CN116656193B - 一种超亲水涂料及形成耐磨、耐煮超亲水涂层的方法 - Google Patents
一种超亲水涂料及形成耐磨、耐煮超亲水涂层的方法 Download PDFInfo
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Abstract
本发明公开了一种超亲水涂料，由如下质量份数的组分混制而成：1～3份丙烯酸树脂、0.3～1份氨基树脂、2～4份正硅酸四乙酯、1～2份氨水、0.5～2份纳米颗粒、0.2～0.5份纳米管、1～3份阴离子表面活性剂和90～95份水。本发明还公开了基于上述超亲水涂料形成耐磨、耐煮超亲水涂层的方法，具体为：将清洁处理后的玻璃基底进行活化处理；将涂料以浸涂、喷涂、辊涂或刮涂的方式涂覆在玻璃基底表面，固化后在玻璃基底表面形成耐磨、耐煮超亲水涂层。
Description
技术领域
本发明涉及一种超亲水涂料，还涉及基于上述涂料形成耐磨、耐煮超亲水涂层的方法。
背景技术
玻璃在建筑、光伏，光学仪器、农业温室、汽车视窗等技术领域均有广泛应用，然而其表面的结露起雾和灰尘积聚现象，不但影响其美观性，同时由于透光率下降导致设备功能失效，甚至会引发安全事故，因此解决玻璃表面的起雾和灰尘积聚问题具有极大的现实意义。
为实现玻璃表面的防雾、自清洁效果，传统方法通过在玻璃表面涂覆纳米级TiO2涂层，在受到太阳光中的紫外光照射后，TiO2固体表面生成空穴(h+)和电子(e-)。空穴(h+)使玻璃表面的水蒸气氧化形成大量的亲水基团(-OH)，由于-OH对水分子的强烈吸附作用，能够使玻璃表面的冷凝液滴快速铺展形成水膜，从而极大地减少光线通过样品时因折射和散射导致的损失，起到防雾效果。同时，电子(e-)能够将附着在表面的有机物氧化为CO2、H2O等简单的无机物。当雨水滴落在涂层表面时，由于表面亲水基团-OH与水之间形成氢键作用力要远大于灰尘等污染物与玻璃表面的范德华力，因此水取代灰尘等污染物吸附于涂层表面形成水膜，表面上原来吸附的灰尘等污染物则被水带走而实现自清洁效果。但是这种传统的防雾自清洁涂层对太阳光强度有很大的依赖，在夜晚、阴天或建筑物的阴面效率低下。同时传统涂层表面的疏松多孔结构，在外力冲击下容易被破坏，亲水性难以长效保持，无法实现长效防雾自清洁效果。
发明内容
发明目的：本发明目的旨在提供一种超亲水涂料，本发明另一目的旨在提供基于上述涂料形成耐磨、耐煮超亲水涂层的方法。
技术方案：本发明所述的超亲水涂料，由如下质量份数的组分混制而成：1～3份丙烯酸树脂、0.3～1份氨基树脂、2～4份正硅酸四乙酯、1～2份氨水、0.5～2份纳米颗粒、0.2～0.5份纳米管、1～3份阴离子表面活性剂和90～95份水。
其中，所述涂料的pH值为8～10。
其中，所述丙烯酸树脂(P299190)的平均分子量为～2000；所述氨基树脂(MR-603)的分子量为300～600。选用的两种树脂在涂料配制及涂层固化过程中发生交联固化，固化后分子量会增大。分子量过低导致涂层强度偏低，分子量过大导致涂料粘度大，液体流平性差，涂层表面粗糙，影响涂层的透明性。
其中，所述纳米颗粒为二氧化硅或氧化铝中的至少一种，所述纳米颗粒的粒径为5～10nm。
