CN112211003B - 一种基于泡沫整理技术的多功能超疏水表面制备方法 - Google Patents

一种基于泡沫整理技术的多功能超疏水表面制备方法 Download PDF

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CN112211003B
CN112211003B CN202011235914.8A CN202011235914A CN112211003B CN 112211003 B CN112211003 B CN 112211003B CN 202011235914 A CN202011235914 A CN 202011235914A CN 112211003 B CN112211003 B CN 112211003B
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黄剑莹
谢孝文
赖跃坤
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Abstract

本发明提供了一种基于泡沫整理技术的多功能超疏水表面制备方法，该方法包括以下步骤：（1）将聚二甲基硅氧烷和固化剂加入到去离子水中，进行搅拌，随后加入表面活性剂，再加入气相二氧化硅纳米颗粒，继续搅拌，得到疏水整理液；（2）上述制备好的疏水整理液通过机械搅拌至发泡，将产生的泡沫施加到织物上，并将织物放入烘箱中干燥，即可获得长效持久的多功能超疏水织物。通过该方法制备超疏水表面织物无需使用有机溶剂，对环境污染小，且处理Z织物需要的整理液较少，节约成本，同时由于泡沫整理技术处理无需将织物浸泡，可以制备单面疏水或双面疏水的织物，以及处理一些浸水易损坏的物品，泛用性强。

