CN114437649A - 一种有机氟改性聚丙烯酸压敏胶及其制备方法 - Google Patents
一种有机氟改性聚丙烯酸压敏胶及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种有机氟改性聚丙烯酸酯压敏胶及其制备方法,包括下列重量份的组份:软单体:70‑95份;硬单体:2‑20份;功能单体:1‑8份;含氟单体:1‑20份;引发剂:0.1‑0.6份;交联剂:0.3‑3份;溶剂:100‑150份,本发明选用含有丙烯酸酯类双键的含氟材料参与自由基聚合反应,与软单体、硬单体、功能单体无规共聚,合成具有超低表面能的丙烯酸酯压敏胶,在该丙烯酸酯压敏胶中加入交联剂,提高内聚能、耐温性、粘结力稳定性,用该压敏胶制备的保护膜,耐湿热性佳,高温高湿环境不污染被保护材料,随时间延长,粘合力增长幅度小,保护膜易贴易撕。
Description
技术领域
本发明涉及胶粘剂技术领域,特别是一种低表面能氟改性丙烯酸酯压敏胶的制备及应用。
背景技术
压敏胶是一种仅需指触压力就能达到粘结目的胶粘剂。压敏胶制品广泛应用于包装、汽车、运输、电子通讯、电器、建材、机械、航空航天、轻工业、医疗卫生、家庭等各个方面。它们方便的应用于封缄、捆扎、遮蔽、密封、保护、增强、拼接、模印、识别、包装、绝缘、固定等各种用途。压敏胶按其化学成分不同可分为:橡胶系压敏胶、聚丙烯酸酯系压敏胶、有机硅系压敏胶,以及聚氨酯压敏、聚异丁烯系压敏胶等,其中聚丙烯酸酯压敏胶因其优良的粘结性、耐老化性、耐温性、透光性,以及原料易得、生产稳定等特点,成为压敏胶领域重要组成部分。
保护膜是聚丙烯酸酯压敏胶重要应用领域,它是由塑料薄膜或纸基材料涂布专用压敏胶,经特定工艺加工而成。保护膜是具有保护功能的材料,主要用于产品制造、运输、储存过程中,贴敷在产品表面,避免产品污染和破坏。电子领域,保护膜是电子产品制程不可或缺的辅料,性能要求非常高,要求优异的易贴敷、耐湿热、耐高温、无污染、易剥离、高透光等,但是目前电子保护膜存在两个问题(1)耐湿热性差。保护膜贴合被保护材料表面后,经高温高湿环境,被保护膜材料表面有白雾。(2)排气性差。保护膜贴合被保护材料时不易操作,润湿性不佳,易有气泡缺陷。(3)粘结力经时不稳定。保护膜贴合在被保护材料表面,随时间延长,粘结力逐渐增加,最后不易撕除。
发明内容
本发明针对现有技术不足,提出一种低表面能含氟丙烯酸酯压敏胶及其制备方法,该压敏胶具有良好的润湿性、优异的耐湿热性、粘合力稳定,以解决上述技术问题。
为解决上述技术问题,本发明提供如下技术方案:本发明氟改性丙烯酸酯压敏胶包括下列重量份的组份:
软单体:70-95份;
硬单体:2-20份;
功能单体:1-8份;
含氟单体:1-20份;
引发剂:0.1-0.6份;
交联剂:0.3-3份;
溶剂:100-150份。
优选地,所述软单体为丙烯酸丁酯、丙烯酸异辛酯、丙烯酸-2-乙基己酯、丙烯酸月桂酯、丙烯酸乙酯、甲基丙烯酸月桂酯中的一种或多种组成。
优选地,所述硬单体为丙烯酸甲酯、甲基丙烯酸甲酯、醋酸乙烯、丙烯腈、苯乙烯、丙烯酸异冰片酯、甲基丙烯酸异冰片酯、甲基丙烯酸四氢呋喃酯中的一种或多种组成。
