CN113291010A - 一种免维护透明薄膜、制备方法及其用途 - Google Patents
一种免维护透明薄膜、制备方法及其用途 Download PDFInfo
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- CN113291010A CN113291010A CN202110522649.XA CN202110522649A CN113291010A CN 113291010 A CN113291010 A CN 113291010A CN 202110522649 A CN202110522649 A CN 202110522649A CN 113291010 A CN113291010 A CN 113291010A
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- fluoroplastic
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Abstract
本发明公开了一种免维护透明薄膜、制备方法及其用途，包括：功能层，以及两层氟塑料透明层；氟塑料透明层设于功能层的两侧，以增大透明薄膜外表面的水接触角；功能层的原料包括：氟塑料、功能添加剂、以及分散剂；氟塑料为50‑65质量份，功能添加剂为5‑10质量份，分散剂为30‑40质量份；其中，功能添加剂包括：无机纳米粒子；分散剂用于将功能添加剂均匀分散于氟塑料中；分散剂为四氟乙烯‑六氟丙烯‑偏氟乙烯共聚物。氟塑料的耐沾污性、不燃性等特性赋予薄膜优良的自清洁能力和阻燃优点。本发明以氟塑料为基材，通过分散剂四氟乙烯‑六氟丙烯‑偏氟乙烯共聚物(THV)将功能添加剂均匀分散于薄膜中间层中，通过三层共挤工艺制得一种免维护透明薄膜。
Description
技术领域
本发明涉及功能薄膜领域，具体涉及一种免维护透明薄膜、制备方法及其用途。
背景技术
随着汽车窗膜的广泛运用，消费者对于提高汽车窗膜防紫外现象的需求越来越大。市场上现有的汽车窗膜普遍采用的基底材料选自聚对苯二甲酸乙二醇酯(PET)、尼龙(PA)、聚碳酸酯(PC)或透明亚克力，但这几种材料不仅耐候性差，而且其透光率小于玻璃，贴附于玻璃上后会影响室内采光，此外，经过长时间使用后薄膜也会产生不同程度的黄变现象，进而影响到薄膜的透光率，影响客户的使用感受。CN110576579发明公开了一种汽车后档用隔热抗紫外黑色透明薄膜及其制备工艺，其采用PET材料，通过三层熔融共挤制备了具有隔热抗紫外的黑色透明膜；CN106381472发明公开了一种用于通航飞机座舱玻璃的防紫外节能疏水薄膜，其采用有机玻璃基底和各种功能涂层实现了防紫外疏水透明的效果，以上两个专利制备工艺复杂、材料耐候性差，产生的废旧塑料会加重环境负担。
紫外光/红外光功能添加剂因其小尺寸效应、表面与界面效应、量子尺寸效应和宏观量子隧道效应等特性受到人们的广泛关注。利用无机纳米材料与聚合物基体之间的相互作用产生新的效应，实现两者之间的优势互补，开发性能优异的材料，已成为当前研究的重要方向之一。
