CN108384476A - 一种偏光片保护膜用压敏胶制备方法及其保护膜 - Google Patents

一种偏光片保护膜用压敏胶制备方法及其保护膜 Download PDF

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CN108384476A
CN108384476A CN201810164456.XA CN201810164456A CN108384476A CN 108384476 A CN108384476 A CN 108384476A CN 201810164456 A CN201810164456 A CN 201810164456A CN 108384476 A CN108384476 A CN 108384476A
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protective film
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安佳丽
周守发
牛正富
何晶晶
王辉
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KUNSHAN LEKAI JINFU PHOTOELECTRIC TECHNOLOGY CO LTD
Hefei Lucky Science and Technology Industry Co Ltd
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Hefei Lucky Science and Technology Industry Co Ltd
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Abstract

本发明公开了一种偏光片保护膜用压敏胶制备方法及其保护膜,所述压敏胶由下述重量含量的原料配制而成:10重量份~40重量份的软单体、5重量份~15重量份的硬单体、2重量份~6重量份的含氟丙烯酸酯单体、0.8重量份~3重量份的交联单体、0.8重量份~2重量份的乙烯基硅烷、0.5重量份~2重量份的抗静电剂、0.5重量份~1.5重量份的引发剂、80重量份~190重量份的溶剂。本发明压敏胶可直接涂布在聚酯薄膜表面,无需外加固化剂、抗静电剂,胶层电阻在1010Ω以下,具有抗静电性能。本发明的偏光片保护膜胶层贴合在偏光片表面时,经高温高湿试验500h后,保护膜与偏光片贴合紧密,无气泡鼓起、撕除保护膜无残胶、暗影等弊病。

Description

一种偏光片保护膜用压敏胶制备方法及其保护膜
技术领域
本发明涉及薄膜技术领域,尤其是一种偏光片保护膜用压敏胶。
背景技术
偏光片是液晶显示器的重要组成部分,为了防止偏光片在组装步骤或运送过程中造成表面的污染或损伤,需要在偏光片的表面贴合保护膜。将偏光片组装入液晶显示器后,将表面保护膜从偏光片表面剥离撕去,撕去表面保护膜的过程中,保护膜上的电阻值高,会产生静电电压,静电电压会破坏液晶显示器的液晶分子和控制液晶显示的驱动电路等组件,所以要求保护膜的胶层需要一定的电阻值,防止撕去保护膜时产生的静电电压对液晶显示器的伤害,压敏胶在与其他物体摩擦时会引起电荷分离而产生静电,溶剂型压敏胶在涂布时,静电产生的火花会引起爆炸,常用的解决方法是在压敏胶配方中加入导电物质,将胶层电阻降低到1010Ω以下,使压敏胶层具有防静电作用。
