CN111303738B - 一种多孔结构的超疏水-润滑复合防冰涂层及制备方法 - Google Patents
一种多孔结构的超疏水-润滑复合防冰涂层及制备方法 Download PDFInfo
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Abstract
本发明属于新材料领域，具体涉及一种多孔结构的超疏水‑润滑复合防冰涂层及制备方法。所述涂层由发泡多孔的超疏水涂层和仿生关节润滑液构成，所述超疏水发泡多孔结构的超疏水‑润滑复合防冰涂层由低分子聚丁二烯、聚丙烯酰、水性聚氨酯、烷基烯酮二聚体复合再经对甲苯磺酰肼加热发泡，制备而成。所获涂层的仿生关节润滑液与低分子聚丁二烯的共混成分，可显著降低冰层粘附力，使得冰层粘附力降低到5kPa以下，起到优异抗冰效果。
Description
技术领域
本发明属于新材料领域，具体涉及一种具有防冰效果的超疏水-润滑复合防冰涂层。
背景技术
冰冻及寒冷天气每年都会给我国带来数以亿计的损失，涉及领域包括航天运输，公共交通，基建设施，甚至电力运输的延误和损耗。线路的覆冰会让电力部门的及时疏通极具挑战，我国作为地大物博的大国，线路覆冰的影响更是位居世界前列。除此以外，覆冰对于飞机机翼的影响也是举足轻重的。严重的覆冰甚至会造成机翼的停转从而引发空难。道路方面，出行安全的提升同样要从轮胎与铁轨的防滑防冰着手，结冰在很大程度上给人民的财产和安全带来了巨大的隐患。因此，开展超疏水防冰涂层材料的研究是有巨大社会意义的。
荷叶由于自身自清洁，防冰以及减阻等特性，从而有良好的超疏水性。“荷叶效应”也是最为大众所熟知的超疏水现象。研究表明，自然界生物的微/纳结构对于研究防冰材料有着重要意义。例如荷叶表面含有微/纳复合的乳突结构，使得表面呈超疏水性[Barthlott,W.；Neinhuis,C.Planta 1997,202,1；Feng,L.；Li,S.H.；Li,Y.S.；Li,H.J.；Zhang,L.J.；Zhai,J.；Song,Y.L.；Liu,B.Q.；Jiang,L.；Zhu,D.B.Advanced Materials2002,14,1857.]。后来的科研工作者受此启发制备了大量的超疏水涂层。所以外力作用对于超疏水表面的微纳结构的破坏会直接影响其表面的超疏水效果以及防冰特性。研究发现，仿猪笼草的含低表面能润滑液的表面表现出了优异的抗压特性以及良好的防冰性能[Wong,T.-S.et al.Nature 2001,477,443；Kim,P.et al.ACS Nano 2012,6,6569；Liu,Q.et al.Applied Surface Science 2015,346,68]。这是利用电化学腐蚀的方法在表面构造多孔结构从而吸附低表面能润滑液，防止低表面能润滑液流走。这种表面对于物体的粘附力极低，这种润滑表面对物体的粘附极低，无论是水还是冰都可以在重力作用下从表面滑落，进而较少外力作用。该方案的难点在于提高防冰材料的耐用性，因为随着使用次数的增加，表面润滑液的数量会减少，粘附力也会增加，失去抗冰效果。
发明内容
针对现有技术中存在不足，本发明提供了一种发泡多孔结构的超疏水-润滑复合防冰涂层及其制备方法，涂层具备优异的抗冰性能，可显著降低冰的粘附力，仿生关节润滑液易于获得，更加环保，且制备方法简单，成本低。
实现本发明目的的技术解决方案为：
一种多孔结构的超疏水-润滑复合防冰涂层，其特征在于，所述防冰涂层由发泡多孔的超疏水涂层和注射到超疏水涂层表面的仿生关节润滑液构成，所述超疏水涂层由低分子聚丁二烯、聚丙烯酰、水性聚氨酯、烷基烯酮二聚体加溶剂混合后再经对甲苯磺酰肼加热发泡，喷涂制备而成。
所述发泡多孔结构的超疏水-润滑复合防冰涂层的制备方法，其特征在于，包括以下步骤：
(1)将低分子聚丁二烯、聚丙烯酰、水性聚氨酯、烷基烯酮二聚体进行混合后，加入庚烷作为溶剂进行加热搅拌溶解，加热搅拌温度20-30℃，加热搅拌时间为1h，再经对甲苯磺酰肼加热发泡，将得到的溶液于常温下采用喷涂方式成膜后，40-60℃下干燥，获得发泡多孔结构的超疏水涂层；
