CN114423605A - 具有耐霜性的疏水膜及其制造方法 - Google Patents

具有耐霜性的疏水膜及其制造方法 Download PDF

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Publication number
CN114423605A
CN114423605A CN202080066583.1A CN202080066583A CN114423605A CN 114423605 A CN114423605 A CN 114423605A CN 202080066583 A CN202080066583 A CN 202080066583A CN 114423605 A CN114423605 A CN 114423605A
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China
Prior art keywords
hydrophobic
layer
film
moisture absorption
substrate
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CN202080066583.1A
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Inventor
白鸟世明
中村浩贵
大川新太朗
安藤宏明
北元美贵
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Toyoda Gosei Co Ltd
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Toyoda Gosei Co Ltd
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Publication of CN114423605A publication Critical patent/CN114423605A/zh
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Abstract

一种具有耐霜性的疏水膜(1)，包括：设置在基板(3)上的吸湿层(5)、以及设置在吸湿层(5)上的疏水层(7)，其中，疏水层(7)包括疏水层基体(9)和附着在疏水层基体上的疏水性成分(11)。一种具有耐霜性的疏水膜的制造方法，包括：在对象表面上形成吸湿层的吸湿层形成步骤；以及在吸湿层上形成疏水层的疏水层形成步骤，疏水层形成步骤包括使疏水性成分附着在疏水层基体上的步骤。

Description

具有耐霜性的疏水膜及其制造方法
技术领域
本发明涉及具有耐霜性的疏水膜及其制造方法。
背景技术
在日本专利6333454号公报中记载了具有与氟烷基硅烷键合的亲水凝胶型二氧化硅粉末的疏水/疏油涂层。
在日本特开2009-073877号公报中记载了具有防霜效果的固体多元醇类组合物。
现有技术文献
专利文献
专利文献1：日本专利6333454号公报
专利文献2：日本特开2009-073877号公报
发明内容
发明所要解决的课题
疏水膜存在对霜的耐性低的问题。
因此，本说明书中所记载的发明之一的目的在于，提供一种具有耐霜性的疏水膜及其制造方法。
此外，本说明书中所记载的发明之一的目的在于，提供一种同时具有防止积雪附着和防止结霜两者的特性的膜及其制造方法。
用于解决课题的方案
本发明基本上是基于这样的实施例：由于采用了疏水性多孔层和吸湿层2层结构，因此可以获得具有耐霜性的疏水膜。