中国专利CN201410013570.4公开了一种保护膜用丙烯酸酯压敏胶,该压敏胶由聚合物A、聚合物B、化合物C混合而成,不含芳烃类溶剂,具有良好的初粘力、剥离力和持粘力,可涂布于PET基材上,用于加工过程及运输,库存的保护,但是该方法需要先分别合成聚合物A和聚合物B,工艺繁琐,且该压敏胶不具有防静电功能;中国专利CN201410053131.6公开了一种防静电保护膜用胶水,通过在丙烯酸酯压敏胶内添加防静电助剂(硫氰化钾、硫氰化锂)实现胶水防静电功能,但是硫氰化钾、硫氰化锂性能不稳定,高热时容易释放高毒性的氰化物和硫化物气体,对操作人员伤害大。
在偏光片的使用过程中,偏光片是在贴合表面保护膜的情况下,进行液晶显示板的显示能力、色域、杂质点等的光学评价的产品检验。因此,要求表面保护膜的胶层与偏光片贴合牢固,在胶层中不含气泡或杂质。
发明内容
本发明需要解决的技术问题针对现有技术工艺复杂、压敏胶性能不稳定等问题,提供一种偏光片保护膜用压敏胶制备方法,所述保护膜的胶层电阻在1010Ω以下。
本发明需要解决的另一个技术问题是提供一种涂布压敏胶的偏光片保护膜,所述保护膜的胶层贴合在偏光片表面时,经高温高湿试验500h后,保护膜与偏光片贴合紧密,无气泡鼓起,撕除保护膜后无残胶、暗影等弊病。
为解决上述技术问题,本发明采用技术方案如下:
一种偏光片保护膜用压敏胶制备方法,所述方法按如下步骤进行:
(1)将10重量份~40重量份的软单体、5重量份~15重量份的硬单体、2重量份~6重量份的含氟丙烯酸酯单体、2重量份~4重量份的引发剂混合均匀,得到预置液;
(2)将30重量份~80重量份溶剂加入到反应器中,升温至75℃~85℃,加入六分之一~四分之一的预置液到反应器中,保温反应15min~40min;将0.8重量份~3重量份的交联单体、0.8重量份~2重量份乙烯基硅烷、0.8重量份~2重量份抗静电剂加入到剩余预置液中混合均匀,得到中间液;
(3)中间液加入到反应器中,保温反应1.5h~3h,降温到50℃~60℃,再加入50重量份~150重量份的溶剂、0.5重量份~2重量份固化剂,得到偏光片保护膜用压敏胶。
上述偏光片保护膜用压敏胶制备方法,所述抗静电剂为聚噻吩与纳米银线的组合。
上述偏光片保护膜用压敏胶制备方法,所述的聚噻吩与纳米银线的重量比例为2:1~5:1。
上述偏光片保护膜用压敏胶制备方法,所述的软单体为甲基丙烯酸月桂酯、丙烯酸-2-乙基己酯中的一种或两种;所述的硬单体为甲基丙烯酸乙酯、苯乙烯中的一种或两种;所述的含氟丙烯酸酯单体为甲基丙烯酸三氟乙酯、丙烯酸三氟乙酯中的一种或两种;所述的引发剂为偶氮二异丁腈、过氧化二苯甲酰中的一种或两种。
上述偏光片保护膜用压敏胶制备方法,所述的溶剂为酯类溶剂与酮类溶剂的组合,酯类溶剂为乙酸乙酯、乙酸丁酯一种或两种组合,酮类溶剂为丙酮、丁酮的一种或两种组合,所述的酯类与酮类溶剂的重量比例为2:1~5:1。
上述偏光片保护膜用压敏胶制备方法,所述的交联单体为三羟甲基丙烷三丙烯酸酯、二丙二醇二丙烯酸酯中的一种或两种。
上述偏光片保护膜用压敏胶制备方法,所述的乙烯基硅烷为二甲基(二甲氨基)乙烯基硅烷、乙烯基三乙酰基硅烷、二乙基甲基乙烯基硅烷中的一种或任意组合。
上述偏光片保护膜用压敏胶制备方法,所述的固化剂为封闭型异氰酸酯固化剂,所述的封闭型异氰酸酯固化剂为异佛尔酮二异氰酸酯封闭型固化剂、六亚甲基二异氰酸酯封闭型固化剂中的一种或任意组合。
一种偏光片保护膜,包含在聚酯薄膜的一面涂布抗静电层,在聚酯薄膜的另一面涂布上述压敏胶,以及在压敏胶表面再贴合一层离型膜。
与现有技术相比,本发明具有如下优点:
1.本发明制备的压敏胶在制备过程中加入抗静电剂、固化剂,使用过程中无抗静电剂、固化剂加入工序,可直接上机涂布,可节省配胶工序,节约成本。
2.本发明抗静电剂为聚合物型抗静电剂与无机抗静电剂复配使用,聚合物型抗静电剂与丙烯酸酯压敏胶相容性较好,无机抗静电剂纳米银线导电性能优异,乙烯基硅烷可以改善纳米银线的表面性能,有助于纳米银线均匀的分散到压敏胶中,本发明的偏光片保护膜用压敏胶,胶层的电阻值在1010Ω以下,具有抗静电作用。