优选地,所述功能单体为丙烯酸羟乙酯、丙烯羟丙酯、4-羟基丁基丙烯酸酯、甲基丙烯酸羟乙酯、甲基丙烯酸羟丙酯、丙烯酸、甲基丙烯酸、衣康酸、丙烯酸铵、N-羟甲基丙烯酰胺、甲基丙烯酸缩水甘油酯中的一种或多种组成。
优选地,所述含氟单体为丙烯酸六氟丁酯、丙烯酸六氟异丙酯、丙烯酸八氟戊酯、丙烯酸12氟庚酯、甲基丙烯酸六氟异丙酯、甲基丙烯酸八氟戊酯、甲基丙烯酸12氟庚酯、全氟癸基乙基丙烯酸酯、全氟丁基乙基丙烯酸酯、全氟烷基乙基甲基丙烯酸酯中的一种或多种组成。
优选地,所述引发剂为过氧化二苯甲酰、偶氮二异丁腈中的一种或二种组成。
优选地,所述交联剂为芳香族聚异氰酸酯、脂肪族聚异氰酸酯、氮丙啶、环氧树脂(GA240)种的一种或多种组成;
优选地,所述溶剂为甲苯、乙酸乙酯、正己烷、丙酮、甲醇中的一种或多种组成。
本发明还提供了有机氟改性聚丙烯酸酯压敏胶的制备方法,其步骤如下:
(1)将软单体、硬单体、功能单体、含氟单体、15%溶剂、70%引发剂混合均匀。取10-30%混合液、50-70%溶剂加入反应釜,加热至70-90℃,当出现回流、泡沫增多时,反应开始,自反应开始计时10-30分钟;
(2)滴加剩余单体、引发剂、溶剂的混合液,90-150分钟滴完,保温1-2小时;
(3)补加剩余30%引发剂,保温2-4小时;
(4)冷却,添加剩余溶剂,固含量调整40-50%,出料。
与现有技术相比,本发明的有益效果为:本发明选用含有丙烯酸酯类双键的含氟材料参与自由基聚合反应,与软单体、硬单体、功能单体无规共聚,合成具有超低表面能的丙烯酸酯压敏胶。低表面能不仅赋予该压敏胶优异的防水性,还另该聚合物在多种板材(金属、塑料、玻璃等)表面均具有良好的润湿性。在该丙烯酸酯压敏胶中加入交联剂,提高内聚能、耐温性、粘结力稳定性,用该压敏胶制备的保护膜,耐湿热性佳,高温高湿环境不污染被保护材料,随时间延长,粘合力增长幅度小,保护膜易贴易撕。
具体实施方式
下面通过具体实施例对本发明进行详细和具体的介绍,以便更好的理解本发明,但是下述实施例并不限制本发明范围。
实施例1:
首先称取50g丙烯酸异辛酯、38.7g丙烯酸丁酯、4g甲基丙烯酸甲酯、0.3g丙烯酸、3g丙烯酸羟乙酯、2g4-羟基丁基丙烯酸酯、2g丙烯酸12氟庚酯混合均匀,取单体混合液30g加入反应瓶,取称取50g乙酸乙酯、20g甲苯、10g丙酮放入反应瓶,称取0.1g偶氮二异丁腈加入反应瓶,在搅拌条件,逐渐加热到70℃以上回流反应,观察反应体系,自出现明显回流开始计时,反应20分钟;
反应20分钟后,取单体混合液70g、乙酸乙酯10g、偶氮二异丁腈0.1g搅拌均匀,将混合液均匀滴入反应瓶,90分钟滴完,然后保温2小时;
保温2小时后,取0.1g偶氮二异丁腈、5g乙酸乙酯混合均匀,加入反应瓶,保温2小时;
最后,加入55g甲苯与乙酸乙酯的混合液稀释到40%固含量,冷却出料;
称取50g胶液,加入1g脂肪族聚异氰酸酯固化剂N75,加入20g乙酸乙酯调稀,搅拌均匀,涂布在50um透明聚酯薄膜上,放入110℃烘箱3分钟,取出,复合硅离型膜,控制干胶层厚度15um,放入50℃后固化2天,制得性能的稳定的保护膜样张。
实施例2:
