CN113214703B - 一种水性光固化超疏水涂料及其制备方法与应用 - Google Patents

一种水性光固化超疏水涂料及其制备方法与应用 Download PDF

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CN113214703B
CN113214703B CN202110495819.XA CN202110495819A CN113214703B CN 113214703 B CN113214703 B CN 113214703B CN 202110495819 A CN202110495819 A CN 202110495819A CN 113214703 B CN113214703 B CN 113214703B
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李晖
陈国强
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Suzhou University
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Abstract

本发明涉及一种水性光固化超疏水涂料及其制备方法与应用，属于水性防水涂料领域。该水性光固化超疏水涂料，原料组分及其质量百分比为光固化涂料1～10％，纳米颗粒水相分散液0.5～5％，余量为水；其中，光固化涂料的原料包括疏水剂、交联剂、光引发剂。本发明采用无溶剂法制备，无论是加工过程还是产品应用，都符合国家环保要求，制备方法简单，对设备要求不高，且成本极低，黏度适中，适合多种功能性整理工艺和基底材料，表面张力较低，且涂层的防护耐久性好。

Description

一种水性光固化超疏水涂料及其制备方法与应用
技术领域
本发明涉及水性防水涂料技术领域，尤其是指一种水性光固化超疏水涂料及其制备方法与应用。
背景技术
超疏水涂料因其优异的表面防护性能，如自清洁、防污、防雾、防冰、防腐等，在很多领域得到应用。超疏水涂料通常由较低的表面张力和层次结构粗糙度组成，但是疏水剂通常需要有机溶剂溶解，且疏水涂层包括颗粒，对基底材料粘附力弱，在使用过程中，涂层易脱落和加速流失，而失去表面的超疏水性。随着国家对环保性的要求，水性涂料、光固化涂料和粉末涂料等是国家大力主推的方向，然而粉末涂料因其较高成本、特定的应用领域以及整理条件的苛刻而受到一定的限制。因此，对于大力发展简单、短流程和性能优异的环保型的水性、光固化涂料的要求是迫切的。
发明内容
为解决上述技术问题，本发明提供了一种水性光固化超疏水涂料及其制备方法与应用。该涂料避免了有机溶剂的使用，可适用于多种基底材料，适合工业加工生产，表面疏水性能优异，耐久性优异。
本发明的第一个目的是提供一种水性光固化超疏水涂料，原料组分及其质量百分比为光固化涂料1～10％，纳米颗粒水相分散液0.5～5％，余量为水；其中，光固化涂料的原料包括疏水剂、交联剂、光引发剂；所述疏水剂为不饱和，且具有较低HLB值的表面活性剂。
在本发明的一个实施例中，所述表面活性剂为季戊四醇油酸酯，单取代、双取代和三取代的季戊四醇油酸酯及衍生物，单取代、双取代和三取代的甘油油酸酯及衍生物，单取代和双取代的聚乙二醇油酸酯及衍生物中的一种或多种。
在本发明的一个实施例中，所述交联剂为巯基衍生物，包括3-巯丙基三乙氧基硅烷、3-巯丙基三甲氧基硅烷、2-巯基乙基三乙氧基硅烷、季戊四醇四-3-巯基丙酸酯中的一种或多种。
在本发明的一个实施例中，所述纳米颗粒为聚四氟乙烯、二氧化硅、氧化锌、碳纳米管、各向异性纳米银中的一种或多种。
在本发明的一个实施例中，所述光引发剂为光引发剂1173、光引发剂651、光引发剂184和光引发剂TPO中的一种或多种。
在本发明的一个实施例中，疏水剂、交联剂、光引发剂的质量比为5：2～4：0.5～5。
