CN111763487A - 一种用于曲面屏贴合粘合剂的制备方法 - Google Patents

一种用于曲面屏贴合粘合剂的制备方法 Download PDF

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CN111763487A
CN111763487A CN202010609732.6A CN202010609732A CN111763487A CN 111763487 A CN111763487 A CN 111763487A CN 202010609732 A CN202010609732 A CN 202010609732A CN 111763487 A CN111763487 A CN 111763487A
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王小莉
王平
梁明月
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Nanjing Huixin Photoelectric Material Co ltd
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Abstract

一种用于曲面屏贴合的粘合剂的制备方法，包括丙烯酸酯聚合物制成的丙烯酸酯压敏胶，PET离型膜基材和PET离型膜重膜，所述丙烯酸酯聚合物包括丙烯酸，丙烯酸甲酯，甲基丙烯酸甲酯，α‑甲基丙烯酸，苯乙烯，醋酸乙酯，N‑羟甲基丙烯酰胺，甲基丙烯酸‑2‑羟基乙酯，丙烯酸羟乙酯，丙烯酸羟丁酯，丙烯酸异辛酯和偶氮二异丁氰，所述丙烯酸酯压敏胶涂布在所述PET离型膜轻膜上经烘箱烘干后在其另一面附上所述PET离型膜重膜，其具有较好的初粘力，附着性好，持粘力高等优点，有较好的粘结和再剥离性能，并对耐热性有很好的改善，适用于多种偏光片。

