CN115304802B - 一种生产线快速固化的保护膜及其应用 - Google Patents
一种生产线快速固化的保护膜及其应用 Download PDFInfo
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Abstract
本发明公开了一种生产线快速固化的保护膜，制备原料以重量份计包括：多元醇聚合物70‑90份，抗氧化剂0.1‑0.5份，催化剂0.01‑0.3份，丙烯酸单体1‑15份，引发剂0.8‑6份，固化剂10‑30份。本发明采用无定型聚酯羟值含量为18‑112mgKOH/g的结晶型聚酯二元醇和羟值含量为27‑56KOH/g的聚酯二元醇协同作用，并搭配二元酸醇酯和丙烯酸单体可以制备得到快速固化的薄膜，并且能够在200℃高温环境中实现剥离，且无残胶。并且将制备得到的预聚体与含羟基的丙烯酸酯反应，可以实现双重固化的效果，进一步增加聚氨酯保护膜的内聚力，防止剥离后出现残胶。
Description
技术领域
本发明涉及一种生产线快速固化的保护膜，涉及C08G，具体涉及用碳-碳不饱和键以外的反应得到的高分子化合物。
背景技术
随着社会的发展，科技的进步，尤其是进入信息时代后，许多微量化的电子元器件在生产制备过程中需要镀膜保护，制备完成后需要去除保护膜，因此开发一种可以快速成膜，使用后又可快速剥离，不留残胶的保护膜至关重要。目前市面上的保护膜多依赖人工覆膜，生产效率较低，并且成品率不高。除此之外，现有的保护膜在临时保护后常常会有残胶遗留到基材表面，需要引入清洗工序清除残胶增加生产步骤，并且这些临时保护膜没有耐高温的性能，在200℃的温度下就会失去保护作用。
中国发明专利CN202111525139.4公开了一种聚氨酯压敏胶保护膜及其制备方法，通过在聚氨酯分子链上引入活性硅氧烷基团，形成致密的硅氧交联结构，使聚氨酯压敏胶具有一定的耐热性能，但是其剥离力较强，在临时保护后剥离时容易产生残胶。中国发明专利CN201610705351.1公开了一种双组份聚氨酯保护膜压敏胶及其合成工艺，通过采用聚氨酯橡胶型胶水，分子链中不含硅元素避免了硅转移产生的残胶问题，但是其耐高温性能不佳。
发明内容
为了改善聚氨酯保护膜的耐高温性能，同时使其容易剥离，不易产生残胶，本发明的第一个方面提供了一种生产线快速固化的保护膜，制备原料以重量份计包括：多元醇聚合物70-90份，抗氧化剂0.1-0.5份，催化剂0.01-0.3份，丙烯酸单体1-15份，引发剂0.8-6份，固化剂10-30份。
作为一种优选的实施方式，所述多元醇聚合物选自聚酯多元醇，聚醚多元醇中的一种或两种的组合，优选的，所述聚醚多元醇的数均分子量为1000-6000。
作为一种优选的实施方式，所述聚醚多元醇选自PPG2000陶氏聚醚2120、聚醚HF1000G河北厚发进出口贸易、聚醚TF330N河北厚发进出口贸易、上海博立尔BM775中的一种或几种的组合。
作为一种优选的实施方式，所述聚醚HF1000G及HF330N(河北厚发进出口贸易)的官能度为3。
作为一种优选的实施方式，所述聚酯多元醇为聚酯二元醇，优选的，所述聚酯二元醇的数均分子量为2000-6000。
作为一种优选的实施方式，所述聚酯二元醇的羟值含量为25-115mgKOH/g。其中结晶聚酯含量大于30重量份。
作为一种优选的实施方式，所述聚酯二元醇选自己二酸-1,4-丁二醇聚酯JH330山东久富新材、新戊二醇-己二酸聚酯1000N旭川化学、新戊二醇-己二酸-1,6-己二醇共聚聚酯二元醇T8560上海勒新化学、聚酯二元醇Dynacoll7250德国赢创、聚酯二元醇Dynacoll7360德国赢创、聚酯二元醇Dynacoll7380德国赢创、聚酯二元醇Dynacoll7150德国赢创中的一种或几种的组合。