有机相和无机相之间界面的强度是聚合物基体复合材料性能最重要的决定因素。但由于功能添加剂具有高的表面能，易于团聚，与有机基体的相容性差，难以均匀分散在基体中，直接或过多的填充，往往容易导致材料的性能下降。专利CN108034400A、CN108300402A分别公开了一种含超细滑石粉的聚氨酯乳液胶黏剂和一种含纳米二氧化硅的水性聚氨酯乳液胶黏剂及其制备方法，专利CN107868441A采用在最终制备的水性聚氨酯乳液中机械混合纳米二氧化硅来提高水性聚氨酯的各项性能。虽然随着功能添加剂粒径的减少，可提高产品的各项性能。但同时纳米粒子比表面积更大、表面能更高，更易团聚，阻碍分子链的运动；另外纳米粒子与聚合物在化学结构和物理形态上有着很大的差异，亲和性差，相容性差，存在相分离现象。而通过对纳米粒子的表面处理可改善纳米粒子的均匀分散性。硅烷偶联剂是一种重要的表面处理剂，它的分子中同时具有能与无机材料结合的反应性基团和与有机材料结合的反应性基团，通过硅烷偶联剂可使两种性能差异很大的材料界面偶联起来。
此外，市场上大多隔热、防紫外、疏水薄膜通常需要进行蒸镀工艺处理，造成工艺复杂，成本较高，且功能层经过一定时间使用后也会产生不同程度的脱落现象。氟塑料是指一种含氟的树脂，主要包括ETFE(乙烯-四氟乙烯)、ECTFE(乙烯-氯化氟乙烯)、FEP(聚全氟乙丙烯)、PCTFE(聚氯化氟乙烯)、PFA(聚四氟乙烯-全氟烷基乙烯基醚)，鉴于氟塑料中氟碳建高达485KJ/mol，因此氟塑料薄膜具有优良的耐沾污性、疏水性、耐热性、耐候性、阻燃性、耐化学性，因此氟塑料逐渐在化工、半导体、LED、建筑领域受到越来越多的关注。但是氟塑料的改性，尤其是纳米粒子在氟塑料中的分散技术在国内研究较少，这限制了氟塑料的应用范围。
发明内容
本发明的目的是为了解决上述问题，提供一种免维护透明薄膜、制备方法及其用途。
为了达到上述目的，本发明提供了一种免维护透明薄膜，所述透明薄膜包括：功能层，以及两层氟塑料透明层；所述氟塑料透明层设于所述功能层的两侧，以增大所述透明薄膜外表面的水接触角；所述功能层的原料包括：氟塑料、功能添加剂、以及分散剂；所述氟塑料为50-65质量份，所述功能添加剂为5-10质量份，所述分散剂为30-40质量份；其中，所述功能添加剂包括：无机纳米粒子；所述分散剂用于将所述功能添加剂均匀分散于所述氟塑料中；所述分散剂为四氟乙烯-六氟丙烯-偏氟乙烯共聚物。
可选的，所述无机纳米粒子包括：紫外光吸收剂和/或红外光吸收剂；所述紫外光吸收剂包括：二氧化钛、三嗪类衍生物中的一种或多种；所述红外光吸收剂包括：掺锑二氧化锡、氧化铈、二萘嵌苯类衍生物中的一种或多种。
可选的，所述氟塑料包括：乙烯-四氟乙烯共聚物、乙烯-三氟氯乙烯共聚物、全氟乙烯丙烯共聚物、聚氯三氟乙烯中的一种或多种。
可选的，所述功能添加剂还包括：表面处理剂，所述表面处理剂占所述功能添加剂质量的2％-10％。
可选的，所述表面处理剂为全氟硅烷偶联剂。
可选的，所述免维护透明薄膜用作窗膜。
本发明还提供了一种免维护透明薄膜的制备方法，包括以下步骤：
步骤1：对所述无机纳米粒子进行表面处理，然后将处理后的无机纳米粒子烘干形成颗粒；
步骤2：使用800目滤网过滤步骤1得到的颗粒，得到功能添加剂细品，通过双螺杆挤出机将所述功能添加剂细品、分散剂、氟塑料按比例混匀，得到分散均匀的功能层粒子；
步骤3：将氟塑料、步骤2得到的功能层粒子加入三层共挤流延机中，得到所述免维护透明薄膜。
可选的，所述步骤1中，对无机纳米粒子进行表面处理的方法包括：采用沸腾造粒工艺将表面处理剂包覆于无机纳米粒子表面。
可选的，所述双螺杆挤出机的长径比为32，压缩比为3.1，工艺温度设置为220℃-280℃。
相比于现有技术，本发明的有益效果为：
(1)本发明的免维护透明薄膜以四氟乙烯-六氟丙烯-偏氟乙烯共聚物(THV)为分散剂，能够使包含无机纳米粒子的功能添加剂更容易在氟塑料基材中分散，从而提高薄膜的性能，以此制得一种免维护透明薄膜；
