85℃的条件下放置500小时,肉眼观察防漏光性,按照以下的基准进行评价。
◎:完全未发现漏光
○:几乎看不到漏光
△:发现少量漏光
×:发现明显的漏光。
性能测试结果见表2:
表2
由表2中所示的测试结果可知,使用了本发明的粘合剂的粘合片,在粘合性、耐久性和防漏光性上均良好的。而比较例的粘合片在虽然在某些性能上满足要求,但其在包括耐久性、粘合性和防漏光性的整体性能上存在缺点。
以上所述,仅为本发明的较佳实施例而已,故不能依此限定本发明实施的范围,即依本发明专利范围及说明书内容所作的等效变化与修饰,皆应仍属本发明涵盖的范围内。
Claims (4)
1.一种粘合剂组合物,其特征在于,由以下成分(A)、成分(B)、成分(C)和成分(D)组成:
(A)以下的单体成分(a1)、(a2)和(a3)共聚而成的重均分子量Mw为210万~250万,且共聚物的分子量分布(Mw/Mn)为15~25的丙烯酸类聚合物;
(a1)85~95重量%(甲基)丙烯酸烷氧基烷基酯,所述(甲基)丙烯酸烷氧基烷基酯选自(甲基)丙烯酸甲氧基乙酯和(甲基)丙烯酸乙氧基乙酯,
(a2)0.5-5重量%含羧基的单体,所述含羧基的单体选自(甲基)丙烯酸、马来酸、富马酸,
(a3)1~10重量%含羟基的单体,所述含羟基的单体选自2-羟基乙基(甲基)丙烯酸酯、4-羟基丁基(甲基)丙烯酸酯、2-羟基丙基(甲基)丙烯酸酯、2-羟基丁基(甲基)丙烯酸酯;
(B)相对于100重量份丙烯酸类聚合物0.5~5重量份异氰酸酯类交联剂;
(C)相对于100重量份丙烯酸类聚合物0.5~1.0重量份硅烷偶联剂;
(D)相对于100重量份丙烯酸类聚合物0.1~0.5重量份交联促进剂。
2.如权利要求1所述的一种粘合剂组合物,其特征在于:所述异氰酸酯类交联剂选自甲苯二异氰酸酯、氯苯二异氰酸酯、六亚甲基二异氰酸酯、四亚甲基二异氰酸酯、异佛尔酮二异氰酸酯、二苯基甲烷二异氰酸酯。
3.如权利要求1所述的一种粘合剂组合物,其特征在于:所述丙烯酸类聚合物(A)的重均分子量Mw为220-230万,优选为220万。
4.如权利要求1所述的一种粘合剂组合物,其特征在于:所述丙烯酸类聚合物(A)的分子量分布为20-25。
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