申请人在实验过程中发现，采用羟值含量不同的聚酯二元醇组合，并搭配二元酸醇酯可以制备得到可以快速固化的薄膜，并且能够在200℃高温环境中实现剥离，且无残胶。猜测可能的原因是：无定型聚酯羟值含量为18-112mgKOH/g的结晶型聚酯二元醇和羟值含量为27-56mgKOH/g的聚酯二元醇协同作用制备得到聚氨酯预聚体，在反应初期形成的预聚体交联密度较低，在加工过程中容易施工，容易铺设至基材表面，防止形成的涂层交联密度较高只能进行人工铺设。申请人进一步发现，通过引入二元酸醇酯可以为后续聚氨酯薄膜的快速交联固化做好准备条件，使聚氨酯预聚体在与丙烯酸单体交联后能够快速形成高密度的涂层薄膜，增大涂层薄膜的内聚力，使其在剥离时容易脱除，防止残胶的产生。申请人进一步发现，形成聚氨酯预聚体后剩余的异氰酸酯可以与丙烯酸单体中的羟基反应形成不饱和双键和NCO的混合结构体系，进一步增加了聚氨酯涂层薄膜的内聚力，使其在80-200℃的高温下，小分子也不易迁出，高温环境下不会出现剥离残胶。
作为一种优选的实施方式，所述丙烯酸单体为含羟基的丙烯酸单体，优选的，选自丙烯酸羟乙酯、丙烯酸羟丙酯、甲基丙烯酸羟乙酯中的一种或几种的组合。
作为一种优选的实施方式，所述固化剂为异氰酸酯固化剂，优选的，所述异氰酸酯固化剂选自脂肪族异氰酸酯或芳香族异氰酸酯中的一种。
作为一种优选的实施方式，所述引发剂为光引发剂，优选的，选自烷基苯酮类引发剂、酰基磷氧化物类引发剂、苯偶酰类引发剂、二苯甲酮类引发剂中的一种或几种的组合。
作为一种优选的实施方式，所述光引发剂选自1-羟基环己基苯基甲酮、2,4,6-三甲基苯基甲酰基-二苯基氧化磷、2-羟基-2-甲基-1-苯基丙酮、2,4,6-三甲基苯甲酰基苯基膦酸乙酯、苯甲酰甲酸甲酯中的一种或几种的组合。
作为一种优选的实施方式，所述抗氧化剂为受阻酚类抗氧化剂，选自德国BASFIrganox 1010、Irganox 245、抗氧剂1076、抗氧剂264、抗氧剂2246中的一种或几种的组合。
作为一种优选的实施方式，所述催化剂为金属催化剂T-12。
作为一种优选的实施方式，所述生产线快速固化的保护膜的制备方法，包括以下步骤：
(1)将多元醇聚合物与抗氧化剂混合，加入固化剂110-130℃反应1-5h；
(2)反应后加入催化剂，冷却至80-100℃后加入丙烯酸单体，加入引发剂，90-100℃反应1h，出料即得。
作为一种优选的实施方式，所述保护膜的涂布方式选自喷涂、辊涂、刮涂方式中的一种或组合。
作为一种优选的实施方式，所述保护膜的涂布温度为25-150℃。
本发明的第二个方面提供了一种生产线快速固化的保护膜的应用，应用于玻璃、铝板、铜板、不锈钢板、芯片、PCB板的涂布保护中。
与现有技术相比，本发明具有以下有益效果：
(1)本发明所述生产线快速固化的保护膜，采用无定型聚酯羟值含量为18-112mgKOH/g的结晶型聚酯二元醇和羟值含量为27-56KOH/g的聚酯二元醇协同作用，并搭配二元酸醇酯和丙烯酸单体可以制备得到快速固化的薄膜，并且能够在200℃高温环境中实现剥离，且无残胶。
(2)本发明所述生产线快速固化的保护膜，采用结晶聚酯含量达到或超过30重量份含量时，并搭配二元酸醇酯和丙烯酸单体可以制备得到快速固化的薄膜，并且能够在常温和200℃高温环境中实现剥离，且无残胶。
(3)本发明所述生产线快速固化的保护膜，将制备得到的预聚体与含羟基的丙烯酸酯反应，可以实现双重固化的效果，进一步增加聚氨酯保护膜的内聚力，防止剥离后出现残胶。
(4)本发明所述生产线快速固化的保护膜，采用脂肪族异氰酸酯IPDI和抗氧化剂协同作用，使聚氨酯保护膜具有良好的耐高温性能和耐黄变性能，在200℃的高温下依旧具有良好的保护效果。
具体实施方式
下面通过实施例对本发明进行具体描述。有必要在此指出的是，以下实施例只用于对本发明作进一步说明，不能理解为对本发明保护范围的限制，该领域的专业技术人员根据上述本发明的内容做出的一些非本质的改进和调整，仍属于本发明的保护范围。
另外，如果没有其它说明，所用原料都是市售得到的。
实施例1
一种生产线快速固化的保护膜，制备原料以重量份计包括：多元醇聚合物73份，抗氧化剂0.3份，催化剂0.05份，丙烯酸单体11份，引发剂3份，固化剂16份。
所述多元醇聚合物为PPG2000陶氏聚醚2120，上海博立尔BM775、河北厚发聚醚HF1000G的组合，HF1000G为三官聚醚重均分子量为1500，重量比为45：20：8。
所述抗氧化剂为Irganox 245；所述催化剂为金属催化剂T-12；