Description

一种用于曲面屏贴合粘合剂的制备方法
技术领域
本发明属于粘合剂技术领域，具体涉及一种用于曲面屏贴合粘合剂的制备方法。
背景技术
曲面屏幕以非刚性玻璃为基底，弹性更好，不易破碎，尤其是被触碰率较高的手机屏幕。曲面屏幕整体的弯曲有利于握持，与手心弧度贴合更好，并且屏幕变得更薄，重量轻且功耗低。最重要的是曲面屏幕增大了可视角度，可以带来更好的感官体验。在以后，曲面屏除了在手机，电视机外，曲面屏更会应用在穿戴式的智能设备上，比如智能手表，头戴式智能眼镜等。
目前的曲面屏胶水具有无色透明、光透过率在90%以上、胶结强度良好，可在室温或中温下固化，固化收缩小等特点。曲面胶可以贴合触控屏与显示屏，消除触控屏与显示屏之间的空气层，从而提高显示效果，并隔绝灰尘和水汽。但是目前存在的问题是曲面屏手机的屏幕是有弧度的，贴上常规全贴合的材料不能满足贴合要求，容易产生变形，气泡反弹，生产完美的贴合的手机膜难度大。
发明内容
有鉴于此，本发明所要解决的技术问题是提供了一种用于曲面屏贴合粘合剂的制备方法。
本发明的技术解决方案是一种用于曲面屏贴合粘合剂的制备方法，包括若干类单体，将所述若干类单体混合均匀至反应釜，然后加入溶剂和引发剂，混合均匀后倒入装有温度计、机械搅拌和冷凝管的四口烧瓶，然后加热反应，当反应体系粘度开始增加时进行保温，之后再加入1-20份的溶剂添加进反应体系中并搅拌均匀，最后冷却出料，得到丙烯酸酯压敏胶水，之后加入异氰酸酯固化剂、0.01-1%光引发剂、0.01-2%UV多官能团交联单体、0.3-2%助剂和0.01-0.5%偶联剂对得到的胶水进行调试。
本发明的进一步改进在于：所述若干类单体包括丙烯酸乙酯、丙烯酸丁酯、丙烯酸异辛酯、丙烯酸羟乙酯，丙烯酸甲酯，丙烯酰胺、甲基丙烯酸甲酯，甲基丙烯酸乙酯，丙烯酸，丙烯酸正辛酯，甲基丙烯酸，甲基丙烯酸环已酯，苯乙烯，醋酸乙烯酯，丙烯酸羟丙酯，甲基丙烯酸乙酯，甲基丙烯酸缩水甘油酯，甲基丙烯酸异辛酯和甲基丙烯酸异冰片酯，选取其中的5-10个单体进行混合至反应釜。
本发明的进一步改进在于：所述溶剂为甲苯、乙酸乙酯，丙酮二甲苯，环已酮，甲醇，乙醇和异丙醇其中一种或多种的混合。
本发明的进一步改进在于：所述引发剂为偶氮二异丁腈，偶氮二异庚腈，过氧化苯酰，过氧化二异丙苯，过氧化二特丁基和过氧化二碳酸二异丙脂其中一种或多种的混合。
本发明的进一步改进在于：加热温度为80℃，保温时间为1-1.5h。
本发明的进一步改进在于：加热时，四口烧瓶内机械搅拌的转数150rap/min，之后加入溶剂时其转数为300 rap/min，搅拌时间为20 min。
本发明的进一步改进在于：所述光引发剂为1173 2-羟基-2-甲基-1-苯基丙酮、184 1-羟基环己基苯基甲酮、TPO 2,4,6-三甲基苯甲酰基-二苯基氧化膦、TPO-L 2,4,6-三甲基苯甲酰基苯基膦酸乙酯的一种或多种的混合。
三羟甲基丙烷三丙烯酸酯。 季戊四醇三丙烯酸酯或TMPTA 或PETA 己二醇二丙烯酸酯 二缩三丙二醇二丙烯酸酯或HDDA 本发明的进一步改进在于：所述多官能团交联单体为TPGDA
本发明的进一步改进在于：所述助剂为消泡剂，所述消泡剂为高碳醇脂肪酸酯复合物、聚氧乙烯聚氧丙烯季戊四醇醚、聚氧乙烯聚氧丙醇胺醚、聚氧丙烯甘油醚和聚氧丙烯聚氧乙烯甘油醚或者聚二甲基硅氧烷。
本发明的进一步改进在于：所述偶联剂为γ-(甲基丙烯酰氧)丙基三甲氧基硅烷γ-缩水甘油醚氧丙基三甲氧基硅烷或者N-β -(氨乙基)-γ -氨丙基甲基二甲氧基硅烷。
与现有技术相比，本发明的有益效果是：该粘合剂具有很好的填充性能，并且通过后UV后，可以减少终端设备中所出现的贴合气泡，并减少贴合气泡反弹情况的发生，并通过单体比例的不同，调整胶体的软硬，来达到高段差填充。
附图说明
图1是实施例1中各组分聚合、交联和接枝反应图。
具体实施方式
以下将配合实施例来详细说明本申请的实施方式，借此对本申请如何应用技术手段来解决技术问题并达成技术功效的实现过程能充分理解并据以实施。
实施例1：
本实施例的技术解决方案是：本发明提供的一种用于曲面屏贴合粘合剂的制备方法、将丙烯酸乙酯、丙烯酸丁酯、丙烯酸异辛酯、丙烯酸羟乙酯、丙烯酸甲酯，丙烯酰胺、甲基丙烯酸甲酯、甲基丙烯酸乙酯、丙烯酸、丙烯酸正辛酯混合均匀至反应釜，之后加入溶剂甲苯及引发剂偶氮二异丁腈，混合均匀后倒入装有温度计、机械搅拌和冷凝管的四口烧瓶，然后加热至80℃反应，此时转数为150rap/min，当反应体系粘度开始增加时计时，保温时间1.5h；后再将1～20份的溶剂甲苯添加进反应体系中，并将转数150rap/min调整为300 rap/min，搅拌20 min；最后冷却出料，得到丙烯酸酯压敏胶，其固含量为25-40％（固含量是乳液或涂料在规定条件下烘干后剩余部分占总量的质量百分数）。