3.本发明丙烯酸酯压敏胶中引入有机硅,有利于改善纳米银线的表面性能,提高纳米银线与压敏胶之间的相容性,使纳米银线均匀的分布在压敏胶中,提高抗静电性。且有机硅有利于压敏胶在偏光片表面的铺展,使保护膜容易贴合在偏光片表面。
4.本发明丙烯酸酯压敏胶中引入含氟丙烯酸酯单体,氟原子可使聚合物主链受到屏蔽,使聚合物具有优异的化学稳定性,且有机氟化合物分子间凝聚力低、表面自由能低,赋予丙烯酸酯压敏胶优异的耐水性。
5.本发明的偏光片保护膜剥离力较低,为2gf/25mm~10gf/25mm,胶层贴合在偏光片表面时,经高温高湿试验500h后,保护膜与偏光片贴合紧密,无气泡鼓起,撕除保护膜无残胶、暗影等弊病,满足偏光片保护膜的使用要求。
具体实施例方式
本发明的聚酯薄膜为38μm的光学级聚酯薄膜,所述的在聚酯薄膜的一面涂布抗静电层的制备方法与CN201511015475.9相同,所述的抗静电层是将成膜树脂、导电型聚噻吩分散液、固化剂、表面活性剂组成的涂布液,涂布于聚酯薄膜的表面固化后形成。
本发明胶层的厚度为10μm~25μm,优选厚度为12μm~20μm。
本发明封闭型异氰酸酯固化剂可以选自下述市售物质但并不限于此:如日本旭化成化学的MF-K60X,拜耳的BL3370MPA,德固萨的B1358等。
以下结合具体实施方式对本发明作进一步的详细说明,但本发明的实施方式并不限于这些实施例。
实施例1
将10g甲基丙烯酸月桂酯、10g甲基丙烯酸乙酯、5g苯乙烯、4g甲基丙烯酸三氟乙酯、0.5g偶氮二异丁腈混合均匀,得到预制液。
将10g乙酸乙酯、15g乙酸丁酯、5g丙酮加入到反应器中,升温至75℃,加入7.38g预制液到反应器中,保温反应25min;将0.8g三羟甲基丙烷三丙烯酸酯、0.8g二甲基(二甲氨基)乙烯基硅烷、0.53g聚噻吩、0.27g纳米银线加入到剩余预制液中,得到中间液。
加入中间液到反应器中,保温反应1.5h,降温到50℃,再加入50g乙酸乙酯、75g乙酸丁酯、10g丙酮、15g丁酮、1gMF-K60X(日本旭化成化学),得到偏光片保护膜用压敏胶。
将该压敏胶涂布于厚度为38μm光学级的聚酯薄膜的非抗静电层面上,将聚酯薄膜放入120℃的烘箱中烘2min,取出聚酯薄膜,在胶层表面覆上一层离型膜,得到胶层厚度为15μm的偏光片保护膜。评估结果列于表1中。
实施例2
将20g甲基丙烯酸月桂酯、20g丙烯酸-2-乙基己酯、10g甲基丙烯酸乙酯、5g苯乙烯、2g丙烯酸三氟乙酯、1g过氧化二苯甲酰混合均匀,得到预制液。
将64g乙酸乙酯、10g丙酮、6g丁酮加入到反应器中,升温至85℃,加入9.67g预制液到反应器中,保温反应15min;将2g三羟甲基丙烷三丙烯酸酯、1g二丙二醇二丙烯酸酯、0.7g二甲基(二甲氨基)乙烯基硅烷、0.7g乙烯基三乙酰基硅烷、0.6g二乙基甲基乙烯基硅烷、1.67g聚噻吩、0.33g纳米银线加入到剩余预制液中,得到中间液。
加入中间液到反应器中,保温反应3h,降温到60℃,再加入80g乙酸乙酯、20g丙酮、20g丁酮、4g BL3370MPA(拜耳),得到偏光片保护膜用压敏胶。
将该压敏胶涂布于厚度为38μm光学级的聚酯薄膜的非抗静电层面上,将聚酯薄膜放入120℃的烘箱中烘2min,取出聚酯薄膜,在胶层表面覆上一层离型膜,得到胶层厚度为12μm的偏光片保护膜。评估结果列于表1中。
实施例3
将30g丙烯酸-2-乙基己酯、5g甲基丙烯酸乙酯、5g苯乙烯、3g甲基丙烯酸三氟乙酯、3g丙烯酸三氟乙酯、0.3g偶氮二异丁腈、0.3g过氧化二苯甲酰混合均匀,得到预制液。