本说明书中所公开的第一个发明涉及具有耐霜性的疏水膜。该膜为具有耐霜性的疏水膜1，其包括设置在基板3上的吸湿层5和设置在吸湿层5上的疏水层7。并且，疏水层7包括：疏水层基体9和附着在疏水层基体上的疏水性成分11。由于其为包括吸湿层和疏水层的2层构成，因此可以得到具有耐霜性的疏水膜。疏水性成分的例子为粒子、分子以及油层。
吸湿层5优选含有防冻液成分。通过含有防冻液成分，即使在寒冷环境下也能确保吸湿性。防冻液成分的例子包括聚二甲基硅氧烷、聚苯基甲基硅氧烷、甘油、乙二醇、聚乙二醇、丙二醇、聚乙烯醇、纤维素、丙烯酸类防冻液、以及丙烯酰胺类防冻液中的1种或2种以上。
吸湿层5优选包含：重均分子量为100以上且小于800的聚乙二醇即第1PEG；以及重均分子量为800以上2000万以下的聚乙二醇即第2PEG。并且，第1PEG与第2PEG的重量比即w1/w2优选为0.001以上1000以下。
在假想的膜的使用环境之一(寒冷地区)中，通过混合分别为液态和固态的第1PEG和第2PEG，即使在倾斜的状态下形成膜，也可以确保吸湿性而不会发生滴哒液体等。需要说明的是，当膜形成在平面上时，则不需要第2PEG。另一方面，例如，当在汽车等上形成膜时，优选将第2PEG混合到第1PEG中以防止吸湿层滴哒液体。
疏水性成分11的例子为疏水性二氧化硅粒子。疏水性成分11的另一个例子是附着在疏水层基体上的疏水性化合物。疏水性化合物为(例如)在端部具有氟原子、甲基、氟甲基、二氟甲基、三氟甲基等疏水官能团的化合物。
疏水层基体9的例子为多孔体。由于疏水层基体9的表面是多孔的，因此附着在疏水层表面的雪不能渗入内部而被除去。此外，由于疏水层基体9的表面是多孔的，因此附着在疏水层表面的水滴被吸湿层吸收，从而可以防止疏水层基体9的表面冻结。
基板3的表面的例子具有聚碳酸酯、丙烯酸树脂或甲基丙烯酸树脂。该膜与聚碳酸酯、丙烯酸树脂或甲基丙烯酸树脂的亲和性优异，因此优选用于汽车和航空器。膜的优选用途为形成在与汽车外部装饰和内部装饰相关的部件表面或航空器的机身表面。
优选的是，还包括存在于吸湿层5与疏水层7之间的间隔层13。由于有间隔层，水蒸气等可以良好地通过，因此吸湿层可以吸收附着在疏水层部分上的水分。此外，由于有间隔层，因此从吸湿层产生的水蒸气可以逸出。
间隔层的孔隙率的例子为0.1％以上99.9％以下。间隔层可以是单纯的框架或柱子。
本说明书所公开的下一个发明涉及具有耐霜性的疏水膜的制造方法。
该方法包括：在对象表面上形成吸湿层的吸湿层形成步骤；以及
在吸湿层上形成疏水层的疏水层形成步骤。并且，疏水层形成步骤包括使疏水性成分附着在疏水层基体上的步骤。
发明效果
本说明书所记载的发明之一可以提供具有耐霜性的疏水膜及其制造方法。
本说明书所记载的发明之一可以提供同时具有防止积雪附着和防止结霜两者的特性的膜及其制造方法。
附图说明
[图1]图1为示出疏水膜的构成例的示意图。
[图2]图2为示出评价实施例1和比较例1、2的过冷水的去除性能时的情形的代替附图的照片。
[图3]图3为示出评价实施例1、2以及3的防雪附着性时的情形的代替附图的照片。
具体实施方式
以下，使用附图对用于实施本发明的方式进行说明。本发明不限于以下所说明的方式，还包括本领域技术人员从以下方式中在显而易见的范围内进行适当地修改而得的方式。
图1为示出疏水膜的构成例的示意图。以下，对疏水膜进行说明。如图1所示，该膜包括：设置在基板3上的吸湿层5；以及设置在吸湿层5上的疏水层7。
