CN113698652A - 一种高氧气阻隔涂布膜及其制备方法 - Google Patents

一种高氧气阻隔涂布膜及其制备方法 Download PDF

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CN113698652A
CN113698652A CN202111053388.8A CN202111053388A CN113698652A CN 113698652 A CN113698652 A CN 113698652A CN 202111053388 A CN202111053388 A CN 202111053388A CN 113698652 A CN113698652 A CN 113698652A
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coating
acrylate
oxygen barrier
high oxygen
monomer
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白永平
钟文
李卫东
殷晓芬
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Wuxi Haite New Material Research Institute Co Ltd
Harbin Institute of Technology of Wuxi Research Institute of New Materials
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Harbin Institute of Technology of Wuxi Research Institute of New Materials
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Abstract

本发明公开了一种高氧气阻隔涂布膜及其制备方法，其中的高氧气阻隔涂布膜包括：基膜；涂层，所述涂层由丙烯酸酯高阻氧涂料涂布、固化在所述基膜上形成。本发明通过自由基聚合将丙烯酸酯硬单体、丙烯酸酯软单体、丙烯酸酯前交联单体和丙烯酸酯后交联单体共聚得到高氧气阻隔涂料。其中，硬单体提供分子链段刚性，软单体防止涂层开裂，前交联单体使聚合物在聚合过程中形成部分网状结构，后交联单体通过再固化过程交联形成致密的网状结构，限制涂层聚合物的分子链段热运动，减少及闭塞氧气的渗透路径来达到提升阻隔性能的效果。通过涂布方式将该涂料涂布在基膜上可以显著改善基膜的氧气阻隔性能。

Description

一种高氧气阻隔涂布膜及其制备方法
技术领域
本发明涉及涂料制备领域，特别是涉及一种高氧气阻隔涂布膜及其制备方法。
背景技术
聚对苯二甲酸乙二醇酯(PET)薄膜以其优异的密封性、透明性、耐高温性和抗拉强度而著称，可满足大多数包装要求。近年来，它已成为食品、医药和化妆品领域的重要包装材料。因此对PET的高性能和新的功能性的需求正在增长，特别是氧气的阻隔性能。由于涂层具有合成工艺简单、设备要求不复杂、功能多样和与基材的良好粘合性，涂层是提高PET薄膜最快捷和实际的方法之一。
发明内容
为了提高PET薄膜对氧气的阻隔性能，本发明首先提供了一种高氧气阻隔涂布膜，其技术方案如下：
一种高氧气涂布膜，包括：
基膜；
涂层，所述涂层由丙烯酸酯高阻氧涂料涂布、固化在所述基膜上形成。
在一些实施例中，所述丙烯酸酯高阻氧涂料由如下重量百分比的单体聚合而成：丙烯酸酯硬单体53-75％；丙烯酸酯软单体15-20％；前交联单体0.2-2％；后交联单体5-25％。
在一些实施例中，所述丙烯酸酯硬单体为甲基丙烯酸甲酯，苯乙烯，丙烯酸异冰片酯，醋酸乙烯酯，甲基丙烯酸异冰片酯种的一种或几种。
在一些实施例中，所述丙烯酸软单体为丙烯酸甲酯，丙烯酸乙酯，丙烯酸丁酯，丙烯酸异辛酯等中的一种或几种。
在一些实施例中，所述前交联单体为二乙烯基苯，四甲基环四硅氧烷，马来酸二烯丙酯中的一种或几种。
在一些实施例中，所述后交联单体为丙烯酸，甲基丙烯酸，丙烯酸羟乙酯，甲基丙烯酸羟乙酯，丙烯酸羟丙酯，丁烯二醇，顺丁烯二酸，反丁烯二酸，顺丁烯二酸肝中的一种或多种。
在一些实施例中，在将所述丙烯酸酯高阻氧涂料涂布至基膜前，加入固化剂，所述固化剂为金属酸酯，金属螯合物，金属盐，异氰酸酯，有机硅烷，聚碳化二亚胺，乙烯亚胺，丙烯亚胺，环氧树脂，氨基树脂中的一种或几种。
在一些实施例中，所述基膜为PET、PE、OPP、PA中的一种或几种的复合膜；所述涂层的厚度为2-8微米。
本发明还提供了一种高氧气阻隔涂布膜的制备方法，其包括以下步骤：
按重量百分比，将丙烯酸酯硬单体、丙烯酸酯软单体、前交联单体、后交联单体通过自由基聚合成丙烯酸酯高氧气阻隔涂料；
采用网纹辊涂布方式，将丙烯酸酯高氧气阻隔涂料均匀涂布在基膜上，网纹目数为100-200目；
涂布膜经烘箱干燥，干燥温度为130-200℃，干燥时长为15-60s；
收卷、放入熟化室内熟化0.5-4d，熟化温度为40-60℃。
在一些实施例中，所述网纹辊涂布方式为微凹逆涂，线速比为0.8-1.5；所述丙烯酸高阻氧涂料的上机粘度为400-1000cps。
本发明的有益效果：
本发明通过自由基聚合将丙烯酸酯硬单体、丙烯酸酯软单体、丙烯酸酯前交联单体和丙烯酸酯后交联单体共聚得到高氧气阻隔涂料。其中硬单体提供分子链段刚性，软单体防止涂层开裂，前交联单体使聚合物在聚合过程中形成部分网状结构，后交联单体通过再固化过程交联形成致密的网状结构，限制涂层聚合物的分子链段热运动，减少自由体积分数，减少及闭塞氧气的渗透路径来达到提升阻隔性能的效果。
通过涂布的方式将该涂料涂布在基膜上，可以显著改善基膜的氧气阻隔性能。在其他性能不变的情况下，可以得到高氧气阻隔的薄膜用于包装材料。
具体实施方式
下面结合具体实例，进一步阐明本说明。本部分的描述仅是示范性和解释性，不应对本发明的保护范围有任何的限制作用。
实施例1
采用自由基聚合将苯乙烯75g，丙烯酸乙酯19.8g，二乙烯基苯0.2g，丙烯酸羟乙酯5g合成丙烯酸酯高氧气阻隔涂料，加入0.5g异氰酸酯，涂料粘度为400cps。
采用网纹目数为100目的网纹辊将涂料均匀涂布在OPP膜上，涂布膜经130℃-150℃的多节烘箱干燥60S。
收卷后放入40℃熟化室熟化4d，得到高阻氧涂布膜。
实施例2
采用自由基聚合将60g醋酸乙烯酯，20g丙烯酸丁酯，5g马来酸二烯丙酯，15g丙烯酸合成丙烯酸酯高氧气阻隔涂料，加入10g环氧树脂，涂料粘度为1000cps。
采用网纹目数为200目的网纹辊将涂料均匀涂布在PA膜上，涂布膜经140℃-180℃的多节烘箱干燥30S。
收卷后放入50℃熟化室熟化2d，得到高阻氧涂布膜。
实施例3
采用自由基聚合将53g甲基丙烯酸甲酯，20g丙烯酸甲酯，2g四乙烯基环四硅氧烷，25g顺丁烯二酸合成丙烯酸酯高氧气阻隔涂料，不加固化剂，涂料粘度为600cps。
采用微凹涂布的方式涂料均匀涂布在PET膜上，线速比为1.1，涂布膜经150℃-190℃的多节烘箱干燥15S。
收卷。放入60℃熟化室熟化0.5d。得到高阻氧涂布膜。
性能测试:
对比例一：普通丙烯酸酯聚合物涂布在OPP膜上
对比例二：无涂布OPP膜
对比例三：普通丙烯酸酯聚合物涂布在PA膜上
对比例四：无涂布PA膜
对比例五：普通丙烯酸酯聚合物涂布在PET膜上
对比例六：无涂布PE膜
测试方法：采用压制法经由设备测试氧气透过量。氧气透过率单位为cm3/m2·24h·0.1Mpa，测试数值越低表明氧气阻隔能力越强。
测试结果如下表所示：
测试样品 氧气透过率(cm<sup>3</sup>/m<sup>2</sup>·24h·0.1MPa)
实施例一 185.9
实施例二 18.4
实施例三 33.1
对比例一 754.2
对比例二 791.5
对比例三 54.7
对比例四 53.1
对比例五 100.2
对比例六 104.4
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下,还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (10)