首先称取74.5g丙烯酸异辛酯、10g丙烯酸甲酯、5g醋酸乙烯、2g衣康酸、3g丙烯酸羟乙酯、0.5g甲基丙烯酸缩水甘油酯、5g丙烯酸六氟丁酯混合均匀,取单体混合液30g加入反应瓶,取称取50g乙酸乙酯、30g甲苯放入反应瓶,称取0.1g过氧化苯甲酰加入反应瓶,在搅拌条件,逐渐加热到80℃以上回流反应,观察反应体系,自出现明显回流开始计时,反应20分钟;
反应20分钟后,取单体混合液70g、甲苯10g、过氧化苯甲酰0.1g搅拌均匀,将混合液均匀滴入反应瓶,90分钟滴完,然后保温2小时;
保温2小时后,取0.1g过氧化苯甲酰、5g甲苯混合均匀,加入反应瓶,保温2小时;
最后,加入55g乙酸乙酯稀释到40%固含量,冷却出料;
称取50g胶液,加入1g芳香族聚异氰酸酯固化剂L75,加入20g乙酸乙酯调稀,搅拌均匀,涂布在50um透明聚酯薄膜上,放入110℃烘箱3分钟,取出,复合硅离型膜,控制干胶层厚度15um,放入50℃后固化2天,制得性能的稳定的保护膜样张。
实施例3:
首先称取28.8g丙烯酸异辛酯、50g丙烯酸丁酯、10g醋酸乙烯、2g丙烯腈、4g丙烯酸、0.2g甲基丙烯酸羟乙酯、5g丙烯酸六氟异丙酯混合均匀,取单体混合液30g加入反应瓶,取称取50g乙酸乙酯、20g甲苯、10g正己烷放入反应瓶,称取0.1g过氧化苯甲酰加入反应瓶,在搅拌条件,逐渐加热到80℃以上回流反应,观察反应体系,自出现明显回流开始计时,反应30分钟;
反应30分钟后,取单体混合液70g、甲苯10g、过氧化苯甲酰0.1g搅拌均匀,将混合液均匀滴入反应瓶,90分钟滴完,然后保温2小时;
保温2小时后,取0.1g过氧化苯甲酰、5g甲苯混合均匀,加入反应瓶,保温2小时;
最后,加入55g乙酸乙酯稀释到40%固含量,冷却出料;
称取50g胶液,加入0.3g环氧固化剂GA240,加入20g乙酸乙酯调稀,搅拌均匀,涂布在50um透明聚酯薄膜上,放入110℃烘箱3分钟,取出,复合硅离型膜,控制干胶层厚度15um,放入50℃后固化2天,制得性能的稳定的保护膜样张。
实施例4:
首先称取29.8g丙烯酸异辛酯、48g丙烯酸丁酯、4g甲基丙烯酸四氢呋喃酯、6g醋酸乙烯、1gN-羟甲基丙烯酰胺、4g丙烯酸、0.2g丙烯酸羟乙酯、7g丙烯酸八氟戊酯混合均匀,取单体混合液30g加入反应瓶,取称取50g乙酸乙酯、30g甲苯放入反应瓶,称取0.1g过氧化苯甲酰加入反应瓶,在搅拌条件,逐渐加热到80℃以上回流反应,观察反应体系,自出现明显回流开始计时,反应30分钟;
反应30分钟后,取单体混合液70g、甲苯10g、过氧化苯甲酰0.1g搅拌均匀,将混合液均匀滴入反应瓶,90分钟滴完,然后保温2小时;
保温2小时后,取0.1g过氧化苯甲酰、5g甲苯混合均匀,加入反应瓶,保温2小时;
最后,加入55g乙酸乙酯稀释到40%固含量,冷却出料;
称取50g胶液,加入0.3g氮丙啶固化剂,加入20g乙酸乙酯调稀,搅拌均匀,涂布在50um透明聚酯薄膜上,放入110℃烘箱3分钟,取出,复合硅离型膜,控制干胶层厚度15um,放入50℃后固化2天,制得性能的稳定的保护膜样张。
实施例5:
首先称取60g乙酸乙酯、10g甲苯、5g丙酮,加入反应瓶,在搅拌条件,加热至70℃以上回流;
称取75.7g丙烯酸-2-乙基己酯、10g甲基丙烯酸月桂酯、3g甲基丙烯酸异冰片酯、0.3g丙烯酸、2g丙烯酰胺、5g丙烯酸羟乙酯、4g甲基丙烯酸12氟庚酯混合均匀,取单体混合液30g加入反应瓶;称取0.1g偶氮二异丁腈加入反应瓶,观察反应体系,自出现反应开始计时,反应15分钟;
