CN113549411A - 一种防静电保护膜用的uv固化热熔压敏胶 - Google Patents

一种防静电保护膜用的uv固化热熔压敏胶 Download PDF

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CN113549411A
CN113549411A CN202110903192.7A CN202110903192A CN113549411A CN 113549411 A CN113549411 A CN 113549411A CN 202110903192 A CN202110903192 A CN 202110903192A CN 113549411 A CN113549411 A CN 113549411A
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sensitive adhesive
melt pressure
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卢新亚
戴莹琨
董德文
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Shenzhen Lihe Bohui Photosensitive Material Co ltd
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Abstract

本发明提供了一种防静电保护膜用的UV固化热熔压敏胶，旨在提供一种储存稳定性好、透明性优异、再剥离性优异、剥离带电少，能有效地降低材料成本和提高生产效率的压敏胶；其技术方案包括侧链含有二苯甲酮基团或甲苯酮衍生化合物以及环氧乙烷链锻的丙烯酸系共聚物，以及离子化合物；属于高分子新材料技术领域。

Description

一种防静电保护膜用的UV固化热熔压敏胶
技术领域
本发明属于高分子新材料技术领域，具体涉及一种防静电保护膜用的UV固化热熔压敏胶；具体涉及一种防静电保护膜用的UV固化热熔压敏胶。
背景技术
电子行业生产过程经常遇到静电问题，静电会把细小的灰尘吸引到电子部件上，导致电子器件暂时或永久性的损坏。为了解决防止静电问题，所有用于电子产品的保护膜都要求有抗静电的性能。例如，在各种显示器或偏光板等光学部件通常使用保护胶膜来保护其表面功能性，这些表面保护膜在液晶显示器或偏光板的组装完成后，需要将其剥离除去。但是表面保护胶膜被剥离时会产生静电、把细小的灰尘吸引到电子部件的问题。而且由于在剥离表面保护胶薄膜时产生的剥离带电，有时会发生液晶或电子电路被破坏的问题。
韩国专利(2009-0101761)公开了一种包括有机粘合剂和离子盐的抗静电压敏胶。但是该压敏胶需要使用大量的离子盐达到降低压敏胶的表面电阻效果，而当压敏胶含有大量的离子盐时，不仅会导致离子盐在配方溶液中产生沉淀，而且会严重损害压敏胶本身的物理性能。
日本专利(2005-031282)公开了一种含金属盐和亲水性单体的压敏胶，其中亲水单体通过吸收空气中的水分来降低电荷水平。但是该类压敏胶的防静电性能显然受空气中温度的影响很大，在实际应用中所受的限制很大。
CN1049461173B公开了一种压敏胶组合物，所述组合物为含聚亚烷基二醇单(甲基)丙烯酸酯单体的共聚物，离子盐，异氰酸酯化合物、交联抑制剂、交联催化剂、抗静电剂、和聚醚改性的硅氧烷的组合物。但其交联过程缓慢，需要在室温和干燥条件下熟化七天，不利生产效率和质量检测。而且其涂布配方含有大量有害溶剂，不符合现代生产的环保节能要求。
发明内容
