CN111303705A - 一种多孔树脂超疏水涂层及制备方法 - Google Patents

一种多孔树脂超疏水涂层及制备方法 Download PDF

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CN111303705A
CN111303705A CN202010077992.3A CN202010077992A CN111303705A CN 111303705 A CN111303705 A CN 111303705A CN 202010077992 A CN202010077992 A CN 202010077992A CN 111303705 A CN111303705 A CN 111303705A
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kaolin
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王楠
杨星光
张程
李何亮
唐玲玲
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Abstract

本发明涉及超疏水界面涂层，具体涉及一种具有抗冰、防覆冰效果的多孔树脂超疏水涂层及制备方法。将改性纳米氧化钴、改性高岭土与聚丙烯酸、聚丙烯、聚氯乙烯进行混合后，加入三氟三氯乙烷作为溶剂在20～30℃条件下进行加热搅拌处理后，常温下采用辊涂形式成膜后于80～90℃下干燥，获得超疏水多孔树脂涂层。本发明与现有技术相比，其显著优点为：1)制备流程简单，设备条件要求较低，容易制备；2)采用易于获得成本不高的原材料；3)所获块状材料可具有优异的疏水特性，具有抗冰、防覆冰效果。

Description

一种多孔树脂超疏水涂层及制备方法
技术领域
本发明涉及超疏水界面涂层，具体涉及一种具有抗冰、防覆冰效果的多孔树脂超疏水涂层及制备方法。
背景技术
覆冰现象在自然界中是一个十分常见的现象，但其对日常的生活生产带来了极大的不便，甚至在一些行业带来了不小的危害。例如：覆冰会导致一些冷冻设备的热传递效率大大降低甚至失效；在温度低，潮湿的环境下，对飞机的整流罩等部位产生积冰，将严重降低飞机飞行时的安全系数；覆冰对电力系统的危害更是严重，如导线舞动、断线、闪络等。
为了防止覆冰对生活生产的各个方面的影响，加之近年来超疏水界面越来越受到科学界的广泛关注，受荷叶启发，人工制造超疏水界面的涂层的方法不断涌现。这种特殊界面具有对水极度排斥性，可应用于抗冰、自清洁、腐蚀防护等领域。主要制备方法大体分为两种：其一，通过构筑低表面微纳米结构表面，即可获得这种超疏水表面；其二，通过修饰低表面微纳米结构表面，即可获得这种超疏水表面。具体方法有：溶胶凝胶法、电化学刻蚀、气相沉积、静电纺丝等方式来制备超疏水界面。但是，在潮湿环境下，上述方法制得的表面会结冰，使原有的超疏水界面性质失去，防冰性能大大下降，而且冰层粘附力较大，失去抗冰效果。
南京航空航天大学沈一洲课题组制备了具有阵列微结构的超疏水表面，并研究了冰层在表面的粘附力，结果显示冰的粘附力可显著下降(Y Shen,M Jin,X Wu,J Tao,XLuo,H Chen,Y Lu,Applied Thermal Engineering 156,2019,111-118)；俄罗斯的Boinovich课题组在金属表面制备获得了具有防结冰能力的超疏水界面，可在冰雪环境下显著降低雪的积累量(Ludmila B.Boinovich，Alexandre M.Emelyanenko,VladimirK.Ivanov,Andrei S.Pashinin,ACS Appl.Mater.Interfaces
2013,5,7,2549-2554)。上述方式都存在界面制备工艺复杂、需精准纳米形状微结构，对制备工艺要求较高的缺点；且获得界面在冷凝结冰环境下，冰层的粘附力较高，无法实现较好的实际抗冰效果。
发明内容
本发明的目的在于提供一种多孔树脂超疏水涂层及其制备方法，涂层具备优异的疏水特性，具有抗冰、防覆冰效果和长效持久性。
实现本发明目的的技术解决方案为：一种多孔树脂超疏水涂层；所述超疏水多孔树脂涂层由聚丙烯酸(PAA)、聚丙烯(PP)、聚氯乙烯(PVC)、改性纳米氧化钴、改性高岭土复合制备而成，具体制备步骤如下：
(1)将纳米氧化钴(5～20nm)、高岭土(30～100μm)置于高温密闭反应釜中，采用羟基封端三氟丙基溶液0.08～0.15mol/L进行改性处理，反应温度为10～30℃，反应时间为2小时，得到改性纳米氧化钴、改性高岭土；其中，羟基封端三氟丙基溶液与纳米氧化钴、高岭土质量比为1：300～400：700～800。
(2)将改性纳米氧化钴、改性高岭土与聚丙烯酸(PAA)、聚丙烯(PP)、聚氯乙烯(PVC)进行混合后，加入三氟三氯乙烷作为溶剂在20～30℃条件下进行加热搅拌处理后，常温下采用辊涂形式成膜后于80～90℃下干燥，获得超疏水多孔树脂涂层；其中，聚丙烯酸(PAA)、聚丙烯(PP)、聚氯乙烯(PVC)、改性纳米氧化钴、改性高岭土、三氟三氯乙烷混合的重量比为1：4～6：16～18：12～16：7～9：11～15。