本发明的第二个目的是提供一种水性光固化超疏水涂料的制备方法，包括如下步骤：
(1)将疏水剂、交联剂、光引发剂按配比搅拌共混，然后置于紫外光源下照射，得到光固化涂料；
(2)将步骤(1)得到的光固化涂料加入水中，搅拌分散，得到乳白色的均相溶液，后加入纳米颗粒水相分散液，再次搅拌分散，得到所述水性光固化超疏水涂料。
在本发明的一个实施例中，在步骤(1)中，所述照射的时间为2～8h，光照的强度为0.5～5mW cm-2。
本发明的第三个目的是应用所述的水性光固化超疏水涂料在涂层中的应用，包括以下步骤：通过浸涂、轧烘焙、旋涂或喷涂工艺，将所述水性光固化超疏水涂料整理到基底材料表面，得到涂层产品。
在本发明的一个实施例中，所述基底材料为软基底材料和硬基底材料；其中，软基底材料为纤维素纤维、蛋白质纤维、合成纤维及其混纺织物、海绵或滤膜；硬基底材料为玻璃、金属、木板、盒子或钢化膜；所述软基底材料适用于浸涂整理，硬基底材料适用于旋涂或喷涂整理。
本发明的上述技术方案相比现有技术具有以下优点：
(1)本发明的光固化涂料，采用无溶剂法制备，无论是加工过程还是最终产品应用，都符合国家环保要求，制备方法简单，对设备要求不高，且成本极低，黏度适中，适合多种功能性整理工艺和基底材料，表面张力较低，且涂层的防护耐久性好。
(2)本发明的水性涂料为基于不饱和的极低HLB值的表面活性剂与巯基衍生物制备的的光固化涂料的水相分散液，其中光固化涂料可以水相分散，且该类型的表面活性剂种类多样，包括不同的官能度、取代基和油酸来源等，交联剂也可基于涂层的成膜和牢度等需求而替换，包括不同官能度和与基底材料的可反应性，纳米颗粒粗糙度可以用其他可水分散的纳米颗粒替换，引入耐磨、不粘、染色、导电、抗菌、光催化、抗紫外、电磁屏蔽等。
(3)本发明的水性光固化超疏水涂料适用于多种基底，不仅可以满足家具、纺织品的功能性需求，还可应用于某些特殊应用领域，如钢材、海洋防腐、食品浪费、高档玻璃仪器设备、触屏电子产品等，具备极高的应用和产业价值。
附图说明
图1是实施例1光固化涂料形态的光学图。
图2是实施例1不添加聚四氟乙烯分散液的光固化涂料水相分散液的光学图。
图3是实施例1添加聚四氟乙烯分散液后的水性光固化超疏水涂料分散液的光学图。
图4是实施例1水性光固化超疏水涂料静置一个月后的光学图。
图5是实施例1棉织物原样的SEM微观图。
图6是实施例1整理棉织物表面的SEM微观图。
图7是实施例1棉织物功能涂层耐水洗性能。
图8是实施例1棉织物功能涂层的耐摩擦性能。
具体实施方式
下面结合附图和具体实施例对本发明作进一步说明，以使本领域的技术人员可以更好地理解本发明并能予以实施，但所举实施例不作为对本发明的限定。
实施例1
一种水性光固化超疏水涂料的制备方法与应用，包括以下步骤：
(1)将季戊四醇油酸酯、3-巯丙基三乙氧基硅烷和光引发剂1173按质量比5：4：1加入石英烧杯中，以100克计量，磁力搅拌均匀，然后将石英烧杯置于紫外灯源下照射4h，光照强度2.5mW cm-2，即得到光固化涂料。
(2)将步骤(1)制备的光固化涂料加入到去离子水中，在1000rpm机械搅拌得到乳白均相溶液，然后加入2.5wt％聚四氟乙烯水相分散液，并再次机械搅拌均匀，即得到水性光固化超疏水涂料。
(3)将棉织物置于步骤(2)制备的水性光固化超疏水涂料中浸渍5分钟，然后过轧辊除去多余整理液，二浸二轧，并置于180℃焙烘10min，最后于140℃下烘干1h，即得到功能棉织物。
实施例2
一种水性光固化超疏水涂料的制备方法与应用，包括以下步骤：
(1)将单取代甘油油酸酯、季戊四醇四-3-巯基丙酸酯和光引发剂651按质量比5：4：3加入石英烧杯中，磁力搅拌均匀，然后将石英烧杯置于紫外灯源下照射6h，光照强度0.5mW cm-2，即得到光固化涂料。