基板3的表面的例子包括聚碳酸酯、丙烯酸树脂或甲基丙烯酸树脂。该膜与聚碳酸酯、丙烯酸树脂或甲基丙烯酸树脂的亲和性优异，因此优选用于汽车和航空器。膜的优选用途为形成在与汽车外部装饰和内部装饰相关的部件表面或航空器的机身表面。与汽车的外部装饰相关的部件的例子为车门、车身、车窗以及车架。与汽车的内部装饰相关的部件的例子为机柜、方向盘、踏板、齿轮及车身的内表面部分。基板自身可以是树脂，也可以是金属。另一方面，当基板为金属时，优选由包含聚碳酸酯、丙烯酸树脂或甲基丙烯酸树脂的树脂层来被覆其表面。基板可以是包括航空器框体的构成部件或包括汽车框体的构成部件。更优选的是，通过将其应用于设置在汽车外部装饰上的毫米波或LiDAR透射罩的表面，无论天气如何都可以提高传感精度。
吸湿层5是指具有吸湿性的层。吸湿层是已知的，例如，如日本专利6396872号公报所述那样。吸湿层的例子为：包含硅胶、氧化铝凝胶、分子筛、沸石以及氯化钙等已知的吸湿剂和作为分散介质的树脂的吸湿层；作为负载有吸湿剂的微孔膜的吸湿层；具有包含非晶二氧化硅、水溶性树脂以及吸湿剂的多孔结构的吸湿层。
吸湿层5优选含有防冻液成分。通过含有防冻液成分，即使在寒冷环境下也能确保吸湿性。防冻液成分的例子包括聚二甲基硅氧烷、聚苯甲基硅氧烷、甘油、乙二醇、聚乙二醇、丙二醇、聚乙烯醇、纤维素、丙烯酸类防冻液以及丙烯酰胺类防冻液中的1种或2种以上。由于这些化合物和树脂是已知的，因此适当地使用已知的树脂即可。例如，在日本专利第3299081号公报中记载有这样的防冻涂料：以重量为基准，其由250～300份水和5～10份的多元醇制成的防冻液、10～50份水溶性醋酸盐、2.0～5.0份水溶性防锈剂以及6～65份水溶性粘合剂构成。并且，在该文献中，多元醇为选自乙基乙二醇、丁基乙二醇、乙二醇、丙二醇、丁二醇、聚乙二醇、聚丙二醇、乙基二乙二醇、丁基二乙二醇、甘油、丙酰甲醇中的1种或2种以上，粘合剂为粘胶纤维、甲基纤维素、乙基纤维素、羟乙基纤维素、羧甲基纤维素、可溶性淀粉、羧甲基淀粉、二醛淀粉、聚乙烯醇、聚丙烯酸钠、聚环氧乙烷、选自水溶性醇酸树脂、水溶性三聚氰胺树脂、水溶性脲醛树脂、水溶性酚醛树脂、水溶性丙烯酸树脂、水溶性环氧树脂、水溶性聚丁二烯树脂中的1种或2种以上的树脂。作为本说明书中的防冻液成分，可以使用将上述公报中记载的多元醇和树脂进行适当地混合而得的物质。
吸湿层5优选包含：重均分子量为100以上且小于800的聚乙二醇即第1PEG；以及重均分子量为800以上2000万以下的聚乙二醇即第2PEG。
第1PEG的重均分子量可以为100以上且小于400，也可以为150以上且小于300。
特别是，第2PEG可以包含重均分子量不同的多个组。第2PEG的重均分子量的例子可以为850以上且小于2000、900以上且小于2000、950以上且小于1500，也可以为2000以上且小于50万、2500以上且小于10万、2500以上且小于1万、3000以上且小于6000，还可以为50万以上2000万以下、50万以上1000万以下、50万以上800万以下、100万以上1000万以下。
并且，第1PEG与第2PEG的重量比即w1/w2优选为0.001以上1000以下(优选的是，0.01以上500以下、0.01以上100以下、0.1以上10以下、0.01以上1000以下、0.05以上100以下、0.1以上50以下)。
在假想的膜的使用环境之一(寒冷地区)中，通过混合分别为液态和固态的第1PEG和第2PEG，即使在倾斜的状态下形成膜，也能确保吸湿性而不会发生滴哒液体。需要说明的是，当膜形成在平面上时，可以不需要第2PEG。另一方面，例如，当在汽车部件或飞机部件等上形成膜时，优选将第2PEG混合到第1PEG中以防止吸湿层滴哒液体。
吸湿层根据用途设为适当的厚度和浓度即可。吸湿层的厚度的例子为0.1mm以上1cm以下，可以为0.5mm以上5mm以下，也可以为0.5mm以上2mm以下。