调试配方：
在制备的丙烯酸酯压敏胶胶水里加入异氰酸酯固化剂、增加交联，提高胶水的韧性，解决胶体溢胶现象。
在配方中加入0.05%的光引发剂（或光敏剂）1173 2-羟基-2-甲基-1-苯基丙酮），和1%UV的多官能团交联单体TPGDA二缩三丙二醇二丙烯酸酯，经过吸收紫外线（UV）光固化设备中的高强度紫外光后，产生活性自由基或离子基，从而引发聚合、交联和接枝反应，见附图1。
其次再加入改善其他性能的助剂，例如1%消泡剂高碳醇脂肪酸酯复合物和0.2%偶联剂γ-(甲基丙烯酰氧)丙基三甲氧基硅烷γ-缩水甘油醚氧丙基三甲氧基硅烷，改善胶的表观及贴合效果。
最后在离型膜上涂100-200μ的干胶，至烘箱烘10-30min，负另一层离型膜，完成压敏胶成品的制作。
Figure DEST_PATH_IMAGE002AAAA
贴合：曲面屏贴合用专用曲面屏贴合机和专用的精密模具,采用G+G方式贴合，贴合好的材料保证无气泡后UV光照。最后把本产品放进环测240H，无返泡现象。
Figure DEST_PATH_IMAGE004
性能：压敏胶粘带180°剥离强度试验方法GB/T2792—1998
压敏胶粘带持粘性试验方法GB/T4851—1998
剥离力 持粘力 定荷 初粘
2000mj/cm2前 2000 10H >10H <5#
2000mj/cm2后 2400 >10H >10H <5#
实施例2：
选取单体丙烯酸正辛酯，甲基丙烯酸，甲基丙烯酸环已酯，苯乙烯，醋酸乙烯酯，丙烯酸羟丙酯，甲基丙烯酸乙酯，甲基丙烯酸缩水甘油酯，甲基丙烯酸异辛酯混合均匀至反应釜，与溶剂异丙醇及引发剂过氧化苯酰混合均匀后倒入装有温度计、机械搅拌和冷凝管的四口烧瓶，然后加热至80℃反应，当反应体系粘度开始增加时计时，保温时间1 h，后再将10份的溶剂异丙醇添加进反应体系中，使转数150rap/min调整为300 rap/min，搅拌20 min；最后冷却出料，调试配方。
在制备的胶水里加入异氰酸酯固化剂、增加交联，提高胶水的韧性，解决胶体溢胶现象，再加入0.05%光引发剂（或光敏剂）TPO-L 2,4,6-三甲基苯甲酰基苯基膦酸乙酯，和0.05%UV多官能团交联单体HDDA己二醇二丙烯酸酯，经过吸收紫外线（UV）光固化设备中的高强度紫外光后，产生活性自由基或离子基，从而引发聚合、交联和接枝反应。
其次再加入一些改善其他的性能的助剂，例如0.5%消泡剂聚氧乙烯聚氧丙醇胺醚和0.3%偶联剂N-β -(氨乙基)-γ -氨丙基甲基二甲氧基硅烷，改善胶的表观及贴合效果。
实施例3：
选取单体丙烯酸乙酯、丙烯酸异辛酯、丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸、丙烯酸正辛酯、甲基丙烯酸环已酯、丙烯酸羟丙酯和甲基丙烯酸异辛酯混合均匀至反应釜，与溶剂乙酸乙酯及引发剂过氧化二异丙苯混合均匀后倒入装有温度计、机械搅拌和冷凝管的四口烧瓶，然后加热至80℃反应，当反应体系粘度开始增加时计时，保温时间1 h，后再将15份的溶剂乙酸乙酯添加进反应体系中，使转数150rap/min调整为300 rap/min，搅拌20 min；最后冷却出料，调试配方。
三羟甲基丙烷三丙烯酸酯，经过吸收紫外线（UV）光固化设备中的高强度紫外光后，产生活性自由基或离子基，从而引发聚合、交联和接枝反应。 在制备的胶水里加入异氰酸酯固化剂、增加交联，提高胶水的韧性，解决胶体溢胶现象，再加入0.05%光引发剂（或光敏剂）184 1-羟基环己基苯基甲酮，和0.05%UV多官能团交联单体TMPTA
其次再加入一些改善其他的性能的助剂，例如0.1%消泡剂聚氧乙烯聚氧丙醇胺醚和0.08%偶联剂N-β -(氨乙基)-γ -氨丙基甲基二甲氧基硅烷，改善胶的表观及贴合效果。
上述说明示出并描述了本发明的若干优选实施例，但如前所述，应当理解本发明并非局限于本文所披露的形式，不应看作是对其他实施例的排除，而可用于各种其他组合、修改和环境，并能够在本文所述发明构想范围内，通过上述教导或相关领域的技术或知识进行改动。而本领域人员所进行的改动和变化不脱离本发明的精神和范围，则都应在本发明所附权利要求的保护范围内。