(2)将步骤(1)制备的光固化涂料加入到去离子水中，在1000rpm机械搅拌得到乳白均相溶液，然后加入0.5wt％二氧化硅水相分散液，并再次机械搅拌均匀，即得到水性光固化超疏水涂料。
(3)将尼龙织物置于步骤(2)制备的水性光固化超疏水涂料中浸渍5分钟，然后过轧辊除去多余整理液，二浸二轧，并置于180℃焙烘10min，最后于140℃下烘干1h，即得到功能棉织物。
实施例3
一种水性光固化超疏水涂料的制备方法与应用，包括以下步骤：
(1)将双取代的聚乙二醇油酸酯、2-巯基乙基三乙氧基硅烷和光引发剂184按质量比5：4：5加入石英烧杯中，磁力搅拌均匀，然后将石英烧杯置于紫外灯源下照射8h，光照强度5mW cm-2，即得到光固化涂料。
(2)将步骤(1)制备的光固化涂料按量加入到去离子水中，在1000rpm机械搅拌得到乳白均相溶液，然后加入5wt％氧化锌水相分散液，并再次机械搅拌均匀，即得到水性光固化超疏水涂料。
(3)将海绵置于步骤(2)制备的水性光固化超疏水涂料中浸渍5分钟，然后过轧辊除去多余整理液，二浸二轧，并置于180℃焙烘10min，最后于140℃下烘干1h，即得到功能棉织物。
测试例
对实施例1制备所得的光固化涂料、水性光固化超疏水涂料以及功能产品采用如下的方法进行测试：
1、粒径测试
将实际功能性整理对应浓度的水性光固化超疏水涂料整理液，使用马尔文电位粒径分析仪(Malvern Zetasizer Nano ZS90)对聚四氟乙烯颗粒的粒径进行测试，测试结果表明光固化涂料可以在水相均匀分散，且稳定性良好，静置1到3个月，涂料没有明显沉降等，粒径尺寸在150nm左右。
2、透射电镜测试
将实际功能性整理对应浓度的水性光固化超疏水涂料整理液过铜网后，置于灯下炙烤烘干，使用透射电子显微镜(JEOL JEM 2100F)对聚四氟乙烯颗粒的形貌以及聚四氟乙烯颗粒与光固化涂料的结合情况进行测试。测试结果表明，本实施制备的水性光固化超疏水涂料整理液中光固化涂料包覆在聚四氟乙烯颗粒表面。
3、光固化涂料透明度测试
在室温条件下，使用紫外可见光分光光度计(TU-1900)对光固化涂料透明度进行测试。结果如图1所示，光固化涂料显示高度透明性，透明度>95％，适合一些玻璃制品、仪器设备以及触屏电子设备等特定产品领域的防水要求。
4、接触角测试
在室温条件下，采用光学接触角测量仪(DataPhysics OCA20)对棉织物表面的疏水性能进行测试，水滴为6μl，取不同位置的接触角值取其平均值。测试结果表明棉织物表面疏水角约为168°，滚动角<5°，具有一个优异的表面超疏水性能。
5、样品微观结构表征
通过场发射冷场电镜(SEM)对棉织物微观结构进行表征，结果如图5所示，棉织物表面是光滑整洁的，除了一些有的褶皱结构之外，然而经水性涂料整理之后，如图6所示，我们能很明显的看到纤维表面被涂层所遮盖，代表水性涂料被整理到棉织物表面，这带来了其表面超疏水性。
6、水洗测试
根据AATCC 61-2006method标准，将棉织物置于200毫升的洗涤剂中(50个钢珠)49℃洗涤45分钟，为1个循环，相当于五个常规家庭洗涤标准。结果如图7所示，将水性光固化超疏水涂料整理到棉织物表面，具有良好的耐久性，可经受至少15次加速洗涤(相当于家庭洗涤75个循环)和1000个马丁旦尔摩擦循环，而保持表面超疏水性。
7、摩擦测试
根据ASTM D4966标准，使用马丁旦尔织物平磨仪来摩擦棉织物，负载压力为12kPa。结果如图8所示，将水性光固化超疏水涂料整理到棉织物表面，具有良好的耐久性，可经受至少1000个马丁旦尔摩擦循环，而保持表面超疏水性。
从图2～4可知，光固化涂料在水相中分散良好，在加入聚四氟乙烯颗粒后，也不影响其在水相当中的分散，且稳定性良好，且至少保持1个月以上而不发生丝毫沉降。
显然，上述实施例仅仅是为清楚地说明所作的举例，并非对实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。