将45g乙酸丁酯、15g丁酮加入到反应器中,升温至80℃,加入9.32g预制液到反应器中,保温反应25min;将1.5g二丙二醇二丙烯酸酯、1g二甲基(二甲氨基)乙烯基硅烷、0.5g二乙基甲基乙烯基硅烷、1.2g聚噻吩、0.3g纳米银线加入到剩余预制液中,得到中间液。
加入中间液到反应器中,保温反应2h,降温到55℃,再加入20g乙酸乙酯、40g乙酸丁酯、20g丁酮、1gMF-K60X(旭化成化学)、1gBL3370MPA(拜耳)、1gB1358(德固萨),得到偏光片保护膜用压敏胶。
将该压敏胶涂布于厚度为38μm光学级的聚酯薄膜的非抗静电层面上,将聚酯薄膜放入120℃的烘箱中烘2min,取出聚酯薄膜,在胶层表面覆上一层离型膜,得到胶层厚度为20μm的偏光片保护膜。评估结果列于表1中。
实施例4
将10g甲基丙烯酸月桂酯、10g丙烯酸-2-乙基己酯、8g苯乙烯、4g丙烯酸三氟乙酯、0.8g偶氮二异丁腈混合均匀,得到预制液。
将20g乙酸乙酯、12g乙酸丁酯、4g丙酮、4g丁酮加入到反应器中,升温至78℃,加入8.2g预制液到反应器中,保温反应35min;将1g三羟甲基丙烷三丙烯酸酯、1.5g二丙二醇二丙烯酸酯、0.8g二乙基甲基乙烯基硅烷、0.9g聚噻吩、0.3g纳米银线加入到剩余预制液中,得到中间液。
加入中间液到反应器中,保温反应1.5h,降温到53℃,再加入80g乙酸乙酯、10g丙酮、10g丁酮、1.5gBL3370MPA(拜耳)、1gB1358(德固萨),得到偏光片保护膜用压敏胶。
将该压敏胶涂布于厚度为38μm光学级的聚酯薄膜的非抗静电层面上,将聚酯薄膜放入120℃的烘箱中烘2min,取出聚酯薄膜,在胶层表面覆上一层离型膜,得到胶层厚度为14μm的偏光片保护膜。评估结果列于表1中。
实施例5
将10g甲基丙烯酸月桂酯、15g丙烯酸-2-乙基己酯、6g甲基丙烯酸乙酯、6g苯乙烯、5g丙烯酸三氟乙酯、0.7g过氧化二苯甲酰混合均匀,得到预制液。
将37.5g乙酸丁酯、12.5g丙酮加入到反应器中,升温至82℃,加入7.12g预制液到反应器中,保温反应20min;将1.8g三羟甲基丙烷三丙烯酸酯、0.6g乙烯基三乙酰基硅烷、0.7g二乙基甲基乙烯基硅烷、1.1g聚噻吩、0.4g纳米银线加入到剩余预制液中,得到中间液。
加入中间液到反应器中,保温反应2.5h,降温到60℃,再加入25g乙酸乙酯、15g乙酸丁酯、5g丙酮、5g丁酮、1.5gBL3370MPA(拜耳),得到偏光片保护膜用压敏胶。
将该压敏胶涂布于厚度为38μm光学级的聚酯薄膜的非抗静电层面上,将聚酯薄膜放入120℃的烘箱中烘2min,取出聚酯薄膜,在胶层表面覆上一层离型膜,得到胶层厚度为18μm的偏光片保护膜。评估结果列于表1中。
对比例1
将30g丙烯酸乙酯、10g甲基丙烯酸甲酯、1g偶氮二异丁腈混合均匀,得到预制液。
将40g乙酸乙酯加入到反应器中,升温至80℃,加入10g预制液到反应器中,保温反应30min;将1g三羟甲基丙烷三丙烯酸酯、1.5g二丙二醇二丙烯酸酯、1g聚噻吩加入到剩余预制液中,得到中间液。
加入中间液到反应器中,保温反应1h,降温到50℃,再加入100g乙酸乙酯,2gBL3370MPA(拜耳)得到偏光片保护膜用压敏胶。
将该压敏胶涂布于厚度为38μm光学级的聚酯薄膜的非抗静电层面上,将聚酯薄膜放入120℃的烘箱中烘2min,取出聚酯薄膜,在胶层表面覆上一层离型膜,得到胶层厚度为15μm的偏光片保护膜。评估结果列于表1中。
对比例2
将40g丙烯酸丁酯、12g甲基丙烯酸甲酯、0.8g过氧化二苯甲酰混合均匀,得到预制液。
将50g甲苯加入到反应器中,升温至75℃,加入8g预制液到反应器中,保温反应30min;将1.5g二丙二醇二丙烯酸酯、1g炭粉加入到剩余预制液中,得到中间液。
加入中间液到反应器中,保温反应1h,降温到50℃,再加入100g乙酸乙酯,2gB1358(德固萨)得到偏光片保护膜用压敏胶。