反应15分钟后,取单体混合液70g、乙酸乙酯20g、偶氮二异丁腈0.1g搅拌均匀,将混合液均匀滴入反应瓶,90分钟滴完,然后保温2小时;
保温2小时后,取0.1g偶氮二异丁腈、5g乙酸乙酯混合均匀,加入反应瓶,保温2小时;
最后,加入55g甲苯稀释到40%固含量,冷却出料;
称取50g胶液,加入1g脂肪族聚异氰酸酯固化剂N75,加入20g乙酸乙酯调稀,搅拌均匀,涂布在50um透明聚酯薄膜上,放入110℃烘箱3分钟,取出,复合硅离型膜,控制干胶层厚度15um,放入50℃后固化2天,制得性能的稳定的保护膜样张。
实施例6:
首先称取50g乙酸乙酯、10g甲苯、10g甲醇,加入反应瓶,在搅拌条件,加热至70℃以上回流;
称取40g丙烯酸异辛酯、43g丙烯酸丁酯、3g丙烯酸异冰片酯、5g苯乙烯、1g丙烯酸、3g丙烯酸羟乙酯、5g甲基丙烯酸6氟丁酯混合均匀,取单体混合液30g加入反应瓶;称取0.1g偶氮二异丁腈加入反应瓶,观察反应体系,自出现反应开始计时,反应15分钟;
反应15分钟后,取单体混合液70g、乙酸乙酯20g、偶氮二异丁腈0.1g搅拌均匀,将混合液均匀滴入反应瓶,90分钟滴完,然后保温2小时;
保温2小时后,取0.1g偶氮二异丁腈、5g乙酸乙酯混合均匀,加入反应瓶,保温2小时;
最后,加入55g甲苯稀释到40%固含量,冷却出料;
称取50g胶液,加入0.5g芳香族聚异氰酸酯固化剂L75,加入20g乙酸乙酯调稀,搅拌均匀,涂布在50um透明聚酯薄膜上,放入110℃烘箱3分钟,取出,复合硅离型膜,控制干胶层厚度15um,放入50℃后固化2天,制得性能的稳定的保护膜样张。
比较例1:
首先称取52g丙烯酸异辛酯、39.7g丙烯酸丁酯、4g甲基丙烯酸甲酯、0.3g丙烯酸、4g丙烯酸羟乙酯混合均匀,取单体混合液30g加入反应瓶,取称取50g乙酸乙酯、20g甲苯、10g丙酮放入反应瓶,称取0.1g偶氮二异丁腈加入反应瓶,在搅拌条件,逐渐加热到70℃以上回流反应,观察反应体系,自出现明显回流开始计时,反应20分钟;
反应20分钟后,取单体混合液70g、乙酸乙酯10g、偶氮二异丁腈0.1g搅拌均匀,将混合液均匀滴入反应瓶,90分钟滴完,然后保温2小时;
保温2小时后,取0.1g偶氮二异丁腈、5g乙酸乙酯混合均匀,加入反应瓶,保温2小时;
最后,加入55g甲苯稀释到40%固含量,冷却出料;
称取50g胶液,加入1g脂肪族聚异氰酸酯固化剂N75,加入20g乙酸乙酯调稀,搅拌均匀,涂布在50um透明聚酯薄膜上,放入110℃烘箱3分钟,取出,复合硅离型膜,控制干胶层厚度15um,放入50℃后固化2天,制得性能的稳定的保护膜样张。
比较例2:
首先称取43g丙烯酸异辛酯、42.8g丙烯酸丁酯、10g醋酸乙烯、4g丙烯酸、0.2g丙烯酸羟乙酯混合均匀,取单体混合液30g加入反应瓶,取称取50g乙酸乙酯、30g甲苯放入反应瓶,称取0.1g过氧化苯甲酰加入反应瓶,在搅拌条件,逐渐加热到80℃以上回流反应,观察反应体系,自出现明显回流开始计时,反应30分钟;
反应30分钟后,取单体混合液70g、甲苯10g、过氧化苯甲酰0.1g搅拌均匀,将混合液均匀滴入反应瓶,90分钟滴完,然后保温2小时;