其中，所述纳米管为埃洛石纳米管，所述纳米管的管径为10～30nm，管长为0.5～2μm。
其中，所述阴离子表面活性剂为α-烯基磺酸钠、羟乙基磺酸钠、十六烷基磺酸钠或十六烷基硫酸钠中的一种。
正硅酸四乙酯在氨水调节的pH＝8～10的碱性溶液中发生不完全水解形成的大量-Si-OH，与引入的埃洛石纳米管、SiO2、Al2O3纳米粒子表面富含的大量-OH以及丙烯酸树脂携带的-COOH，会脱水缩聚分别形成醚键和酯基，同时丙烯酸树脂和氨基树脂发生的酰胺化反应能够使涂层形成致密的三维立体网络结构。涂层中各组分之间的共价键结合力使涂层具有超高耐磨性能。另外，由于埃洛石纳米管内壁带有正电荷，溶液中引入的阴离子表面活性剂被快速地吸附到纳米管内部，增加了表活迁移出涂层的空间位阻，延缓了表面活性剂在润湿或泡水环境中的释放速度。同时，SiO2、Al2O3纳米粒子的引入在提高涂层致密性的同时能够进一步增加表面活性剂的迁移位阻，因此涂层在煮沸2h后仍表现出良好的防雾自清洁性能，从而具有长效防雾、自清洁功能。
基于上述超亲水涂料形成耐磨、耐煮超亲水涂层的方法，包括如下步骤：
(1)将清洁处理后的玻璃基底进行活化处理：将玻璃基底先用无水乙醇做去脂处理(用无水乙醇浸泡30min)，然后将玻璃基底放入过氧化氢与浓硫酸的混合溶液中，浸泡10～30s后取出，用水冲洗、干燥后备用；玻璃基底在过氧化氢和浓硫酸的混合溶液中浸泡后，表面形成大量的-Si-OH，与涂层中的-OH、-NH2以及-COOH发生化学交联反应，使涂层与基底之间具有强大的结合力，进一步提高涂层的耐磨性能；
(2)将涂料以浸涂、喷涂、辊涂或刮涂的方式涂覆在步骤(1)的玻璃基底表面，固化后在玻璃基底表面形成耐磨、耐煮超亲水涂层。
其中，步骤(1)中，过氧化氢与浓硫酸的混合体积比为3：7；过氧化氢的质量浓度为30％；浓硫酸的质量浓度为98％。
其中，步骤(2)中，固化条件为在150～220℃下加热15min。在高温下固化能够促进三维立体强交联网络结构的形成，使涂层表现出优异的耐磨性能，Taber摩擦磨损实验证明，涂层在承受250g载荷的CS-10F磨轮摩擦2000圈后，仍具有良好的防雾性能。
有益效果：相比于现有技术，本发明具有如下显著的优点：(1)本发明采用粒径为5～10nm的球形纳米粒子和管径为10～30nm，管长为0.5～2μm的埃洛石纳米管作为涂层的复合填料，使形成的防雾自清洁涂层具有高的透光率和超高的耐磨性能，Taber摩擦磨损实验证明，涂层在承受250g载荷的CS-10F磨轮摩擦2000圈后，仍保持良好的防雾性能；(2)通过纳米管对表面活性剂的负载，协同纳米粒子在涂层中的紧密堆积以及树脂对填料的包覆作用，增加了表面活性剂的迁移位阻，延缓了其在泡水或润湿环境中的流失速度，涂层在煮沸2h后，仍具有良好的防雾自清洁性能；(3)同时由于涂层表面的光滑结构，降低了污染物与涂层表面的接触面积，形成的水膜能够更快地将污染物与涂层表面隔离，实现自清洁效果。
附图说明
图1为实施例1玻璃基底上涂层的制备流程图；
图2为实施例1中涂层的水接触角、表面原子力显微镜(AFM)粗糙结构图和防雾效果图；其中，(a)为涂有实施例1涂层的水接触角(WCA)；(b)为5μL液滴在涂层和空白玻璃表面的铺展情况对比；(c)为实施例1涂层在80℃水热加湿环境下2min后的防雾效果图；(d)为实施例1涂层的AFM粗糙结构图；