本发明与现有技术相比，其显著优点为：1)制备流程简单，设备条件要求较低，容易制备；2)采用易于获得成本不高的原材料；3)所获块状材料可具有优异的疏水特性，具有抗冰、防覆冰效果。
附图说明
图1实例1水滴接触角。
图2实例2水滴接触角、滚动角。
图3实例3水滴接触角。
具体实施方式
下面结合附图对本发明作进一步详细描述。
本发明的目的在于提供一种多孔树脂超疏水涂层及其制备方法。该涂层由聚丙烯酸(PAA)、聚丙烯(PP)、聚氯乙烯(PVC)、改性纳米氧化钴、改性高岭土复合制备而成。涂层具备优异的疏水特性，具有抗冰、防覆冰效果和长效持久性。本发明的一种多孔树脂超疏水涂层制备方法包括以下步骤：
(1)将纳米氧化钴(5～20nm)、高岭土(30～100μm)放入不锈钢高温反应釜中，并于旁边放置小坩埚，内装辛烷稀释的羟基封端三氟丙基溶液0.08～0.15mol/L；加热反应釜至反应温度为10～30℃并保持2小时后，取出即可得到改性纳米氧化钴、改性高岭土；
(2)将改性纳米氧化钴、改性高岭土与聚丙烯酸(PAA)、聚丙烯(PP)、聚氯乙烯(PVC)进行混合后，加入适量三氟三氯乙烷作为溶剂进行加热搅拌20～30℃处理1小时，常温下采用辊涂机进行辊涂，并于80～90℃下干燥，获得超疏水多孔树脂涂层；
其中，步骤(1)中，氟硅烷溶液与纳米氧化钴(5～20nm)、高岭土(30～100μm)质量比为1：300～400：700～800；步骤(2)中其中，聚丙烯酸(PAA)、聚丙烯(PP)、聚氯乙烯(PVC)、改性纳米氧化钴、改性高岭土、三氟三氯乙烷混合重量比为1：4～6：16～18：12～16：7～9：11～15。
下面结合实施例对本发明做进一步详细的说明：
实施例1：
(1)将纳米氧化钴(粒径15nm)、高岭土(粒径70μm)放入不锈钢高温反应釜中，小坩埚内装辛烷稀释的浓度为0.08mol/L羟基封端三氟丙基；加热反应釜至反应温度为10℃并反应2小时后，取出即可得到改性纳米氧化钴、改性高岭土；其中，羟基封端三氟丙基溶液与纳米氧化钴(粒径15nm)、高岭土(粒径70μm)质量比为1：350：750。
(2)将步骤(1)获得的聚丙烯酸(PAA)、聚丙烯(PP)、聚氯乙烯(PVC)、改性纳米氧化钴、改性高岭土与三氟三氯乙烷按照质量比16：12：7：1：4：11，进行混合后，加热25℃搅拌1小时处理，常温下采用辊涂机进行辊涂，并于85℃下干燥，获得多孔树脂涂层；
制备得到的多孔树脂涂层，水滴接触角为90°，如图1所示；得到的多孔涂层，在-30℃环境下，接触面积为1cm2、高3cm的冰块，其表面冰层粘附力高达60kPa。
实施例2：
(1)将纳米氧化钴(粒径5nm)、高岭土(粒径60μm)放入不锈钢高温反应釜中，小坩埚内装辛烷稀释的浓度为0.12mol/L羟基封端三氟丙基加热反应釜至反应温度为20℃并保持2小时后，取出即可得到改性纳米氧化钴、改性高岭土；其中，羟基封端三氟丙基溶液与纳米氧化钴(粒径5nm)、高岭土(粒径60μm)质量比为1：400：800。
(2)将步骤(1)获得的聚丙烯酸(PAA)、聚丙烯(PP)、聚氯乙烯(PVC)、改性纳米氧化钴、改性高岭土与三氟三氯乙烷按照质量比17：14：8：1：5：13，进行混合后，加热20℃搅拌处理1小时，常温下采用辊涂机进行辊涂，并于90℃下干燥，获得多孔树脂涂层；
制备得到的多孔树脂涂层，水滴接触角为158°，滚动角为2°，如图2所示；得到的多孔涂层，在-30℃环境下，接触面积为1cm2、高3cm的冰块，其表面冰层粘附力为20kPa.
实施例3：
(1)将纳米氧化钴(粒径20nm)、高岭土(粒径80μm)放入不锈钢高温反应釜中，小坩埚内装辛烷稀释的浓度为0.15mol/L羟基封端三氟丙基；加热反应釜至反应温度为30℃并保持2小时后，取出即可得到改性纳米氧化钴、改性高岭土；其中，羟基封端三氟丙基溶液与纳米氧化钴(粒径20nm)、高岭土(粒径80μm)质量比为1：300：700。
(2)将步骤(1)获得的聚丙烯酸(PAA)、聚丙烯(PP)、聚氯乙烯(PVC)、改性纳米氧化钴、改性高岭土与三氟三氯乙烷按照质量比17：15：9：1：6：14，进行混合后，加热30℃搅拌处理1小时，常温下采用辊涂机进行辊涂，并于80℃下干燥，获得多孔树脂涂层；
制备得到的多孔树脂块状材料，水滴接触角为120°，如图3所示；得到的多孔涂层，在-30℃环境下，接触面积为1cm2、高3cm的冰块，其表面冰层粘附力为120kPa.
对比例：
按照背景介绍中文献《Understanding the frosting and defrostingmechanism on the superhydrophobic surfaces with hierarchical structures forenhancing anti-frosting performance》所叙述制备超疏水界面，步骤如下：
(1)超声波清洗硅片后，覆盖厚度为～5μm的SU-8光刻胶；
(2)覆盖光刻胶掩膜版后，采用UV光照5～10秒；
(3)采用氟硅烷对处理后的表面进行化学疏水修饰后，得到所需超疏水涂层实验发现：该涂层只能在严格清洗后的硅片上制备，受用范围较为狭窄；采用光刻技术，工艺复杂、重复性差，且不具备大规模制备的前景；所获得涂层，在-30℃环境下，接触面积为1cm2、高3cm的冰块，表面冰层粘附力高达200kPa，抗冰效果不佳。