本发明的目的在于提供一种防静电保护膜用的UV固化热熔压敏胶，该UV固化热熔压敏胶具有储存稳定性好、透明性优异、再剥离性优异、剥离带电少，能有效地降低材料成本和提高生产效率等优点。
为达到上述目的，本发明的防静电保护膜用的UV固化热熔压敏胶组成为侧链含有二苯甲酮基团和环氧乙烷链锻的丙烯酸系共聚物和离子化合物混合物。
作为进一步优选，所述的丙烯酸系共聚物(A)总量100重量份，侧链含有二苯甲酮基团或甲苯酮衍生化合物的单体是0.1-5.0重量份，含有环氧乙烷链锻的单体是1.0-40.0重量份。
上述侧链含有二苯甲酮基团或甲苯酮衍生化合物的单体包括但不限于4-甲基丙烯酸二苯甲酮酯，4-丙烯酸二苯甲酮酯，4-[2-(甲基丙烯酰氧基)乙氧基]二苯甲酮(4-[2-(methacryloyloxy)ethoxy]benzophenone),4-[2-(丙烯酰氧基)乙氧基]二苯甲酮(4-[2-(acryloyloxy)ethoxy]benzophenone)，和其混合物。
上述侧链含有环氧乙烷链锻的单体包括但不限于聚环氧乙烷单(甲基)丙烯酸酯，甲氧基聚环氧乙烷(甲基)丙烯酸酯、乙氧基聚环氧乙烷(甲基)丙烯酸酯，聚环氧丙烷单(甲基)丙烯酸酯，甲氧基聚环氧丙烷(甲基)丙烯酸酯、乙氧基聚环氧丙烷(甲基)丙烯酸酯，聚(环氧乙烷-CO-二氧化碳)(甲基)丙烯酸酯或它们的混合物。
优选的，上述的防静电保护膜用的UV固化热熔压敏胶，所述的侧链含有二苯甲酮基团或甲苯酮衍生化合物、环氧乙烷链锻的丙烯酸系共聚物制备的：
1)称取100份共聚单体混合物，0.5-2份二苯甲酮基团或甲苯酮衍生化合物的单体，60-70份乙酸乙酯和0.5份偶氮二异丁氰；
2)向配有搅拌机、回流冷却器、温度计以及氮气导入管的圆底烧瓶导入氮气分钟，然后分别加入步骤1)中的50wt％共聚单体混合物，50wt％二苯甲酮基团或甲苯酮衍生化合物的单体，50wt％乙酸乙酯、50wt％偶氮二异丁氰；
3)在氮气气氛下搅拌下升温至回流温度75-82℃，用约0.5-1.5小时的时间滴加剩余各个共聚单体，剩余的乙酸乙酯、偶氮二异丁氰混合后的溶液，然后回流温度下继续反应6小时，得到紫外光固化(甲基)丙烯酸类共聚物。
作为进一步优选，侧链含有二苯甲酮基团或甲苯酮衍生化合物、环氧乙烷链锻的丙烯酸的制备方法为：
1)称取53-64份丙烯酸异辛酯，10-20份丙烯酸羟乙酯，3份丙烯酸羟乙酯，3份4-羟基丁基丙烯酸酯，0.5-2份4-甲基丙烯酸二苯甲酮酯，10-40份丙烯酸系共聚物；60-70份乙酸乙酯和0.5份偶氮二异丁氰，苯甲醇0-20份，甲氧基聚乙二醇类丙烯酸酯0-20份；
2)向配有搅拌机、回流冷却器、温度计以及氮气导入管的圆底烧瓶导入氮气分钟，然后分别加入步骤1)中的50wt％共聚单体，50wt％乙酸乙酯、50wt％偶氮二异丁氰；
3)在氮气气氛下搅拌下升温至回流温度75-82℃，用约0.5-1.5小时的时间滴加剩余各个共聚单体，剩余的乙酸乙酯、偶氮二异丁氰混合后的溶液，然后回流温度下继续反应6小时，得到紫外光固化(甲基)丙烯酸类共聚物。
作为进一步优选，上述UV固化热熔压敏胶中丙烯酸系共聚物总量100重量份，离子化合物是0.1-20.0重量份，更优选0.5-5.0重量份。
上述离子化合物为碱金属的无机盐，碱金属的有机盐，季铵盐和吡啶嗡盐。碱金属的无机盐的例子包括但不限于氯化钠、氯化钾、氯化锂、高氯酸锂、高氯酸钾、硝酸钾、硝酸钠、碳酸钠、硫氰酸钠、LiBr、LiI、LiBF4、LiPF6、LiSCN等。根据导电性和安全性，优选氯化钠、氯化钾、高氯酸锂等作为防静电添加剂。碱金属的有机盐的例子包括但不限于醋酸钠、藻酸钠、木质素磺酸钠、甲苯磺酸钠、LiCF3SO3,Li(CF3SO2)2N,Li(C2F5SO2)2N,Li(CF3SO2)3C等，优选Li(CF3SO2)2N,Li(C2F5SO2)2N，等含氟酰亚胺的锂盐。吡啶嗡盐的例子包括但不限1-辛基吡啶嗡六氟磷酸盐、1-壬基吡啶嗡六氟磷酸盐、2-甲基-1-十二烷基吡啶嗡六氟磷酸盐、1-辛基吡啶嗡十二烷基苯磺酸盐、十二烷基吡啶嗡十二烷基苯磺酸盐等。
