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CN108329501A - 一种热稳定聚酯片材的制备方法 - Google Patents

一种热稳定聚酯片材的制备方法 Download PDF

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CN108329501A
CN108329501A CN201810095053.4A CN201810095053A CN108329501A CN 108329501 A CN108329501 A CN 108329501A CN 201810095053 A CN201810095053 A CN 201810095053A CN 108329501 A CN108329501 A CN 108329501A
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何建锋
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Suzhou Villa Electronics Technology Co Ltd
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Abstract

本发明涉及一种耐用性高、生产简单且性价比高的热稳定聚酯片材的制备方法。该方法包括以下步骤：热稳定聚丙烯酸酯溶液的制备、辅助助剂加入聚丙烯酸酯溶液制成热稳定涂层液、将热稳定涂层液辊涂在聚酯片材上形成热稳定膜。本发明在聚酯片材表面涂覆含有热稳定剂的聚丙烯酸酯膜，使热稳定剂与聚酯片材的结合牢度得到提高，从而使聚酯片材热稳定的持久时间得到了延长，耐用性得到了提高。同时聚丙烯酸酯膜手感与聚酯膜相似、价格较低廉，制备工艺简单，无毒环保，有利于节省成本和资源。

Description

一种热稳定聚酯片材的制备方法
技术领域
本发明涉及聚酯片材领域，尤其涉及一种热稳定聚酯片材的制备方法。
背景技术
聚酯片材（PET）以聚对苯二甲酸乙二酯为主要原料，是一种具有优良的电绝缘性能、耐气候性、耐弱酸性和耐油性、无毒性、抗化学药品稳定性、加工性的材料。聚酯片材因具有诸多优点而被作为各类纺织品、精密仪器、电器元件的高档包装材料；录音带、录像带、电影胶片、计算机软盘、金属镀膜及感光胶片等的基材，也应用于电气绝缘材料、电容器膜、柔性印刷电路板及片材开关等电子领域和机械领域。随着应用的越来越广泛，聚酯片材热稳定性的问题日益突出。
聚酯材料耐高温性较差，工作温度一高就会出现软化变形的问题，从而限制了其使用范围。传统的方法是将热稳定剂做成溶液涂覆于基材表面再烘干，或者直接加入基材中。后者成本较高且存在相容性、稳定性的问题，前者由于其简单易行，在实际成产中应用较多。但是将热稳定剂溶解或者稀释后再涂覆于基材表面，助剂和基材的结合牢度较低、耐用性较差。因此提供一种耐用性高、生产简单且性价比高的热稳定聚酯片材的制备方法是本发明所要解决的问题。
发明内容
本发明克服了现有技术的不足，提供了一种耐用性高、生产简单且性价比高的热稳定聚酯片材的制备方法。
为达到上述目的，本发明采用的技术方案为：提供了一种热稳定聚酯片材的制备方法，特征在于，包括以下步骤：
（1）热稳定聚丙烯酸酯溶液的制备：
将丙烯酸甲酯39.5-45质量份，丙烯酸-2-羟乙酯19.5-24.5质量份，丙烯酸正丁酯20.5-24.5质量份，甲基丙烯酸12.5-15质量份称量后混合均匀得到混合反应单体；称量混合反应单体100质量份、乳化剂4-7.5质量份、引发剂0.15-0.55质量份和热稳定剂0.25-1.5质量份；反应釜中通入水并升温，依次加入乳化剂和1/5（质量）引发剂；温度在80-85℃时滴加混合反应单体以及4/5（质量）引发剂并继续升温；2-5h滴加完成，在87-92℃时恒温反应2-3.5h；降温，在温度为35-55℃时加入热稳定剂，保温1-2h，之后降温至常温得到成品，固含量控制在25-30%（质量百分数）；
（2）热稳定涂层液的制备：
取热稳定聚丙烯酸酯溶液100质量份，加入容器中以转速为120-180rpm搅拌，逐次加入消泡剂2.5-4.5质量份以及流平剂1.5-2.5质量份，搅拌45-80min，温度控制在25-45℃；
（3）热稳定涂层的形成：
将所述热稳定涂层液涂覆到聚酯片材的两侧，烘干，控制涂层厚度为100-150nm。
作为一种优选方案，所述热稳定涂层液涂覆到聚酯片材的涂覆方式为辊涂。
作为一种更优选方案，所述辊涂方式为：将热稳定涂层液加到聚酯片材表面，之后聚酯片材以平幅状态恒速通过挤压辊，所述挤压辊给聚酯片材施加一定压力。
作为一种更优选方案，所述聚酯片材通过挤压辊的速度为12-24m/min，所述挤压辊给聚酯片材施加的压力为0.5-2kg。
作为一种优选方案，所述热稳定涂层液涂覆到聚酯片材的两侧后向涂层中加入异佛尔酮二异氰酸酯。
作为一种更优选方案，所述热稳定涂层液和异佛尔酮二异氰酸酯质量比为6：0.8-1.2。
作为一种更优选方案，所述热稳定涂层液烘干温度为100-110℃，烘干时间为50-90min。
作为一种优选方案，所述乳化剂为AEO-9和SDS的组合，AEO-9与SDS的质量比为2：1；引发剂为过硫酸钠。
作为一种更优选方案，所述乳化剂加入温度控制在35-55℃，所述1/5（质量）引发剂加入温度控制在78-82℃。