将该压敏胶涂布于厚度为38μm光学级的聚酯薄膜的非抗静电层面上,将聚酯薄膜放入120℃的烘箱中烘2min,取出聚酯薄膜,在胶层表面覆上一层离型膜,得到胶层厚度为12μm的偏光片保护膜。评估结果列于表1中。
表1性能数据表
表中各项性能的测试方法如下:
(1)透光率、雾度测试
参照标准GB/T2410-2008,利用雾度计(型号:“U3000”),撕去离型膜,测量透光率(T)和雾度(H)。
(2)剥离力测试
将保护膜裁成300*25mm尺寸,撕去离型膜,将保护膜贴合在偏光片表面,使用电子万能试验机(型号:AGS-X),在角度180○、拉伸速度300mm/min的条件下进行剥离测试。
(3)胶层电阻测试
将保护膜裁成12*12mm尺寸,撕去离型膜,在高阻计(型号:SME-8310)上测试胶面电阻。
(4)高温高湿试验
将保护膜裁成150*25mm尺寸,撕去离型膜,将保护膜胶层贴合在偏光片表面,放入可程式恒温恒湿试验箱,经80℃、90%湿度500h后,观察保护膜在偏光片表面有无折皱、脱离、气泡产生,若无,则判断为合格,若有,则判断为不合格。

Claims (8)

1.一种偏光片保护膜用压敏胶制备方法,其特征在于,制备按如下步骤进行:
(1)将10重量份~40重量份的软单体、5重量份~15重量份的硬单体、2重量份~6重量份的含氟丙烯酸酯单体、1重量份~4重量份的引发剂混合均匀,得到预置液;
(2)将30重量份~80重量份溶剂加入到反应器中,升温至75℃~85℃,加入1/6-1/4的预置液到反应器中,保温反应15min~40min;将0.8重量份~3重量份的交联单体、0.8重量份~2重量份乙烯基硅烷、0.8重量份~2重量份抗静电剂加入到剩余预置液中混合均匀,得到中间液;
(3)加入中间液到反应器中,保温反应1.5h~3h,降温到50℃~60℃,再加入50重量份~150重量份的溶剂、固化剂,得到偏光片保护膜用压敏胶;
所述抗静电剂为聚噻吩与纳米银线的组合。
2.根据权利要求1所述的偏光片保护膜用压敏胶制备方法,其特征在于,所述聚噻吩与纳米银线的重量比例为2:1~5:1。
3.根据权利要求1所述的偏光片保护膜用压敏胶制备方法,其特征在于,所述软单体为甲基丙烯酸月桂酯或丙烯酸-2-乙基己酯中的一种或两种;所述硬单体为甲基丙烯酸乙酯或苯乙烯中的一种或两种;所述的含氟丙烯酸酯单体为甲基丙烯酸三氟乙酯或丙烯酸三氟乙酯中的一种或两种;所述的引发剂为偶氮二异丁腈或过氧化二苯甲酰中的一种或两种。
4.根据权利要求1所述的偏光片保护膜用压敏胶制备方法,其特征在于,所述的溶剂为酯类溶剂与酮类溶剂的组合,酯类溶剂为乙酸乙酯或乙酸丁酯一种或两种组合,酮类溶剂为丙酮或丁酮的一种或两种组合,所述的酯类与酮类溶剂的重量比例为2:1~5:1。
5.根据权利要求1所述的偏光片保护膜用压敏胶制备方法,其特征在于,所述的交联单体为三羟甲基丙烷三丙烯酸酯或二丙二醇二丙烯酸酯中的一种或两种。
6.根据权利要求1所述的偏光片保护膜用压敏胶制备方法,其特征在于,所述的乙烯基硅烷为二甲基(二甲氨基)乙烯基硅烷、乙烯基三乙酰基硅烷或二乙基甲基乙烯基硅烷中的一种或任意组合。
7.根据权利要求1所述的偏光片保护膜用压敏胶制备方法,其特征在于,所述的固化剂为封闭型异氰酸酯固化剂,所述的封闭型异氰酸酯固化剂为异佛尔酮二异氰酸酯封闭型固化剂或六亚甲基二异氰酸酯封闭型固化剂中的一种或任意组合。
8.一种偏光片保护膜,其特征在于,包含在聚酯薄膜的一面涂布抗静电层,在聚酯薄膜的另一面涂布如权利要求1-7任一项所述方法制备的偏光片保护膜用压敏胶,以及在压敏胶表面再贴合一层离型膜。
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