Claims (8)

1.一种水性光固化超疏水涂料，其特征在于：原料组分及其质量百分比为光固化涂料1～10％，纳米颗粒水相分散液0.5～5％，余量为水；
其中，光固化涂料的原料包括疏水剂、交联剂、光引发剂；
所述疏水剂为季戊四醇油酸酯，单取代、双取代和三取代的季戊四醇油酸酯及衍生物，单取代、双取代和三取代的甘油油酸酯及衍生物，单取代和双取代的聚乙二醇油酸酯及衍生物中的一种或多种；
所述交联剂为3-巯丙基三乙氧基硅烷、3-巯丙基三甲氧基硅烷、2-巯基乙基三乙氧基硅烷、季戊四醇四-3-巯基丙酸酯中的一种或多种。
2.根据权利要求1所述的水性光固化超疏水涂料，其特征在于：所述纳米颗粒为聚四氟乙烯、二氧化硅、氧化锌、碳纳米管、各向异性纳米银中的一种或多种。
3.根据权利要求1所述的水性光固化超疏水涂料，其特征在于：所述光引发剂为光引发剂1173、光引发剂651、光引发剂184和光引发剂TPO中的一种或多种。
4.根据权利要求1所述的水性光固化超疏水涂料，其特征在于：疏水剂、交联剂、光引发剂的质量比为5：2～4：0.5～5。
5.根据权利要求1～4任一项所述的水性光固化超疏水涂料制备方法，其特征在于，包括如下步骤：
(1)将疏水剂、交联剂、光引发剂按配比搅拌共混，然后置于紫外光源下照射，得到光固化涂料；
(2)将步骤(1)得到的光固化涂料加入水中，搅拌分散，得到乳白色的均相溶液，后加入纳米颗粒水相分散液，再次搅拌分散，得到所述水性光固化超疏水涂料。
6.根据权利要求5所述的水性光固化超疏水涂料制备方法，其特征在于：在步骤(1)中，所述照射的时间为2～8h，光照的强度为0.5～5mWcm-2。
7.根据权利要求1～4任一项所述的水性光固化超疏水涂料在涂层中的应用，其特征在于，包括以下步骤：通过浸涂、轧烘焙、旋涂或喷涂工艺，将所述水性光固化超疏水涂料整理到基底材料表面，得到涂层产品。
8.根据权利要求7所述的水性光固化超疏水涂料在涂层中的应用，其特征在于：所述基底材料为软基底材料或硬基底材料；
其中，软基底材料为纤维素纤维、蛋白质纤维、合成纤维及其混纺织物、海绵或滤膜；硬基底材料为玻璃、金属、木板、盒子或钢化膜；
所述软基底材料适用于浸涂整理，硬基底材料适用于旋涂或喷涂整理。
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