Claims (5)

1.一种多孔树脂超疏水涂层，其特征在于，所述超疏水多孔树脂涂层由聚丙烯酸(PAA)、聚丙烯(PP)、聚氯乙烯(PVC)、改性纳米氧化钴、改性高岭土混合、辊涂制备而成；改性纳米氧化钴和改性高岭土是由纳米氧化钴、高岭土采用羟基封端三氟丙基溶液改性处理得到的。
2.如权利要求1所述的一种多孔树脂超疏水涂层的制备方法，其特征在于，具体步骤如下：
(1)将纳米氧化钴、高岭土置于高温密闭反应釜中，采用羟基封端三氟丙基溶液进行改性处理，得到改性纳米氧化钴、改性高岭土；
(2)将改性纳米氧化钴、改性高岭土与聚丙烯酸(PAA)、聚丙烯(PP)、聚氯乙烯(PVC)进行混合后，加入三氟三氯乙烷作为溶剂加热搅拌处理后，常温下采用辊涂形式成膜后干燥，获得超疏水多孔树脂涂层。
3.如权利要求2所述的一种多孔树脂超疏水涂层的制备方法，其特征在于，步骤(1)中，纳米氧化钴的粒径为5～20nm，高岭土的粒径为30～100μm；羟基封端三氟丙基溶液的浓度为0.08～0.15mol/L，改性处理的反应温度为10～30℃，反应时间为2小时；羟基封端三氟丙基溶液与纳米氧化钴、高岭土质量比为1：300～400：700～800。
4.如权利要求2所述的一种多孔树脂超疏水涂层的制备方法的制备方法，其特征在于，步骤(2)中，在20～30℃条件下加热搅拌处理，干燥温度为80～90℃；聚丙烯酸(PAA)、聚丙烯(PP)、聚氯乙烯(PVC)、改性纳米氧化钴、改性高岭土、三氟三氯乙烷混合的重量比为1：4～6：16～18：12～16：7～9：11～15。
5.如权利要求2所述的一种多孔树脂超疏水涂层的制备方法的制备方法，其特征在于，步骤(1)中，将纳米氧化钴、高岭土放入不锈钢高温反应釜中，并于旁边放置小坩埚，内装辛烷稀释的羟基封端三氟丙基溶液。
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