图3为实施例1～3涂层的SEM表面形貌图；其中，(a)为实施例1涂层，(b)为实施例2涂层，(c)为实施例3涂层；
图4为实施例1涂层的沙尘自清洁效果图；
图5为实施例1涂层与空白玻璃户外环境放置300天后的自清洁效果图；
图6为实施例1涂层摩擦2000圈、实施例2涂层摩擦500圈、实施例3涂层摩擦800圈后的SEM表面形貌图；其中，(a)为实施例1涂层，(b)为实施例2涂层，(c)为实施例3涂层；
图7为实施例1涂层摩擦2000圈、实施例2涂层摩擦500圈、实施例3涂层摩擦800圈后的防雾效果图，虚线内区域为磨损处；其中，(a)为实施例1涂层，(b)为实施例2涂层，(c)为实施例3涂层；
图8为实施例1涂层煮沸2h、实施例5涂层煮沸1h、实施例6涂层煮沸1h后的SEM表面形貌图；其中，(a)为实施例1涂层，(b)为实施例5涂层，(c)为实施例6涂层；
图9为实施例1涂层煮沸2h、实施例5涂层煮沸1h、实施例6涂层煮沸1h后的防雾效果图，红框部分为对应区域测定接触角；其中，(a)为实施例1涂层，(b)为实施例5涂层，(c)为实施例6涂层。
具体实施方式
下面结合附图对本发明的技术方案作进一步说明。
实施例1
本发明超亲水涂料，由如下质量份数的组分混制而成：1份丙烯酸树脂、0.3份氨基树脂、4份正硅酸四乙酯、2份氨水、0.5份粒径为10nm左右的SiO2纳米颗粒、0.2份管径为20nm、管长为1μm左右的埃洛石纳米管、1份十六烷基磺酸钠和90份水。
上述超亲水涂料的制备方法，具体为：将1份丙烯酸树脂、0.3份氨基树脂、4份正硅酸四乙酯、2份氨水、0.5份粒径为10nm左右的SiO2纳米颗粒、0.2份管径为20nm、管长为1μm左右的埃洛石纳米管、1份十六烷基磺酸钠以及90份水混合后，在50℃恒温水浴和200转/分钟条件下，搅拌均匀后得到超亲水涂料。
基于上述超亲水涂料形成耐磨、耐煮超亲水涂层的方法，包括如下步骤：
(1)将清洁处理后的玻璃基底进行活化处理：将玻璃基底用无水乙醇浸泡30min，做去脂处理，然后将玻璃基底放入体积比为3：7的过氧化氢(30％，AR)与浓硫酸(98％，AR)的混合溶液中，浸泡10～30s后取出，用水冲洗、干燥后备用；
(2)将超亲水涂料以浸涂的方式涂覆在步骤(1)的玻璃基底表面形成涂层，将涂层样品放入烘箱中于200℃下烘烤15min，得到耐磨、耐煮超亲水涂层。
实施例1涂层的表面平滑致密，表面粗糙度为9.6nm,透光率均达到91.3％。涂层的水下油接触角为142.5°，具有优异的水下疏油性能。涂层与玻璃基底结合力好(13.7±0.3MPa)，维氏硬度为97。图2(a)所示涂层的水接触角为3.8°，表现出超亲水性能。图2(b)所示，与空白玻璃表面相比，液滴(5μL)在涂层表面能够完全铺展，形成水膜，降低了光线透过时因折射导致的损失，保证透光率。图2(c)所示涂层表现出良好的防雾性能。图2(d)所示涂层具有纳米级粗糙度；图3(a)所示涂层表面平滑致密。通过图4防沙尘试验结果表明，涂层表现出优异的自清洁性能。通过图5户外自清洁防污染试验结果表明，与空白玻璃相比，涂层在户外放置300天后，表面仍保持透明光洁。图6(a)所示，实施例1涂层经过250g载荷Taber摩擦磨损2000圈后，涂层结构完整，且图7(a)所示，摩擦区域接触角为9.7°，说明仍表现出良好的防雾性能。图8(a)所示，涂层在水中煮沸2h后，由于整体结构保持完整，且图9(a)所示，表面接触角为8.6°，保持良好的亲水性，说明仍具有优异的防雾性能。