(2)将步骤(1)制备得到的发泡多孔结构的超疏水涂层表面注入仿生关节润滑液，得到发泡多孔结构的超疏水-润滑复合防冰涂层。
进一步地，步骤(1)中所述低分子聚丁二烯、聚丙烯酰、水性聚氨酯、烷基烯酮二聚体、庚烷混合重量比为1：2-5：5-6：3-6：7-9。
进一步地，步骤(1)中所述甲苯磺酰肼的添加量为低分子聚丁二烯、聚丙烯酰、水性聚氨酯、烷基烯酮二聚体和庚烷组成的混合物总质量的20-50wt.％,加热温度为50～80℃，加热发泡时间为1小时。
进一步地，步骤(2)中所述仿生关节润滑液为纳米石墨烯改性的透明质酸(HA)，将纳米石墨烯加入到透明质酸里面即可得到，纳米石墨烯粒径范围为70～100nm，添加量为仿生关节润滑液总质量的1～2.5wt.％；润滑液采用微量注射器添加到超疏水涂层表面，添加量为0.3～0.5g/cm2。
本发明与现有技术相比，其显著优点为：1)低分子聚丁二烯、聚丙烯酰、水性聚氨酯、烷基烯酮二聚体的庚烷溶液经喷涂成膜后，在干燥后自动形成多孔膜结构，表面水滴接触角可高达155°，具备优异的疏水性。同时，制备工艺简单，设备要求低，可大规模制备；2)采用纳米石墨烯改性的透明质酸(HA)润滑液，不含氟、更环保，且易于获得；3)所获涂层的仿生关节润滑液与低分子聚丁二烯的共混成分，可显著降低冰层粘附力，使得冰层粘附力降低到5kPa以下，起到优异抗冰效果。
附图说明
图1为实施例1水滴接触角。
图2为实施例2水滴接触角。
图3为实施例3水滴接触角。
具体实施方式
下面结合附图以及具体实施例对本发明作进一步的说明，但本发明的保护范围并不限于此。
本发明所提供发泡多孔结构的超疏水-润滑复合防冰涂层，具备优异的抗冰性能，可显著降低冰的粘附力。所述防冰涂层由发泡多孔结构的超疏水-润滑复合防冰涂层和仿生关节润滑液构成，所述发泡多孔结构的超疏水-润滑复合防冰涂层由低分子聚丁二烯、聚丙烯酰、水性聚氨酯、烷基烯酮二聚体复合制备而成。
所述防冰涂层的制备方法包括以下步骤：
(1)首先，将低分子聚丁二烯、聚丙烯酰、水性聚氨酯、烷基烯酮二聚、庚烷(溶剂)体按照重量比1：2-5：5-6：3-6：7-9进行混合后，于20-30℃条件下加热搅拌处理1h后，加入混合物总质量20～50wt.％的甲苯磺酰肼于50～80℃发泡1小时，常温下采用喷涂成膜后在40～60℃下干燥，获得发泡多孔结构的超疏水涂层；
(2)其次，将粒径为70～100nm的纳米石墨烯，按照重量比1～2.5wt.％加入到透明质酸(HA)润滑液中，超声波分散后得到仿生关节润滑液；
(3)最后，将发泡多孔结构的超疏水涂层表面通过微量注射器注入纳米石墨烯改性的仿生关节润滑液0.3-0.5g/cm2，得到发泡多孔结构的超疏水-润滑复合防冰涂层。
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)将低分子聚丁二烯、聚丙烯酰、水性聚氨酯、烷基烯酮二聚体、庚烷按照质量比1：3：5：3：7，进行混合后，加热25℃搅拌处理1h后，加入混合物总质量20wt.％的甲苯磺酰肼于70℃发泡1小时，常温下采用喷枪进行喷涂，并于50℃下干燥，获得发泡多孔结构的超疏水-润滑复合防冰涂层；
(2)将粒径为90nm的纳米石墨烯，按照重量比2wt.％加入到透明质酸(HA)润滑液中，超声波分散后得到改性仿生关节润滑液；
(3)采用微量注射器，注入纳米石墨烯改性透明质酸(HA)0.3g/cm2后，得到复合涂层。
制备得到的发泡多孔结构的超疏水-润滑复合防冰涂层，水滴接触角为120°，如图1所示；得到的复合涂层，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10kPa。
实施例2：
(1)将低分子聚丁二烯、聚丙烯酰、水性聚氨酯、烷基烯酮二聚体、庚烷按照质量比1：4：6：5：8，进行混合后，加热30℃搅拌处理1h，加入45wt.％的甲苯磺酰肼于75℃发泡1小时,常温下采用喷枪进行喷涂，并于40℃下干燥，获得发泡多孔结构的超疏水涂层；