作为一种更优选方案，所述热稳定剂为烷基磷酸二酯或磷酸三甲酯的一种或两种。
本发明的有益技术效果在于：提供了一种耐用性高、生产简单且性价比高的热稳定聚酯片材的制备方法。在聚酯片材表面涂覆含有热稳定剂的聚丙烯酸酯膜，提高了热稳定剂与聚酯片材的结合牢度，从而使聚酯片材热稳定性的持久时间得到了延长，耐用性得到了提高。同时聚丙烯酸酯膜手感与聚酯膜相似、价格较低廉，制备工艺简单，无毒环保，有利于节省成本和资源。
具体实施方式
下面结合具体实施例对本发明作进一步描述。以下实施例仅用于更加清楚地说明本发明的技术方案，而不能以此来限制本发明的保护范围。
实施例1
本发明提供了一种热稳定聚酯片材的制备方法，步骤如下：
（1）将丙烯酸甲酯43质量份，丙烯酸-2-羟乙酯20质量份，丙烯酸正丁酯24.5质量份，甲基丙烯酸12.5质量份称量后混合均匀得到混合反应单体；称量混合反应单体100质量份、乳化剂AEO-9与SDS的组合（质量比2：1）6质量份、引发剂过硫酸钠0.3质量份、烷基磷酸二酯0.5质量份和磷酸三甲酯0.5质量份；反应釜中通入水并升温，在35℃时加入AEO-9与SDS的组合（质量比2：1），在78℃时加入1/5（质量）过硫酸钠；当升温至82℃时滴加混合反应单体以及4/5（质量）过硫酸钠并继续升温；4h滴加完成，在87℃时恒温反应3.5h；降温，在温度为55℃时加入烷基磷酸二酯和磷酸三甲酯，保温2h，之后降温至常温得到热稳定聚丙烯酸酯溶液成品，固含量为25.2%（质量百分数）。
（2）取热稳定聚丙烯酸酯溶液100质量份，加入容器中以转速为160rpm搅拌，逐次加入、消泡剂4.5质量份，流平剂2.5质量份，搅拌60min，得到热稳定涂层液，温度控制在45℃。
（3）将所述热稳定涂层液涂覆到聚酯片材的两侧，涂覆方式为辊涂。即将热稳定涂层液加到聚酯片材表面，之后聚酯片材以平幅状态，以18m/min通过挤压辊，挤压辊给聚酯片材施加1kg压力。涂布后向热稳定涂层中加入异佛尔酮二异氰酸酯，加入量为热稳定涂层液和异佛尔酮二异氰酸酯质量比为6：1。在105℃条件下烘干90min，得到热稳定聚酯片材，控制涂层厚度为120nm。
实施例2
本发明提供了一种热稳定聚酯片材的制备方法，步骤如下：
（1）将丙烯酸甲酯39.5质量份，丙烯酸-2-羟乙酯24.5质量份，丙烯酸正丁酯22质量份，丙烯酸14质量份称量后混合均匀得到混合反应单体；称量混合反应单体100质量份、乳化剂AEO-9与SDS的组合（质量比2：1）4质量份、引发剂过硫酸钠0.15质量份和烷基磷酸二酯0.25质量份；反应釜中通入水并升温，在45℃时加入AEO-9与SDS的组合（质量比2：1），在80℃时加入1/5（质量）过硫酸钠，之后滴加混合反应单体以及4/5（质量）过硫酸钠并继续升温；2h滴加完成，在92℃时恒温反应3h；降温，在温度为44℃时加入烷基磷酸二酯，保温1.5h，之后降温至常温得到热稳定聚丙烯酸酯溶液成品，固含量为29.5%（质量百分数）。
（2）取热稳定聚丙烯酸酯溶液100质量份，加入容器中以转速为120rpm搅拌，逐次加入消泡剂2.5质量份，流平剂2.5质量份搅拌80min，得到热稳定涂层液，温度控制在38℃。
（3）将所述热稳定涂层液涂覆到聚酯片材的两侧，涂覆方式为辊涂。即将热稳定涂层液加到聚酯片材表面，之后聚酯片材以平幅状态，以12m/min通过挤压辊，挤压辊给聚酯片材施加2kg压力。该步骤有利于热稳定涂层液在聚酯片材上均匀涂布。涂布后向热稳定涂层中加入异佛尔酮二异氰酸酯，加入量为热稳定涂层液和异佛尔酮二异氰酸酯质量比为7.5：1。该步骤的目的在于加快热稳定涂层的固化。加入异佛尔酮二异氰酸酯后，在110℃条件下烘干50min，得到热稳定聚酯片材，控制涂层厚度为100nm。
实施例3
本发明提供了一种热稳定聚酯片材的制备方法，步骤如下：
（1）将丙烯酸甲酯45质量份，丙烯酸-2-羟乙酯19.5质量份，丙烯酸正丁酯20.5质量份，甲基丙烯酸15质量份称量后混合均匀得到混合反应单体；称量混合反应单体100质量份、乳化剂AEO-9与SDS的组合（质量比2：1）7.5质量份、引发剂过硫酸钠0.55质量份和磷酸三甲酯1.5质量份；反应釜中通入水并升温，在55℃时加入AEO-9与SDS的组合，在82℃时加入1/5（质量）过硫酸钠；当升温至85℃时滴加混合反应单体以及4/5（质量）过硫酸钠并继续升温；5h滴加完成，在92℃时恒温反应2h；降温，在温度为35℃时加入磷酸三甲酯，保温1h，之后降温至常温得到热稳定聚丙烯酸酯溶液成品，固含量为24.1%（质量百分数）。
（2）取热稳定聚丙烯酸酯溶液100质量份，加入容器中以转速为180rpm搅拌，逐次加入，消泡剂3.5质量份，流平剂1.5质量份，搅拌45min，得到热稳定涂层液，温度控制在25℃。
（3）将所述热稳定涂层液涂覆到聚酯片材的两侧，涂覆方式为辊涂。即将热稳定涂层液加到聚酯片材表面，之后聚酯片材以平幅状态，以24m/min通过挤压辊，挤压辊给聚酯片材施加0.5kg压力。涂布后向热稳定涂层中加入异佛尔酮二异氰酸酯，加入量为热稳定涂层液和异佛尔酮二异氰酸酯质量比为5：1。在100℃条件下烘干70min，得到热稳定聚酯片材，控制涂层厚度为150nm。
以上依据本发明的理想实施例为启示，通过上述的说明内容，相关人员完全可以在不偏离本项发明技术思想的范围内，进行多样的变更以及修改。本项发明的技术性范围并不局限于说明书上的内容，必须要根据权利要求范围来确定技术性范围。