实施例2
实施例2形成耐磨、耐煮超亲水涂层的方法同实施例1完全相同，唯一区别在于，实施例2的超亲水涂料中不含埃洛石纳米管。
由于实施例2涂层中的填料仅为球形SiO2纳米颗粒，涂层在受到外力作用时，纳米粒子发生滚动摩擦，更容易偏离其原始位置，使涂层结构受到破坏，相比实施例1涂层耐磨性能出现显著下降。Taber摩擦磨损实验证明，实施例2涂层样品在摩擦500圈后，涂层已经被磨穿，如图6(b)所示，摩擦区域水接触角为27.1°，丧失防雾性能，如图7(b)所示。同时，由于埃洛石纳米管在涂层中的缺失，减小了表面活性剂向水中扩散的阻力，涂层在煮沸1h后防雾性能丧失。
实施例3
实施例3形成耐磨、耐煮超亲水涂层的方法同实施例1完全相同，唯一区别在于，实施例3的超亲水涂料中不含SiO2纳米颗粒。
由于实施例3涂层表面出现少量未被完全包覆的埃洛石纳米管，涂层表面粗糙度增大至11.8nm，导致其水下油接触角减小至116.8°，涂层无自清洁性能。涂层中埃洛石纳米管具有较大的长径比，其在涂层中的位移变化首先是通过滑动和转动实现，只有当受到较大的外力作用时，埃洛石纳米管被破碎，才会在出现类似纳米球状粒的滚动现象，导致涂层的完整性被破坏。为了确保涂层的高透光率，涂层中埃洛石含量较低，未完全分散在整个涂层中，导致涂层大部分区域主要由丙烯酸树脂和氨基树脂等有机组分构成，使涂层的硬度出现显著下降(维氏硬度为73)，Taber摩擦磨损实验证明，样品在摩擦800圈后，摩擦区域大部分涂层已经剥落，如图6(c)所示，摩擦区域接触角增大至27.1°，丧失防雾性能，如图7(c)所示。同时，由于纳米颗粒在涂层中的缺失，导致涂层致密度降低，减小了表面活性剂向水中扩散的阻力，涂层在煮沸1.5h后防雾性能丧失。
实施例4
实施例4形成耐磨、耐煮超亲水涂层的方法同实施例1完全相同，唯一区别在于，实施例4的超亲水涂料中不含正硅酸四乙酯。
由于实施例4涂层的交联程度下降，与玻璃基底结合力较小(10.1MPa)，同时涂层硬度出现显著下降(维氏硬度为80)，导致涂层耐磨性降低，涂层摩擦1200圈后，丧失防雾性能。同时，涂层交联强度的降低，导致其结构在水溶液中被快速破坏，涂层变得疏松多孔，减小了表面活性剂向水中扩散的阻力，涂层在煮沸1.0h后防雾性能丧失。
实施例5
实施例5形成耐磨、耐煮超亲水涂层的方法同实施例1完全相同，唯一区别在于，实施例5的超亲水涂料中不含丙烯酸树脂。
由于实施5涂层各组分之间交联强度下降，使涂层的硬度出现下降(维氏硬度为94)，与玻璃基底结合力较小(9.7MPa)，导致涂层耐磨性降低，涂层摩擦800圈后，丧失防雾性能。同时，未加入丙烯酸树脂导致涂层中氨基树脂未发生充分交联，涂层在煮沸1h后，大部分区域从基底表面脱落，如图8(b)所示，涂层表面水接触角增大至32.3°，丧失防雾性能，如图9(b)所示。
实施例6