作为进一步优选，上述防静电保护膜用的UV固化热熔压敏胶中丙烯酸系共聚物的重均分子量为1万～50万，更优选10万～30万。
进一步地，上述防静电保护膜用的UV固化热熔压敏胶可与一种或多种添加剂混合，例如增粘树脂、抗氧化剂、光稳定剂、粘接促进剂。
进一步地，上述防静电保护膜用的UV固化热熔压敏胶可混入交联化合物来进一步有提高压敏胶产品的性能。合适的交联化合物包括但不制于多官能团的(甲基)丙烯酸酯交联剂和其它的能够交联丙烯酸聚合物的双官能或多官能化合物。
进一步地，上述防静电保护膜用的UV固化热熔压敏胶为不含有机溶剂的热熔胶或液态胶。进一步地，本申请所述的方法特别有利于生产UV固化热熔压敏胶，所有的添加剂可以在聚合反应的末期加入到共聚物溶液中。在溶剂被去除之后，混合物形成无溶剂UV固化热熔压敏胶。
上述的一种防静电保护膜用的UV固化热熔压敏胶可在200至500nm范围内的紫外光照射下，于空气中或氮气中交联。
上述UV固化热熔压敏胶可用于制备一种光学部件用表面防静电保护膜，其结构为UV固化热熔压敏胶在塑料薄膜衬底上UV交联形成的均匀平整的胶膜。
进一步地，上述防静电保护膜的胶层相反的面上进行抗静电和防污染处理来进一步有提高产品的性能
上述防静电保护膜适用保护偏光板用表面。
与现有技术相比，本发明提供的压敏胶透明度优良，可以在贴合保护状态下进行光学膜的外观检查，低剥离力，而且贴附后剥离力变化小，防静电效果优良，性能持久稳定。
本发明提供的防静电保护膜用的UV固化热熔压敏胶所制备的防静电保护膜适用于液晶面板、等离子体显示器、偏光板、CRT,OLED等光学部件表面保护。而且本压敏胶配方的储存稳定性好再剥离性优异、剥离带电少，能有效地降低材料成本和提高生产效率。
本发明提供的压敏胶不含有机溶，环境友好。
具体实施方式
下面结合具体实施例对本发明的权利要求做进一步的详细说明。
实施例1-8
侧链含有二苯甲酮基团或甲苯酮衍生化合物、环氧乙烷链锻的丙烯酸系共聚物的制备：
向配有搅拌机、回流冷却器、温度计以及氮气导入管的2升4颈圆底烧瓶导入氮气5分钟，然后分别加入表1所示各个共聚单体总重量份的50％，乙酸乙酯(作为溶剂)的总重量份的50％，自由基热引发剂偶氮二异丁氰(VAZO64)总重量份的50％。接下来，在氮气气氛下搅拌下升温至回流温度(约80℃)。用约1小时的时间滴加剩余各个共聚单体，剩余的乙酸乙酯和偶氮二异丁氰混合后的溶液，然后回流温度下继续反应6小时，从而得到了具有表1中所示的分子量的紫外光固化(甲基)丙烯酸类共聚物。
表1实施例1-8中各个组分及其重量份
Figure BDA0003200541860000041
Figure BDA0003200541860000051
实施例9-16防静电保护膜样品制备：
表1所列的丙烯酸类聚合物溶液(固含量为60％)100重量份与离子化合物1-20重量份混合均匀，然后在减压条件下加热至120℃以脱挥溶剂。脱掉后的压敏胶样品固含量至少大于99.5％。采用热熔涂布的方式将压敏胶均匀地涂在25微米厚的聚酯薄膜上，其涂布量控制在20克/平方米。然后在台式紫外线固化机(中压汞柱，H灯，120瓦/厘米)进行UV固化，所有样品UVC固化剂量控制在40mJ/cm2。得到实施例9-16防静电保护膜样品。
说明：
实施例1-8制备的侧链含有二苯甲酮基团或甲苯酮衍生化合物、环氧乙烷链锻的丙烯酸系共聚物依次记为丙烯酸系共聚物1-8。