(2)将粒径为80nm的纳米石墨烯，按照重量比1.5wt.％加入到透明质酸(HA)润滑液中，超声波分散后得到改性仿生关节润滑液；
(3)采用微量注射器，注入纳米石墨烯在透明质酸(HA)0.4g/cm2后，得到复合涂层。
制备得到的发泡多孔结构的超疏水-润滑复合防冰涂层，水滴接触角为130°，如图2所示；得到的滑液注入式复合涂层，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6kPa。
实施例3：
(1)将低分子聚丁二烯、聚丙烯酰、水性聚氨酯、烷基烯酮二聚体、庚烷按照质量比1：4：5：6：9，进行混合后，加热20℃搅拌处理1h,加入25wt.％的甲苯磺酰肼于60℃发泡1小时，常温下采用喷枪进行喷涂，并于50℃下干燥，获得发泡多孔结构的超疏水涂层；
(2)将粒径为85nm的纳米石墨烯，按照重量比1.5wt.％加入到透明质酸(HA)润滑液中，超声波分散后得到改性仿生关节润滑液
(3)采用微量注射器，注入纳米石墨烯在透明质酸(HA)0.35g/cm2后，得到复合涂层。
制备得到的发泡多孔结构的超疏水-润滑复合防冰涂层，水滴接触角为155°，如图3所示；得到的滑液注入式复合涂层，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4kPa。
对比例：
按照背景技术中的文献《Liquid-infused nanostructured surfaces withextreme anti-ice and anti-frost performance》所叙述制备的润滑液注入式抗冰涂层，步骤如下：
(1)配置浓度为0.1～0.2M的聚吡络单聚体溶液；
(2)采用恒电位沉积的方式，制备获得涂层；
(3)注入Krytox 100全氟润滑液。
实验发现：该涂层采用电化学方式，只能在金属表面获得，受用范围较为狭窄；所制备涂层，润滑液容易蒸发，导致涂层失效；对比例所制备涂层，在-30℃环境下，接触面积为1cm2、高3cm的冰块，冰的表面粘附力高达20kPa,远高于本发明所述制备的涂层的粘附力，抗冰效果较差。
所述实施例为本发明的优选的实施方式，但本发明并不限于上述实施方式，在不背离本发明的实质内容的情况下，本领域技术人员能够做出的任何显而易见的改进、替换或变型均属于本发明的保护范围。
Claims (2)
1.一种多孔结构的超疏水-润滑复合防冰涂层，其特征在于，所述防冰涂层由发泡多孔的超疏水涂层和注射到超疏水涂层表面的仿生关节润滑液构成，所述超疏水涂层由低分子聚丁二烯、聚丙烯酰胺、水性聚氨酯、烷基烯酮二聚体加溶剂混合后再经对甲苯磺酰肼加热发泡，喷涂制备而成；所述的一种多孔结构的超疏水-润滑复合防冰涂层的制备方法具体步骤如下：
（1）将低分子聚丁二烯、聚丙烯酰胺、水性聚氨酯、烷基烯酮二聚体、庚烷按照质量比1：4：5：6：9，进行混合后，加热20 ℃搅拌处理1h, 加入25 wt.%的对甲苯磺酰肼于60 ℃发泡1小时，常温下采用喷枪进行喷涂，并于50℃下干燥，获得发泡多孔结构的超疏水涂层；
（2）将粒径为85 nm的纳米石墨烯，按照重量比1.5 wt.%加入到透明质酸润滑液中，超声波分散后得到改性仿生关节润滑液；
（3）采用微量注射器，按照0.35 g/cm2注入改性仿生关节润滑液后，得到复合涂层。
2.如权利要求1所述的一种多孔结构的超疏水-润滑复合防冰涂层的制备方
法，其特征在于，具体步骤如下：
（1）将低分子聚丁二烯、聚丙烯酰胺、水性聚氨酯、烷基烯酮二聚体、庚烷按照质量比1：4：5：6：9，进行混合后，加热20 ℃搅拌处理1h, 加入25 wt.%的对甲苯磺酰肼于60 ℃发泡1小时，常温下采用喷枪进行喷涂，并于50℃下干燥，获得发泡多孔结构的超疏水涂层；
（2）将粒径为85 nm的纳米石墨烯，按照重量比1.5 wt.%加入到透明质酸润滑液中，超声波分散后得到改性仿生关节润滑液；
（3）采用微量注射器，按照0.35 g/cm2注入改性仿生关节润滑液后，得到复合涂层。
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