Claims (10)

1.一种热稳定聚酯片材的制备方法，特征在于，包括以下步骤：
（1）热稳定聚丙烯酸酯溶液的制备：
将丙烯酸甲酯39.5-45质量份，丙烯酸-2-羟乙酯19.5-24.5质量份，丙烯酸正丁酯20.5-24.5质量份，甲基丙烯酸12.5-15质量份称量后混合均匀得到混合反应单体；称量混合反应单体100质量份、乳化剂4-7.5质量份、引发剂0.15-0.55质量份和热稳定剂0.25-1.5质量份；反应釜中通入水并升温，依次加入乳化剂和1/5（质量）引发剂；温度在80-85℃时滴加混合反应单体以及4/5（质量）引发剂并继续升温；2-5h滴加完成，在87-92℃时恒温反应2-3.5h；降温，在温度为35-55℃时加入热稳定剂，保温1-2h，之后降温至常温得到成品，固含量控制在25-30%（质量百分数）；
（2）热稳定涂层液的制备：
取热稳定聚丙烯酸酯溶液100质量份，加入容器中以转速为120-180rpm搅拌，逐次加入消泡剂2.5-4.5质量份以及流平剂1.5-2.5质量份，搅拌45-80min，温度控制在25-45℃；
（3）热稳定涂层的形成：
将所述热稳定涂层液涂覆到聚酯片材的两侧，烘干，控制涂层厚度为100-150nm。
2.根据权利要求1所述的热稳定聚酯片材的制备方法，其特征在于：所述热稳定涂层液涂覆到聚酯片材的涂覆方式为辊涂。
3.根据权利要求2所述的热稳定聚酯片材的制备方法，其特征在于：所述辊涂方式为：将热稳定涂层液加到聚酯片材表面，之后聚酯片材以平幅状态恒速通过挤压辊，所述挤压辊给聚酯片材施加一定压力。
4.根据权利要求3所述的热稳定聚酯片材的制备方法，其特征在于：所述聚酯片材通过挤压辊的速度为12-24m/min，所述挤压辊给聚酯片材施加的压力为0.5-2kg。
5.根据权利要求1所述的热稳定聚酯片材的制备方法，其特征在于：所述热稳定涂层液涂覆到聚酯片材的两侧后向涂层中加入异佛尔酮二异氰酸酯。
6.根据权利要求5所述的热稳定聚酯片材的制备方法，其特征在于：所述热稳定涂层液和异佛尔酮二异氰酸酯质量比为6：0.8-1.2。
7.根据权利要求6所述的热稳定聚酯片材的制备方法，其特征在于：所述热稳定涂层液烘干温度为100-110℃，烘干时间为50-90min。
8.根据权利要求1-7任一所述的热稳定聚酯片材的制备方法，其特征在于：所述乳化剂为AEO-9和SDS的组合，AEO-9与SDS的质量比为2：1；引发剂为过硫酸钠。
9.根据权利要求8所述的热稳定聚酯片材的制备方法，其特征在于：所述乳化剂加入温度控制在35-55℃，所述1/5（质量）引发剂加入温度控制在78-82℃。
10.根据权利要求9所述的热稳定聚酯片材的制备方法，其特征在于：所述热稳定剂为烷基磷酸二酯或磷酸三甲酯的一种或两种。
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