实施例9-16防静电保护膜组分及其重量份
Figure BDA0003200541860000052
Figure BDA0003200541860000061
实施例9-16防静电保护膜样品按照以下所述的测试方法，评价其剥离力、表面电阻值、再剥离性、透明性和胶配方的储藏稳定性。
(1)剥离力
防静电保护膜样品在玻璃板上剥离试力按GGB/T2792-2014测试方法，玻璃板上贴合24小之后，使用桌上型拉力试验机来进行测试。
(2)表面电阻值
静电保护膜样品表面电阻按GB/T1410-2006测试方法，用RT-1000表面电阻测试仪测定压敏胶层表面的表面电阻值(Q/口)。
(3)再剥离性
防静电保护膜样品贴合在玻璃板上，在60℃和95％相对湿度的条件下放置24小时，再在23℃和50％相对湿度的条件下放置1小时，最后从玻璃板剥离，目测保护膜样品在玻璃板的胶残留性。具体按照以下4级评价剥离后的状态。
(4)胶带透明性
防静电保护膜样品贴合在玻璃板上，在60℃和95％相对湿度的条件下放置24小时，再在23℃和50％相对湿度的条件下放置1小时，目测评价保护膜样品在玻璃板上透明性。
(4)胶配方的储藏稳定性
将压敏胶样品装入在密闭容器中，在50℃的条件下放置1周后，测其粘度上升程度。
实施例9 实施例10 实施例11 实施例12 实施例13 实施例14 实施例15 实施例16
丙烯酸类聚合物溶液 实施例1 实施例2 实施例3 实施例4 实施例5 实施例6 实施例7 实施例8
剥离力(g/25mm) 30 27 23 20 35 20 35 40
表面电阻值(Q/口) 7.1x10<sup>8</sup> 5.7x10<sup>8</sup> 4.5x10<sup>8</sup> 4.1x10<sup>8</sup> 7.3x10<sup>8</sup> 7.0x10<sup>8</sup> 7.5x10<sup>8</sup> 9.1x10<sup>8</sup>
再剥离性 完全无残胶 完全无残胶 完全无残胶 完全无残胶 完全无残胶 完全无残胶 完全无残胶 完全无残胶
胶带透明性 完全透明 完全透明 完全透明 完全透明 完全透明 完全透明 完全透明 轻微雾状
胶配方的储藏稳定性 粘度设变化 粘度设变化 粘度设变化 粘度设变化 粘度设变化 粘度设变化 粘度设变化 粘度设变化
实施例17-18
制备热固化(甲基)丙烯酸酯溶剂压敏胶：
向配有搅拌机、回流冷却器、温度计以及氮气导入管的2升4颈圆底烧瓶导入氮气5分钟，然后分别加入表3所示各个共聚单体的总重量份的50％，适量乙酸乙酯和偶氮二异丁氰(VAZ064)分别作为溶剂和自由基热引发剂。接下来，在氮气气氛下搅拌下升温至回流温度(约80℃)。用约1小时的时间滴加剩余50％各个共聚单体、乙酸乙酯、偶氮二异丁氰混合后的溶液，然后回流温度下继续反应6小时，从而得到了具有表1中所示的分子量的热固化(甲基)丙烯酸类共聚物。
上述热固化丙烯酸类聚合物100重量份，分别添加8.0重量份的甲苯二异氰酸酯交联剂(CORONATEL，日本聚氨酯公司)，3.0重量份高氯酸锂和适量甲苯，并进行混合均匀，从而得到了热固化压敏胶溶液(50％固含量)。
上述所得到的热固化压敏胶涂在25微米厚的聚酯离型膜上，经在100℃干燥去除溶剂后，形成厚度为20微米的胶层。形成保护膜样品需要在室温下经过2天，以确保热固化完全。
对比实施例17和18进行剥离力、表面电阻值、再剥离性、透明性和胶配方的储藏稳定性。其中剥离力、表面电阻值、再剥离性、透明性类似实施例9和10，但在加入热固化交联剂24小时后，配方粘度增加-倍以上，失去良好的涂布性能。在同等条件下，实施例9和10配方粘度没有任何变化，仍保持了良好的热熔涂布性能。