(2)本发明的功能添加剂包括紫外光吸收剂、红外光吸收剂等无机纳米粒子，通过紫外光吸收剂、红外光吸收剂对氟塑料进行改性，可以制得一种防紫外隔热透明薄膜；
(3)本发明的免维护透明薄膜采用三层共挤流延工艺制备，不需要蒸镀工艺，不存在功能层脱落的问题；
(4)本发明的免维护透明薄膜的基材为含氟塑料，具有优良的耐沾污特性，室外条件下，雨水冲洗即可清洗薄膜表面，且在整个薄膜使用寿命内均不需要额外清洗，免清洗费，使用成本低。
附图说明
图1为本发明实施例中免维护透明薄膜的结构示意图。
图中：1-氟塑料透明层，2-功能层。
具体实施方式
以下结合附图和实施例对本发明的技术方案做进一步的说明。
如图1所示，本发明提供了一种免维护透明薄膜，所述透明薄膜由功能层2及两层氟塑料透明层1构成，氟塑料透明层1设于功能层2的两侧，以增大所述透明薄膜外表面的水接触角；所述功能层2的原料包括：以质量百分数计的50％-65％的氟塑料、5％-10％的功能添加剂、30％-40％的分散剂；其中，所述功能添加剂包含无机纳米粒子，所述分散剂用于将所述功能添加剂均匀分散于所述氟塑料中；所述分散剂为四氟乙烯-六氟丙烯-偏氟乙烯共聚物。
其中，上述氟塑料透明层1，以及功能层2使用的氟塑料均由熔融指数为5-30g/10min的氟塑料制成。现有技术中，有机相和无机相之间界面的强度是聚合物基体复合材料性能最重要的决定因素。但由于无机功能添加剂具有高的表面能，易于团聚，与有机基体的相容性差，难以均匀分散在基体中，直接或过多的填充，往往容易导致材料的性能下降。氟塑料的碳氟键化学键键能高达485KJ/mol，导致其表面能很低，难以与其它化合物反应，因此功能添加剂很难均匀的分散于氟塑料中，难于制备薄膜。常规分散剂无法与氟塑料相融，在氟塑料加工温度时易产生降解。四氟乙烯-六氟丙烯-偏氟乙烯共聚物(THV)的分解温度大于400℃，且与氟塑料有良好的相容性，申请人首次以此作为分散剂制得一种免维护透明薄膜。
本发明的氟塑料透明层1呈透明状，占整个透明薄膜厚度的20％-40％，功能层2占整个透明薄膜厚度的60％-80％，整个透明薄膜的总厚度为50-500μm。本发明的免维护透明薄膜尤其适用于作为窗膜，其表面水接触角较大，基本不需要额外清洗，减少了使用过程中的清洗费，使用成本较低。
一些实施例中，所述氟塑料为乙烯-四氟乙烯共聚物(ETFE)、乙烯-三氟氯乙烯共聚物(ECTFE)、全氟乙烯丙烯共聚物(FEP)、聚氯三氟乙烯(PCTFE)中的一种或多种；所述氟塑料呈固态粒子状，与PET、PA等材料相比，其具有优异的化学稳定性、耐候性、防粘性、疏水性。
一些实施例中，所述无机纳米粒子包括：紫外光吸收剂/红外光吸收剂，其用于对所述氟塑料进行改性，以使所述功能层2能够吸收紫外线或红外线。
一些实施例中，紫外光吸收剂选自：二氧化钛、三嗪类衍生物中的一种或多种，红外光吸收剂选自：掺锑二氧化锡、氧化铈、二萘嵌苯类衍生物中的一种或多种。
优选的，上述紫外光吸收剂与红外光吸收剂的添加比例为1:1-2。
优选的，上述紫外光吸收剂与红外光吸收剂的粒径大小为100nm-1000nm。
优选的，所述功能添加剂还包括：表面处理剂，所述表面处理剂为含氟硅烷偶联剂，其占所述功能添加剂的2％-10％，分子内氟原子数大于10，分子量大于300，物理形态为液态，表面处理剂配置成溶液后一方面利于表面处理剂均匀的与无机纳米粒子接触，另一方面表面处理剂溶液挥发后会与无机纳米粒子表面通过氢键等物理作用力结合在一起，从而利于无机纳米粒子在氟塑料中分散分布。本发明以全氟硅烷偶联剂(全氟癸基三乙氧基硅烷、全氟癸基三甲氧基硅烷)作为实施例。