疏水层7是指具有疏水性质的层。疏水膜或疏水层是已知的，例如，如日本专利6304411号公报所述那样。例如，通过如下方式进行评价即可：当将约2μL纯水置于疏水层表面时，用接触角仪测定水滴与试样表面形成的角。接触角仪的例子为协和界面科学制的CA-X型，在大气中(约25℃)进行测定即可。在初期接触角中，接触角可以为80°以上、进一步可以为108°以上、更进一步可以为110°以上。
本说明书中的疏水膜为具有耐霜性的疏水膜。耐霜性是已知的性能，例如，如在日本专利6566945号公报中所评价的那样。在本说明书中，对于耐霜性，在温度为5℃、相对湿度为50％的环境下，将基板冷却至-15℃，观察霜的经时变化即可。然后，例如，与玻璃基板相比，霜的经时变化优异的即可被认为具有耐霜性。
疏水层7包括：疏水层基体9和附着在疏水层基体上的疏水性成分11。
疏水层基体9的例子为多孔体。由于疏水层基体9的表面为多孔的，因此附着在疏水层的表面的雪不能渗入内部而被除去。此外，由于疏水层基体9的表面为多孔的，因此附着在疏水层表面的水滴被吸湿层吸收，从而可以防止疏水层基体9的表面冻结的情况。关于多孔，可以在随机位置处具有孔隙，也可以是网状的。当多孔为网状时，从上述观点来看，多孔的网眼的例子为50μm以上4000μm以下，可以为100μm以上2000μm以下，也可以为50μm以上800μm以下，也可以为100μm以上600μm以下。对疏水层基体9的厚度没有特别地限制。
疏水性成分的例子为粒子、分子以及油层。疏水性粒子的例子为疏水性二氧化硅粒子。疏水性二氧化硅粒子是指对普通的二氧化硅微粒的表面进行化学改性，从而赋予疏水性后的二氧化硅粒子。从疏水性的观点来看，引入至二氧化硅微粒表面的改性基团的例子为甲基、乙基、丙基、丁基、异丙基、氟原子、氟甲基、二氟甲基、三氟甲基等疏水性基团。例如，在日本特开平9-110414号公报、日本特开平9-241016号公报、日本特开平6-115924号公报、以及日本特开2003-342017号公报中记载有疏水性二氧化硅粒子。
疏水性二氧化硅粒子的平均粒径(D50)的例子为10nm以上500nm以下，也可以为30nm以上400nm以下、50nm以上300nm以下。平均粒径(D50)是指将微粒分散在水中，使用激光衍射式的粒度分布测定装置所测定的粒子的粒径，D50是指当测定100个试样的粒径时，从粒径小的开始计数时第50个的粒径，也就是测定试样的平均粒径。疏水性二氧化硅粒子以适当的浓度附着在基体上即可。
疏水性成分11的另一个例子为附着在疏水层基体上的疏水性化合物。疏水性化合物为(例如)在端部具有氟原子、甲基、氟甲基、二氟甲基、三氟甲基等疏水性官能团的化合物。
疏水性成分的另一个例子为具有疏水性的油层。它可以通过在基体上涂布疏水性树脂而形成。疏水性树脂的例子为氟树脂和硅酮树脂。疏水性树脂的其他例子为：通过将氟类添加剂混合到甲基丙烯酸树脂、丙烯酸树脂、氨基甲酸酯树脂、环氧树脂等树脂中以使其表面疏水化而得的树脂。在基体上涂布适量的疏水性树脂，并使其固化，从而可以得到疏水层。
优选的是，还包括存在于吸湿层5与疏水层7之间的间隔层13。由于有间隔层，水蒸气等可以良好地通过，因此吸湿层可以吸收附着在疏水层部分的水分。此外，由于有间隔层，因此从吸湿层产生的水蒸气可以逸出。从上述观点来看，适当地调整间隔层的厚度即可。间隔层的厚度的例子为10μm以上2mm以下，可以为40μm以上1mm以下，也可以为50μm以上1mm以下，也可以为100μm以上1μm以下，也可以为50μm以上500μm以下，还可以为100μm以上400μm以下。