1.一种高氧气阻隔涂布膜，其特征在于，所述高氧气阻隔涂布膜包括：
基膜；
涂层，所述涂层由丙烯酸酯高阻氧涂料涂布、固化在所述基膜上形成。
2.如权利要求1所述的高氧气阻隔涂布膜，其特征在于，所述丙烯酸酯高阻氧涂料由如下重量百分比的单体聚合而成：
丙烯酸酯硬单体53-75％；
丙烯酸酯软单体15-20％；
前交联单体0.2-2％；
后交联单体5-25％。
3.如权利要求1所述的高氧气阻隔涂布膜，其特征在于，所述丙烯酸酯硬单体为甲基丙烯酸甲酯，苯乙烯，丙烯酸异冰片酯，醋酸乙烯酯，甲基丙烯酸异冰片酯种的一种或几种。
4.如权利要求1所述的高氧气阻隔涂布膜，其特征在于，所述丙烯酸软单体为丙烯酸甲酯，丙烯酸乙酯，丙烯酸丁酯，丙烯酸异辛酯等中的一种或几种。
5.如权利要求1所述的高氧气阻隔涂布膜，其特征在于，所述前交联单体为二乙烯基苯，四甲基环四硅氧烷，马来酸二烯丙酯中的一种或几种。
6.如权利要求1所述的高氧气阻隔涂布膜，其特征在于，所述后交联单体为丙烯酸，甲基丙烯酸，丙烯酸羟乙酯，甲基丙烯酸羟乙酯，丙烯酸羟丙酯，丁烯二醇，顺丁烯二酸，反丁烯二酸，顺丁烯二酸肝中的一种或多种。
7.如权利要求1所述的高氧气阻隔涂布膜，其特征在于，在将所述丙烯酸酯高阻氧涂料涂布至基膜前，加入固化剂，所述固化剂为金属酸酯，金属螯合物，金属盐，异氰酸酯，有机硅烷，聚碳化二亚胺，乙烯亚胺，丙烯亚胺，环氧树脂，氨基树脂中的一种或几种。
8.如权利要求1所述的高氧气阻隔涂布膜，其特征在于，所述基膜为PET、PE、OPP、PA中的一种或几种的复合膜；
所述涂层的厚度为2-8微米。
9.一种如权利要求2至8任一项所述的高氧气阻隔涂布膜的制备方法，其特征在于，其包括以下步骤：
按重量百分比，将丙烯酸酯硬单体、丙烯酸酯软单体、前交联单体、后交联单体通过自由基聚合成丙烯酸酯高氧气阻隔涂料；
采用网纹辊涂布方式，将丙烯酸酯高氧气阻隔涂料均匀涂布在基膜上，网纹目数为100-200目；
涂布膜经烘箱干燥，干燥温度为130-200℃，干燥时长为15-60s；
收卷、放入熟化室内熟化0.5-4d，熟化温度为40-60℃。
10.如权利要求9所述的制备方法，其特征在于：
所述网纹辊涂布方式为微凹逆涂，线速比为0.8-1.5；
所述丙烯酸高阻氧涂料的上机粘度为400-1000cps。
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