上述免维护透明薄膜通过以下方法进行制备：
步骤1：对所述无机纳米粒子进行表面处理，然后将处理后的无机纳米粒子烘干形成颗粒；
步骤2：使用800目滤网过滤步骤1得到的颗粒，得到功能添加剂细品，通过双螺杆挤出机将所述功能添加剂细品、分散剂、氟塑料按比例混匀，得到分散均匀的功能层粒子；
步骤3：将氟塑料、步骤2得到的功能层粒子加入三层共挤流延机中，得到所述免维护透明薄膜。
实施例1
本实施例提供了一种免维护透明薄膜，所述功能层由50质量份的氟塑料、10质量份的功能添加剂、40质量份的分散剂制成；上述的功能添加剂为全氟癸基三乙氧基硅烷处理好的二氧化钛、氧化铈；上述的分散剂为四氟乙烯-六氟丙烯-偏氟乙烯共聚物(THV)。
所述免维护透明薄膜通过三层共挤流延工艺制备，其制备方法如下：
步骤1：首先称取500g全氟癸基三甲氧基硅烷，然后将500g全氟癸基三甲氧基硅烷超声分散到乙醇中配置成浓度为2％的溶液，再称取5Kg平均粒径为100nm的紫外光/红外光吸收剂，其中纳米氧化铈为2.5Kg，纳米二氧化钛为2.5Kg，采用沸腾造粒工艺将全氟癸基三甲氧基硅烷溶液与无机纳米粒子混合均匀，最后将混合均匀的粒子置于烘箱中在80℃条件下烘1h，通过800目过滤网获得全氟癸基三甲氧基硅烷处理过的纳米功能粒子。
步骤2：首先将30Kg的四氟乙烯-六氟丙烯-偏氟乙烯共聚物(THV)和步骤1得到的纳米功能粒子置于高混机内分别在1000r/min和3000r/min条件下各混合10min和3min，然后将混合物料与65Kg的ETFE粉末于高混机内在3000r/min条件下混合5min而得到混合均匀的共混料。
步骤3：将步骤2获得的共混料投入到双螺杆挤出机内，进行共混造粒，其中挤出机长径比为32，压缩比为3.1，工艺温度设置为220℃-280℃。
步骤4：将氟塑料透明层1的ETFE粒子通过吸料系统投入单螺杆挤出机Ⅰ和单螺杆挤出机Ⅲ的料仓中、将步骤2得到的共混料投入单螺杆挤出机Ⅱ的料仓中，启动加热装置使模具和挤出机预热30min，预热温度为300℃-350℃；达到工艺温度后，在压力作用下将得到的熔融体经过挤出机的T型模口共流延挤出，通过牵引辊引流到冷却辊上快速骤冷，同时经过气刀的辅助冷却和压紧，形成表面平整薄膜，通过红外线薄膜测厚仪实时监测薄膜厚度，制得所述免维护透明薄膜。
其中，T型模口温度设置为350℃，冷却辊温度为110℃，单螺杆挤出机的螺杆长径比为28，压缩比为3.1，温度设置为330℃-350℃。制得的免维护透明薄膜厚度为50μm，氟塑料透明层1的厚度为5μm，功能层2的厚度为40μm。
实施例2
实施例2与实施例1的区别在于：
功能层2由65质量份的氟塑料、5质量份的功能添加剂、30质量份的分散剂组成。
实施例3
实施例3与实施例1的区别在于：
功能层2由60质量份的氟塑料、7质量份的功能添加剂、33质量份的分散剂组成。
对比例1
本对比例与实施例1的区别在于：
对比例1将实施例1功能层2中的分散剂替换为聚四氟乙烯微粉和乙撑基双硬脂酰胺。
对比例2
对比例2与实施例1的区别在于：
对比例2将实施例1功能层2中的分散剂替换为低密度聚乙烯蜡。
对比例3
对比例3与实施例1的区别在于：
对比例3将实施例1氟塑料透明层1的材料替换为尼龙。
对比例4
对比例4与实施例1的区别在于：
对比例4将实施例1氟塑料透明层1的材料替换为聚对苯二甲酸乙二醇酯。
根据以下方法对实施例1-3和对比例1-2进行性能检测，结果如下表所示：
实施例1-3与对比例1-4的性能检测表