另外，对比实施例17和18交联过程缓慢，需要在室温和干燥条件下熟化七天，不利生产效率和质量检测。而且其涂布配方含有大量有害溶剂，不符合现代生产的环保节能要求。
表3热固化(甲基)丙烯酸酯溶剂压敏胶各个参数
Figure BDA0003200541860000081
以上所述仅为本发明的较典型实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所做的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (10)

1.一种防静电保护膜用的UV固化热熔压敏胶，其特征在于，包括侧链含有二苯甲酮基团或甲苯酮衍生化合物以及环氧乙烷链锻的丙烯酸系共聚物，以及离子化合物。
2.根据权利要求1所述的防静电保护膜用的UV固化热熔压敏胶，其特征在于，相对丙烯酸系共聚物总量100重量份，侧链含有二苯甲酮基团或甲苯酮衍生化合物的单体是0.1-5.0重量份，含有环氧乙烷链锻的单体是1.0-40.0重量份。
3.根据权利要求1所述的防静电保护膜用的UV固化热熔压敏胶，其特征在于，当丙烯酸系共聚物(A)总量100重量份，离子化合物是0.1-20.0重量份。
4.根据权利要求1所述的防静电保护膜用的UV固化热熔压敏胶，其特征在于，所述的侧链含有二苯甲酮基团或甲苯酮衍生化合物、环氧乙烷链锻的丙烯酸系共聚物制备的：
1)称取100份共聚单体混合物，0.5-2份二苯甲酮基团或甲苯酮衍生化合物的单体，50-100份有机溶剂和0.2-1.0份自由基热引发剂；
2)向配有搅拌机、回流冷却器、温度计以及氮气导入管的圆底烧瓶导入氮气分钟，然后分别加入步骤1)中的50wt％共聚单体混合物，50wt％二苯甲酮基团或甲苯酮衍生化合物的单体，50wt％乙酸乙酯、50wt％偶氮二异丁氰；
3)在氮气气氛下搅拌下升温至回流温度75-82℃，用约0.5-1.5小时的时间滴加剩余各个共聚单体，剩余的乙酸乙酯、偶氮二异丁氰混合后的溶液，然后回流温度下继续反应6小时，得到紫外光固化(甲基)丙烯酸类共聚物。
5.根据权利要求1所述的一种防静电保护膜用的UV固化热熔压敏胶，其特征在于，含有环氧乙烷链锻的单体为聚环氧乙烷单(甲基)丙烯酸酯，甲氧基聚环氧乙烷(甲基)丙烯酸酯、乙氧基聚环氧乙烷(甲基)丙烯酸酯，聚环氧丙烷单(甲基)丙烯酸酯，甲氧基聚环氧丙烷(甲基)丙烯酸酯、乙氧基聚环氧丙烷(甲基)丙烯酸酯，聚(环氧乙烷-CO-二氧化碳)(甲基)丙烯酸酯或它们的混合物。
6.根据权利要求1所述的一种防静电保护膜用的UV固化热熔压敏胶，其特征在于，所述的离子化合物为碱金属的无机盐、碱金属的有机盐、季铵盐和吡啶嗡盐的其中之一。
7.根据权利要求1所述的一种防静电保护膜用的UV固化热熔压敏胶，其特征在于，丙烯酸系共聚物的重均分子量为1万～50万。
8.根据权利要求1所述的一种防静电保护膜用的UV固化热熔压敏胶，其特征在于，所述的防静电保护膜用的UV固化热熔压敏胶还添加有抗氧化剂、光稳定剂、交联化合物、粘接促进剂的其中之一或者任何混合。
9.根据权利要求1所述的一种防静电保护膜用的UV固化热熔压敏胶，其特征在于，所述的防静电保护膜用的UV固化热熔压敏胶在200至500nm范围内的紫外光照射下，于空气中或氮气中交联。
10.一种光学部件用表面保护膜，其特征在于，是采用权利要求1所述的防静电保护膜用的UV固化热熔压敏胶在薄膜衬底上，在200至500nm范围内的紫外光照射下，于空气中或氮气中交联形成的胶膜。
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