间隔层的孔隙率(开孔率)的例子为0.1％以上99.9％以下(或者1％以上99％以下、3％以上10％以下、3％以上50％以下、5％以上20％以下、5％以上15％以下)。间隔层可以是单纯的框架或柱子。间隔层也可以为网状。
接下来，对具有耐霜性的疏水膜的制造方法进行说明。包括：在对象表面上形成吸湿层的吸湿层形成步骤；以及在吸湿层上形成疏水层的疏水层形成步骤。
吸湿层形成步骤
吸湿层形成步骤是用于在对象表面上形成吸湿层的步骤。对象物的表面构成基板。在吸湿层形成步骤中，将通常为液态的树脂与通过对通常为固态的树脂进行加热使其液化而得的树脂混合以制备涂布液。在涂布液中可以添加各种辅助原材料。并且，根据基板的形状等，使用适当的涂布方法将涂布液涂布在基板上。涂布方法的例子为：喷涂、旋涂、辊涂以及浸渍涂布。
疏水层形成步骤
疏水层形成步骤是将疏水性成分附着在疏水层基体上以形成疏水层。在疏水层形成步骤中，在吸湿层上形成疏水层。此时，可以在吸湿层上设置间隔层，并在间隔层上形成疏水层。各层可以使用(例如)UV固化性树脂来将吸湿层与间隔层、间隔层与疏水层粘接在一起。此外，也可以使用已知的粘接剂来粘接相邻的层。
该膜具有疏水性、耐霜性、除雪性能。因此，例如，通过在与汽车外部装饰和内部装饰相关的部件表面、航空器部件的表面或建筑物的表面上形成膜，可以发挥这些性能。
疏水性的评价
对于疏水性，评价接触角和滚动角(転落角)即可。
耐过冷水试验
对于耐过冷水，将过冷水(-1℃，10μL)从5cm的高度滴到倾斜20°的基板上，观察其行为即可。
耐霜性的评价
对于耐霜性，在温度5℃、相对湿度50％的环境下将基板冷却至-15℃，观察霜的经时变化即可。
防雪附着性能评价
在人工降雪装置内(温度：-15℃，积雪深度：4cm/1小时(换算为水1mm/1小时))设置倾斜70°的基板，观察经时变化即可。
实施例1
使用2.5cm×7.6cm尺寸的玻璃基板(松波硝子社制)作为基板。将重均分子量为200的聚乙二醇(和光純薬社制：PEG200)与加热至150℃的重均分子量为400万的聚乙二醇(和光純薬社制；PEG4M)以10:1的重量比搅拌并混合。这样得到了混合液。将2g混合液均匀地涂布在玻璃基板上。其结果，在基板上得到了厚度为约1mm的吸湿层。准备了网眼为174μm、线径为80μm的聚酯网(くればぁ社制)作为基体。将含有全氟烷基的硅烷(C6)(ゲレスト社制)、二氧化硅(日本アエロジル社制)以及乙醇以1重量％、1.5重量％以及97.5重量％的重量比混合，从而制备了二氧化硅微粒分散液。将二氧化硅微粒分散液喷涂在基体上，以使二氧化硅微粒附着在基体上。这样形成了疏水层。
将厚度为180μm的PET膜(東洋紡社制)加工成与基板的外框相同的形状，以形成宽度为3mm的框体。在框体的上面和下面涂布紫外线固化性树脂。将涂布有紫外线固化性树脂的框体安装在吸湿层上。框体的上部安装有疏水层。然后，向基板照射紫外线，以使紫外线固化性树脂固化。
这样，在玻璃基板上形成了膜。
[比较例]
将玻璃基板本身作为比较例1。
除了未设置疏水层以外，与实施例1同样地形成了膜(比较例2)
评价了实施例1和比较例1、2的物性。
接触角和滚动角的测定结果示于表1。
[表1]
表1接触角和滚动角的测定结果
接触角(°) 滚动角(°)
比较例1 7.9 未滚动
比较例2 7.4 未滚动
实施例1 150 11
如表1所示，比较例1、2表现出亲水性，而实施例1表现出超疏水性。
接下来，观察实施例1和比较例1、2的过冷水去除性能。其结果示于图2。如图2所示，实施例1具有过冷水去除性能。其原因据认为是：通过间隔层在疏水层与吸湿层之间形成了空气层，因此水滴无法穿过疏水层。