1.光学性能测试：采用深圳市林上科技有限公司生产的太阳膜透光率测试仪(型号LS182)，参照ASTM D1003标准方法进行；
2.水接触角测试：采用晟鼎接触角测量仪(型号ZT-705SB)进行薄膜水接触角角度的检测，参照说明书方法进行；
3.耐候性测试：采用色差测试仪测试薄膜的b1值，然后将其置于UVA@340nm荧光灯测试照射120Kwh/m2，最后再次用色差测试仪测试薄膜的b2值，b2与b1相减得到薄膜的黄变值；
4.可见光保持率：先通过分光光度计测试薄膜在400nm-800nm间的透过率R1，然后将样品置于氙灯老化实验箱内进行照射1000h，最后通过分光光度计测试薄膜在400nm-800nm间的透过率R2，计算R2/R1即为可见光保持率。
综上所述，本发明通过四氟乙烯-六氟丙烯-偏氟乙烯共聚物(THV)和表面活性剂将无机纳米粒子分散于氟塑料内，对含氟塑料进行共混改性，最后通过共挤工艺制得一种免维护透明薄膜。
尽管本发明的内容已经通过上述优选实施例作了详细介绍，但应当认识到上述的描述不应被认为是对本发明的限制。在本领域技术人员阅读了上述内容后，对于本发明的多种修改和替代都将是显而易见的。因此，本发明的保护范围应由所附的权利要求来限定。
Claims (9)
1.一种免维护透明薄膜，其特征在于，所述免维护透明薄膜包括：
功能层，以及两层氟塑料透明层；所述氟塑料透明层设于所述功能层的两侧，以增大所述透明薄膜外表面的水接触角；所述功能层的原料包括：氟塑料、功能添加剂、以及分散剂；所述氟塑料为50-65质量份，所述功能添加剂为5-10质量份，所述分散剂为30-40质量份；
其中，所述功能添加剂包括：无机纳米粒子；所述分散剂用于将所述功能添加剂均匀分散于所述氟塑料中；所述分散剂为四氟乙烯-六氟丙烯-偏氟乙烯共聚物。
2.如权利要求1所述的免维护透明薄膜，其特征在于，所述无机纳米粒子包括：紫外光吸收剂和/或红外光吸收剂；所述紫外光吸收剂包括：二氧化钛、三嗪类衍生物中的一种或多种；所述红外光吸收剂包括：掺锑二氧化锡、氧化铈、二萘嵌苯类衍生物中的一种或多种。
3.如权利要求1所述的免维护透明薄膜，其特征在于，所述氟塑料包括：乙烯-四氟乙烯共聚物、乙烯-三氟氯乙烯共聚物、全氟乙烯丙烯共聚物、聚氯三氟乙烯中的一种或多种。
4.如权利要求1所述的免维护透明薄膜，其特征在于，所述功能添加剂还包括：表面处理剂，所述表面处理剂占所述功能添加剂质量的2％-10％。
5.如权利要求4所述的免维护透明薄膜，其特征在于，所述表面处理剂为全氟硅烷偶联剂。
6.如权利要求1-5任意一项所述的免维护透明薄膜的用途，其特征在于，所述免维护透明薄膜用作窗膜。
7.如权利要求1-5任意一项所述的免维护透明薄膜的制备方法，其特征在于，包括以下步骤：
步骤1：对所述无机纳米粒子进行表面处理，然后将处理后的无机纳米粒子烘干形成颗粒；
步骤2：使用800目滤网过滤步骤1得到的颗粒，得到功能添加剂细品，通过双螺杆挤出机将所述功能添加剂细品、分散剂、氟塑料按比例混匀，得到分散均匀的功能层粒子；
步骤3：将氟塑料、步骤2得到的功能层粒子加入三层共挤流延机中，得到所述免维护透明薄膜。
8.如权利要求7所述的免维护透明薄膜的制备方法，其特征在于，所述步骤1中，对无机纳米粒子进行表面处理的方法包括：采用沸腾造粒工艺将表面处理剂包覆于无机纳米粒子表面。
9.如权利要求7所述的免维护透明薄膜的制备方法，其特征在于，所述双螺杆挤出机的长径比为32，压缩比为3.1，工艺温度设置为220℃-280℃。
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