保温2小时后,取0.1g过氧化苯甲酰、5g甲苯混合均匀,加入反应瓶,保温2小时;
最后,加入55g乙酸乙酯稀释到40%固含量,冷却出料;
称取50g胶液,加入0.3g氮丙啶固化剂,加入20g乙酸乙酯调稀,搅拌均匀,涂布在50um透明聚酯薄膜上,放入110℃烘箱3分钟,取出,复合硅离型膜,控制干胶层厚度15um,放入50℃后固化2天,制得性能的稳定的保护膜样张。
以上对本发明的具体实施例进行了详细描述,但其只是作为范例,本发明并不限制于以上描述的具体实施例。对于本领域技术人员而言,任何对本发明进行的等同修改和替代也都在本发明的范畴之中。因此,在不脱离本发明的精神和范围下所作的均等变换和修改,都应涵盖在本发明的范围内。
Claims (7)
1.一种有机氟改性聚丙烯酸压敏胶,其特征在于,包括下列重量份的组份:
软单体:70-95份;
硬单体:2-20份;
功能单体:1-8份;
含氟单体:1-20份;
引发剂:0.1-0.6份;
交联剂:0.3-3份;
溶剂:100-150份。
2.根据权利要求1所述的一种有机氟改性聚丙烯酸压敏胶,其特征在于,所述软单体为丙烯酸丁酯、丙烯酸异辛酯、丙烯酸-2-乙基己酯、丙烯酸月桂酯、丙烯酸乙酯、甲基丙烯酸月桂酯中的一种或多种组成。
3.根据权利要求1所述的一种有机氟改性聚丙烯酸压敏胶,其特征在于,所述硬单体为丙烯酸甲酯、甲基丙烯酸甲酯、醋酸乙烯、丙烯腈、苯乙烯、丙烯酸异冰片酯、甲基丙烯酸异冰片酯、甲基丙烯酸四氢呋喃酯中的一种或多种组成。
4.根据权利要求1所述的一种有机氟改性聚丙烯酸压敏胶,其特征在于,所述功能单体为丙烯酸羟乙酯、丙烯羟丙酯、4-羟基丁基丙烯酸酯、甲基丙烯酸羟乙酯、甲基丙烯酸羟丙酯、丙烯酸、甲基丙烯酸、衣康酸、丙烯酸铵、N-羟甲基丙烯酰胺、甲基丙烯酸缩水甘油酯中的一种或多种组成。
5.根据权利要求1所述的一种有机氟改性聚丙烯酸压敏胶,其特征在于,所述含氟单体为丙烯酸六氟丁酯、丙烯酸六氟异丙酯、丙烯酸八氟戊酯、丙烯酸12氟庚酯、甲基丙烯酸六氟异丙酯、甲基丙烯酸八氟戊酯、甲基丙烯酸12氟庚酯、全氟癸基乙基丙烯酸酯、全氟丁基乙基丙烯酸酯、全氟烷基乙基甲基丙烯酸酯中的一种或多种组成。
6.根据权利要求1所述的一种有机氟改性聚丙烯酸压敏胶,其特征在于,所述引发剂为过氧化二苯甲酰、偶氮二异丁腈中的一种或两种组成;所述交联剂为芳香族聚异氰酸酯、脂肪族聚异氰酸酯、氮丙啶、环氧树脂(GA240)种的一种或多种组成;所述溶剂为甲苯、乙酸乙酯、正己烷、丙酮、甲醇中的一种或多种组成。
7.根据权利要求1所述的一种有机氟改性聚丙烯酸压敏胶的制备方法,其特征在于,其步骤如下:
(1)将软单体、硬单体、功能单体、含氟单体、15%溶剂、70%引发剂混合均匀。取10-30%混合液、50-70%溶剂加入反应釜,加热至70-90℃,当出现回流、泡沫增多时,反应开始,自反应开始计时10-30分钟;
(2)滴加剩余单体、引发剂、溶剂混合液,90-150分钟滴完,保温1-2小时;
(3)补加剩余30%引发剂,保温2-4小时;
(4)冷却,添加剩余溶剂,固含量调整40-50%,出料。
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