所述丙烯酸单体为丙烯酸羟乙酯，所述引发剂为1-羟基环己基苯基甲酮；
所述固化剂为IPDI脂肪族异氰酸酯。
所述生产线快速固化的保护膜的制备方法，包括以下步骤：
(1)将多元醇聚合物与抗氧化剂混合，加入固化剂120℃反应3h；
(2)反应后加入催化剂，冷却至90℃后加入丙烯酸单体，加入引发剂，90℃反应1h，出料即得。
实施例2
一种生产线快速固化的保护膜，制备原料以重量份计包括：多元醇聚合物73份，抗氧化剂0.3份，催化剂0.05份，丙烯酸单体12份，引发剂4份，固化剂16份。
所述多元醇聚合物为己二酸-1,4-丁二醇聚酯HJ330山东久富新材，聚酯二元醇Dynacoll7250德国赢创的组合，重量比为48：25。
所述抗氧化剂为Irganox1010；所述催化剂为金属催化剂T-12；
所述丙烯酸单体为丙烯酸羟乙酯，所述引发剂为1-羟基环己基苯基甲酮；
所述固化剂为IPDI脂肪族异氰酸酯。
所述生产线快速固化的保护膜的制备方法，包括以下步骤：
(1)将多元醇聚合物与抗氧化剂混合，加入固化剂120℃反应3h；
(2)反应后加入催化剂，冷却至90℃后加入丙烯酸单体，加入引发剂，90℃反应1h，出料即得。
实施例3
一种生产线快速固化的保护膜，制备原料以重量份计包括：多元醇聚合物87份，抗氧化剂0.3份，催化剂0.05份，丙烯酸单体12份，引发剂5.1份，固化剂15份。
所述多元醇聚合物为聚酯二元醇Dynacoll7250德国赢创，己二酸-1,4-丁二醇聚酯HJ330山东久富新材、聚酯二元醇Dynacoll7360德国赢创的组合，重量比为25：19：43。
所述抗氧化剂为Irganox1010；所述催化剂为金属催化剂T-12；
所述丙烯酸单体为丙烯酸羟乙酯，所述引发剂为2,4,6-三甲基苯基甲酰基-二苯基氧化磷；
所述固化剂为IPDI脂肪族异氰酸酯。
所述生产线快速固化的保护膜的制备方法，包括以下步骤：
(1)将多元醇聚合物与抗氧化剂混合，加入固化剂120℃反应3h；
(2)反应后加入催化剂，冷却至90℃后加入丙烯酸单体，加入引发剂，90℃反应1h，出料即得。
性能测试
依据上述方法将制备得到的聚氨酯料采用喷涂的方式，在45℃下喷涂至玻璃板表面，采用秒表测试LED固化成膜时间；然后剥离，观察是否有残胶；重新喷涂后置于200℃的环境中放置2h，然后剥离，观察是否有残胶。
采用标准方法测试制备的聚氨酯料的结晶聚酯含量。测试结果见表1。
表1
Claims (7)
1.一种生产线快速固化的保护膜，其特征在于，制备原料以重量份计包括：多元醇聚合物70-90份，抗氧化剂0.1-0.5份，催化剂0.01-0.3份，丙烯酸单体1-15份，引发剂0.8-6份，固化剂10-30份；
所述多元醇聚合物选自聚酯多元醇；所述聚酯多元醇为聚酯二元醇；所述聚酯二元醇的数均分子量为2000-6000；
所述聚酯二元醇为无定型聚酯羟值含量为18-112mgKOH/g的结晶型聚酯二元醇和羟值含量为27-56mgKOH/g的聚酯二元醇，其中结晶聚酯含量大于30重量份。
2.根据权利要求1所述生产线快速固化的保护膜，其特征在于，所述丙烯酸单体为含羟基的丙烯酸单体，选自丙烯酸羟乙酯、丙烯酸羟丙酯、甲基丙烯酸羟乙酯中的一种或几种的组合。
3.根据权利要求1所述生产线快速固化的保护膜，其特征在于，所述固化剂为异氰酸酯固化剂，所述异氰酸酯固化剂选自脂肪族异氰酸酯或芳香族异氰酸酯中的一种。
4.根据权利要求1所述生产线快速固化的保护膜，其特征在于，所述引发剂为光引发剂，选自烷基苯酮类引发剂、酰基磷氧化物类引发剂、苯偶酰类引发剂、二苯甲酮类引发剂中的一种或几种的组合。
5.根据权利要求1所述生产线快速固化的保护膜，其特征在于，所述保护膜的涂布方式选自喷涂、辊涂、刮涂方式中的一种或组合。
6.根据权利要求1所述生产线快速固化的保护膜，其特征在于，所述保护膜的涂布温度为25-150℃。
7.一种根据权利要求1-6任一项所述生产线快速固化的保护膜的应用，其特征在于，应用于玻璃、铝板、铜板、不锈钢板、芯片、PCB板的涂布保护中。
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