作为间隔层，使用了厚度为180μm的经加工后的PET膜。虽然可以不存在间隔层，但是优选将疏水层与吸湿层隔开。因此，认为存在有间隔是好的。据认为间隔层的厚度优选为0.1μm以上1cm左右，并且据认为可以在该范围内进行适当的调整。此外，虽然使用了PET膜作为原材料，但是只要能发挥间隔功能，则可以不考虑材质。
[实施例2、3]
网眼直径的研究
使用网眼为352μm且线径为71μm的网(实施例2)、网眼为1293μm且线径为400μm的网(实施例3)作为聚酯网，除此以外，与实施例1同样地形成了膜。对实施例1、2及3的防雪附着性进行了评价。其结果示于图3。
图3(a)示出降雪前的膜的情形，图3(b)示出从降雪开始30分钟后的膜的情形。在图3中，从左侧开始示出比较例1、实施例1～3。如图3所示，实施例1和2的防雪附着性非常高(◎)。另一方面，实施例3的防雪附着性比通常高(△)。可以看出，网眼和线径越小，则表现出越高的防雪附着性。
[实施例4～13]
构成吸湿层的树脂的研究
将用于获得吸湿层的树脂成分设为表2所示的组成，除此以外，与比较例2同样地形成了膜。所得到的膜的防霜性能一并示于表2。
[表2]
表2树脂特征和防霜性能(时间)
Figure BDA0003560457510000111
由此可知，PEG200的比例越多，表现出越高的防霜性能。
这是因为，PEG的分子量越低，越提高吸湿性。
工业实用性
本发明涉及具有耐霜性的疏水膜及其制造方法，可用于因雪、霜而发生故障的各种产业。这样的产业的例子为航空器产业和汽车产业。
符号说明
1 疏水膜
3 基板
5 吸湿层
7 疏水层
9 疏水层基体
11 疏水性成分
13 间隔层

Claims (12)

1.一种膜，其为具有耐霜性的疏水膜(1)，包括：
设置在基板(3)上的吸湿层(5)、以及设置在所述吸湿层(5)上的疏水层(7)，
所述疏水层(7)包括：疏水层基体(9)和附着在所述疏水层基体上的疏水性成分(11)。
2.根据权利要求1所述的膜，其中，
所述吸湿层(5)包含防冻液成分。
3.根据权利要求2所述的膜，其中，
所述防冻液成分包含聚二甲基硅氧烷、聚苯基甲基硅氧烷、甘油、乙二醇、聚乙二醇、丙二醇、聚乙烯醇、纤维素、丙烯酸类防冻液、以及丙烯酰胺类防冻液中的1种或2种以上。
4.根据权利要求1所述的膜，其中，
所述吸湿层(5)包含：
重均分子量为100以上且小于800的聚乙二醇即第1PEG；以及
重均分子量为800以上2000万以下的聚乙二醇即第2PEG，
第1PEG与第2PEG的重量比即w1/w2为0.001以上1000以下。
5.根据权利要求1所述的膜，其中，
所述疏水性成分(11)为疏水性二氧化硅粒子。
6.根据权利要求1所述的膜，其中，
所述疏水性成分(11)为附着在所述疏水层基体上的疏水性化合物。
7.根据权利要求1所述的膜，其中，
所述疏水层基体(9)为多孔体。
8.根据权利要求1所述的膜，其中，
所述基板(3)的表面具有聚碳酸酯、丙烯酸树脂或甲基丙烯酸树脂。
9.根据权利要求7所述的膜，其中，
还包括存在于所述吸湿层(5)与所述疏水层(7)之间的间隔层(13)。
10.根据权利要求9所述的膜，其中，
所述间隔层的孔隙率为0.1％以上99.9％以下。
11.根据权利要求1至10中任一项所述的膜，其中，
所述膜形成在与汽车外部装饰和内部装饰相关的部件表面或航空器的机身表面。
12.一种具有耐霜性的疏水膜的制造方法，包括：
在对象表面上形成吸湿层的吸湿层形成步骤；以及
在所述吸湿层上形成疏水层的疏水层形成步骤，
所述疏水层形成步骤包括使疏水性成分附着在疏水层基体上的步骤。
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