实施例6形成耐磨、耐煮超亲水涂层的方法同实施例1完全相同，唯一区别在于，实施例6的超亲水涂料中不含氨基树脂。
由于实施6涂层各组分之间交联强度下降，使涂层的硬度出现下降(维氏硬度为92)，与玻璃基底结合力较小(9.2MPa)，导致涂层耐磨性降低，涂层摩擦800圈后，丧失防雾性能。同时，未加入氨基树脂导致涂层中丙烯酸树脂未发生充分交联，涂层在煮沸1h后，包覆填料树脂的溶解、流失导致涂层完整性丧失，如图8(c)所示，表面水接触角增大至40.6°，丧失防雾性能，如图9(c)所示。
本发明涂层中的填料，纳米粒子和埃洛石纳米管表面存在的大量-OH，与正硅酸四乙酯非完全水解后形成的大量-OH反应，形成的高硬度三维网络结构，丙烯酸树脂与氨基树脂强交联反应形成涂层骨架，使涂层具有极高的强度，同时，活化处理的玻璃表面存在的大量-OH，与涂层中的-OH，-COOH反应，使涂层与基底之间存在强大的结合力，使涂层表现出优异的耐磨性能。同时，由于纳米粒子和埃洛石纳米管被树脂包覆，涂层具有纳米级粗糙度的致密平滑表面，在一定的润湿环境中，能够快速清除其表面的油污和灰尘(润湿环境中，超亲水涂层表面形成一层水膜，将污染物和涂层表面隔离开，污染物随着水膜在涂层表面滑落)，表现出传统超亲水涂层所不具备的自清洁性能。
Claims (9)
1.一种超亲水涂料，其特征在于，由如下质量份数的组分混制而成：1~3份丙烯酸树脂、0.3~1份氨基树脂、2~4份正硅酸四乙酯、1~2份氨水、0.5~2份纳米颗粒、0.2~0.5份纳米管、1~3份阴离子表面活性剂和90~95份水；所述纳米管为埃洛石纳米管，所述纳米管的管径为10~30nm，管长为0.5~2μm。
2.根据权利要求1所述的超亲水涂料，其特征在于：所述涂料的pH值为8~10。
3.根据权利要求1所述的超亲水涂料，其特征在于：所述丙烯酸树脂的分子量为800~1000。
4.根据权利要求1所述的超亲水涂料，其特征在于：所述氨基树脂的分子量为300~600。
5.根据权利要求1所述的超亲水涂料，其特征在于：所述纳米颗粒为二氧化硅或氧化铝中的至少一种，所述纳米颗粒的粒径为5~10nm。
6.根据权利要求1所述的超亲水涂料，其特征在于：所述阴离子表面活性剂为α-烯基磺酸钠、羟乙基磺酸钠、十六烷基磺酸钠或十六烷基硫酸钠中的一种。
7.基于权利要求1所述的超亲水涂料形成耐磨、耐煮超亲水涂层的方法，其特征在于，包括如下步骤：
（1）将清洁处理后的玻璃基底进行活化处理：将玻璃基底先用无水乙醇做去脂处理，然后将玻璃基底放入过氧化氢与浓硫酸的混合溶液中，浸泡10~30s后取出，用水冲洗、干燥后备用；
（2）将涂料以浸涂、喷涂、辊涂或刮涂的方式涂覆在步骤（1）的玻璃基底表面，固化后在玻璃基底表面形成耐磨、耐煮超亲水涂层。
8.根据权利要求7所述的形成耐磨、耐煮超亲水涂层的方法，其特征在于：步骤（1）中，过氧化氢与浓硫酸的混合体积比为3：7；过氧化氢的质量浓度为30%；浓硫酸的质量浓度为98%。
9.根据权利要求7所述的形成耐磨、耐煮超亲水涂层的方法，其特征在于：步骤（2）中，固化条件为在150~220℃下加热15~20min。
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