Claims (10)

1.一种用于曲面屏贴合粘合剂的制备方法，其特征在于：包括若干类单体，将所述若干类单体混合均匀至反应釜，然后加入溶剂和引发剂，混合均匀后倒入装有温度计、机械搅拌和冷凝管的四口烧瓶，然后加热反应，当反应体系粘度开始增加时进行保温，之后再加入1-20份的溶剂添加进反应体系中并搅拌均匀，最后冷却出料，得到丙烯酸酯压敏胶水，之后加入异氰酸酯固化剂、0.01-1%光引发剂、0.01-2%UV多官能团交联单体、0.3-2%助剂和0.01-0.5%偶联剂对得到的胶水进行调试。
2.如权利要求 1 所述的一种用于曲面屏贴合粘合剂的制备方法，其特征在于：所述若干类单体包括丙烯酸乙酯、丙烯酸丁酯、丙烯酸异辛酯、丙烯酸羟乙酯、丙烯酸甲酯、丙烯酰胺、甲基丙烯酸甲酯、甲基丙烯酸乙酯、丙烯酸、丙烯酸正辛酯、甲基丙烯酸、甲基丙烯酸环已酯、苯乙烯、醋酸乙烯酯、丙烯酸羟丙酯、甲基丙烯酸乙酯、甲基丙烯酸缩水甘油酯、甲基丙烯酸异辛酯和甲基丙烯酸异冰片酯，选取其中的5-10个单体进行混合至反应釜。
3.如权利要求 1 所述的一种用于曲面屏贴合粘合剂的制备方法，其特征在于：所述溶剂为甲苯、乙酸乙酯，丙酮二甲苯，环已酮，甲醇，乙醇和异丙醇其中一种或多种的混合。
4.如权利要求 1 所述的一种用于曲面屏贴合的粘合剂的制备方法，其特征在于：所述引发剂为偶氮二异丁腈，偶氮二异庚腈，过氧化苯酰，过氧化二异丙苯，过氧化二特丁基和过氧化二碳酸二异丙脂其中一种或多种的混合。
5.如权利要求 1所述的一种用于曲面屏贴合粘合剂的制备方法，其特征在于：加热温度为80℃，保温时间为1-1.5h。
6.如权利要求 1 所述的一种用于曲面屏贴合粘合剂的制备方法，其特征在于：加热时，四口烧瓶内机械搅拌的转数150rap/min，之后加入溶剂时其转数为300 rap/min，搅拌时间为20 min。
7.如权利要求 1 所述的一种用于曲面屏贴合粘合剂的制备方法，其特征在于：所述光引发剂为1173 2-羟基-2-甲基-1-苯基丙酮、184 1-羟基环己基苯基甲酮、TPO　 2,4,6-三甲基苯甲酰基-二苯基氧化膦、TPO-L 2,4,6-三甲基苯甲酰基苯基膦酸乙酯的一种或多种的混合。
8.三羟甲基丙烷三丙烯酸酯。
9. 季戊四醇三丙烯酸酯或TMPTA 或PETA 己二醇二丙烯酸酯 二缩三丙二醇二丙烯酸酯或HDDA 如权利要求 1 所述的一种用于曲面屏贴合粘合剂的制备方法，其特征在于：所述多官能团交联单体为TPGDA
如权利要求 1 所述的一种用于曲面屏贴合粘合剂的制备方法，其特征在于：所述助剂为消泡剂，所述消泡剂为高碳醇脂肪酸酯复合物、聚氧乙烯聚氧丙烯季戊四醇醚、聚氧乙烯聚氧丙醇胺醚、聚氧丙烯甘油醚和聚氧丙烯聚氧乙烯甘油醚或者聚二甲基硅氧烷。
10.如权利要求 1 所述的一种用于曲面屏贴合粘合剂的制备方法，其特征在于：所述偶联剂为γ-(甲基丙烯酰氧)丙基三甲氧基硅烷γ-缩水甘油醚氧丙基三甲氧基硅烷或者N-β -(氨乙基)-γ -氨丙基甲基二甲氧基硅烷。
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