Description

一种基于泡沫整理技术的多功能超疏水表面制备方法
技术领域
本发明涉及一种基于泡沫整理技术的多功能超疏水表面制备方法，属于纺织品功能整理技术领域。
背景技术
衣服是人们日常生活中必不可少的物品，棉质衣服具有透气性好，可生物降解，穿着舒适等特点，但也因其良好的亲水性和吸湿性，容易沾染污渍。
随着织物表面处理技术的发展，研究者通过仿生自然界中荷叶等超疏水表面，获得了超疏水织物，该超疏水织物具有自清洁、防污等功能，受到了人们的广泛关注。但是目前超疏水功能织物大规模工业化还有很多制约因素，一是超疏水功能需要用到低表面能的疏水剂改性，而不含氟的疏水剂材料用通常方法难以保证疏水性；二是由于疏水剂的疏水性，配置整理液时通常需要使用各种有机溶剂使疏水剂溶解，而有机溶剂的大量使用会严重危害环境以及作业人员的人身安全。不仅如此，传统织物整理方法还要消耗大量的水资源，同时产生大量的印染废水，若处理不当则会造成严重危害环境，若完全处理则会大大提高生产成本，制约我国纺织产业迈向中高端市场。此外，传统的浸轧方法需要将物料完全浸入到整理液中，对于一些蓄水性能较强的物料，浸渍处理后带液率较高，导致后续的干燥成型麻烦，使得生产效率低下。
根据工信部发布的《印染行业绿色发展技术指南（2019版）》，推动印染行业绿色发展，事关人民对美好生活新期待，事关纺织工业可持续发展，事关污染防治攻坚战取得胜利。在这一背景下，泡沫整理这一绿色环保技术再次成为大家关注的焦点。泡沫整理技术通过引入发泡剂，将整理液转化成泡沫，进而将泡沫施加到织物表面，渗入织物内部，对织物进行整理。相比传统纺织品浸轧方法，泡沫整理技术能使织物带液率由60%-80%下降到20%-40%，用水量降低50%左右，染化料和助剂用量降低30%左右，在烘燥环节可节能40%左右。如何将泡沫整理技术完美地利用在织物表面处理领域，实现绿色高效的超疏水表面制备是值得研究的方向。
发明内容
为了解决上述问题，本发明提供了一种基于泡沫整理技术的多功能超疏水表面制备方法，通过泡沫整理技术制备表面带有含气相纳米二氧化硅的聚二甲基硅氧烷涂层的多功能超疏水织物，实现了在不含有机溶剂的水性环境下的超疏水织物制备。
为了达到上述效果，本发明采用了以下技术方案：
一种基于泡沫整理技术的多功能超疏水表面制备方法，其特征在于，该方法包括以下步骤：
S1：将聚二甲基硅氧烷和固化剂加入到去离子水中，进行搅拌，随后加入表面活性剂，再加入气相二氧化硅纳米颗粒，继续搅拌，得到疏水整理液；
S2:上述制备好的疏水整理液通过机械搅拌至发泡，将产生的泡沫施加到织物上，并将织物放入烘箱中干燥，即可获得长效持久的多功能超疏水织物。
本发明方法包括两个步骤，第一个步骤为疏水整理液的制备，第二个步骤为泡沫整理技术在织物表面的应用和实施。聚二甲基硅氧烷是一种疏水的油状液体，无法直接与去离子水混合成溶液，因此需要添加表面活性剂，表面活性剂具有亲水端和疏水端，能够与水相和油相相融，使两者形成浑浊液，不再分层，同时表面活性剂也具有发泡作用，当浑浊液受到剧烈搅拌时，会产生大量泡沫。气相二氧化硅是一种多孔白色蓬松粉末，它具备的化学惰性以及特殊的触变性能明显改善制品的抗拉强度，抗撕裂性和耐磨性，可以起到增强织物疏水表面层的使用寿命的作用，还能增强弹性，使得织物发生拉伸时表面层的因为具有较强的延伸性而不至于出现撕裂现象。此外，气相二氧化硅还具有消泡作用，可以将加入表面活性剂后产生的泡沫消除，避免部分原料混杂在泡沫中导致液体搅拌不均匀。第二步中需要先通过机械搅拌的方式使整理液发泡，随后将产生的泡沫均匀涂覆在织物的表面，并进行干燥处理。在烘箱干燥过程中，水分逐渐流失，固化剂发挥作用，使得液状的聚二甲基硅氧烷封端形成固态的疏水表面层，由于泡沫具有一定渗入性，疏水表面层并不仅仅附着在织物表面，而是与织物形成一定交联关系，从而得到长效持久的具有疏水表面层的织物。
此外，需要说明的是，上下文中提到的“织物”并不局限于天然纤维或人造纤维纺织形成的布料，还包括无纺布、以及纸张等可作为涂层载体的片装基材。下文中所提到的配比均为质量比。
进一步地，表面活性剂的成分为十二烷基硫酸钠和十二烷醇中的一种或多种。
十二烷基硫酸钠是一种高效的发泡剂，相较于十二烷基磺酸钠而言具有更好的亲水性，使得油水两相的混合度更高，且价格低廉，生物毒性低，适用于与人体直接接触的织物的处理。十二烷醇一方面可以作为起泡剂用，另一方面通过调整十二烷醇和十二烷基磺酸钠的配比可以调整泡沫的表面粘度，进而调整泡沫的寿命。当十二烷醇相对含量升高时，表面粘度升高，泡沫寿命一定程度上会提高，使得操作过程中不会因为泡沫快速消解而影响效果。
进一步地，表面活性剂中包含十二烷基硫酸钠和十二烷醇，且十二烷基硫酸钠与十二烷醇的配比为1:0.2~1:0.8。
如上文所述，十二烷醇的加入会使泡沫表面粘度升高，提高泡沫寿命，当十二烷醇添加含量过高时，会导致泡沫表面粘度过高，在施加到织物表面后，可能会导致烘干处理过程时间过长以及涂层厚度不均匀的问题。
进一步地，聚二甲基硅氧烷与固化剂的配比为1:0.01~1:1。
聚二甲基硅氧烷为油状液体，若要使其附着在织物表面上，则需对其高分子链进行固化处理，使其形成稳定的疏水层。聚二甲基硅氧烷在市场上购买时往往具有配套的固化剂，如道康宁184组分A和道康宁184组分B，前者是聚二甲基硅氧烷预聚物，后者是对应的固化剂，固化剂成分通常为一些硅烷偶联剂，如A151、A171、A172等。
进一步地，聚二甲基硅氧烷与表面活性剂的配比为1:0.2~1:0.4。
表面活性剂加入的量太多的话可能会导致体系中出现反乳化现象，即原本在体系中分散的细小油滴汇聚成大油滴，重新与水相分离。此外还会导致混合体系中液体粘度增大，使得后续机械搅拌形成泡沫的过程变得困难。
进一步地，聚二甲基硅氧烷和气相二氧化硅纳米颗粒的配比为1:0.4~1:1.2。
进一步地，机械搅拌的转速为300~3500r/min，搅拌时间为20~1500s。
机械搅拌的转速和搅拌时间呈负关系，由于搅拌以得到泡沫为目的，当转速大的时候容易快速得到泡沫，需要的搅拌时间相对较短，转速慢则需要更多搅拌时间。此外，转速需要维持在合适的范围，若转速过慢，则搅拌棒难以将空气鼓入到液体中而形成泡沫，若搅拌过快会消耗过多能量，造成浪费，且还有可能导致液体飞溅。
进一步地，织物在烘箱中的干燥温度为40~200℃，干燥时间为15~240min。
干燥温度和干燥时间应当成负相关，在较高温度下泡沫的裂解和表面疏水层的固化速率较快，需要的固化时间也较短，例如200℃下，干燥时间应当在15~20min，若时间过长，一方面浪费能源、影响效率，另一方面长时间暴露在高温下，织物以及表面层可能会出现质量下降的问题。
进一步地，所述的S1步骤中，搅拌方式为超声波振荡搅拌。
由于第一步配置疏水整理液时需要先后加入多种原料，此时采用机械搅拌一方面不利于原料的添加，另一方面在加入表面活性剂之后机械搅拌容易产生泡沫，影响物料的均匀混合。
进一步地，所述的S1步骤中制得的疏水整理液中还添加有织物染料。
本发明在配置疏水整理液时，可预先加入用于织物染色的染料，在最后对织物涂覆泡沫处理时可附带起到染色作用。
综上所述，本发明具有以下优点：
1、本发明采用水性整理液对织物进行处理，无需使用大量的有机溶剂，且原料中不使用含氟添加剂，对环境友好，保障操作人员的人身安全，同时降低生产成本。
2、本发明采用泡沫整理技术对织物进行处理，使得处理后的织物带液率少，易于后续的干燥成型处理，使后续处理更加简单高效，同时处理织物时需要消耗的整理液也大大减少，节省了原料使用，降低成本。
3、本发明采用的泡沫整理技术可以仅对织物进行单面处理，使织物的受处里面形成超疏水结构，而另一面依然为吸水结构，在穿着衣物时，可以有效防止外界液体污染，同时保证布料的吸汗性，对穿着舒适度影响较小；同样地，也可以使用添加了不同种类染料的疏水整理液对布料的两面进行处理，从而得到双面异色的织物产品，或者对织物同一面的不同区域使用不同颜色的疏水整理液泡沫处理，得到多种色块或花纹组合。
4、本发明处理时对基底的破坏性小，适用于多种基底表面，包括但不限于棉麻等天然纤维织物、涤纶和腈纶等人造纤维织物甚至纸张等片装结构基底，具有广泛的适用性，有望实现功能性超疏水织物的大规模产业化。
附图说明
图1是通过本发明方法处理得到的超疏水织物表面结构的扫描电子显微镜图像以及水接触角图；
图2是通过本发明方法制备的超疏水织物对几种常见液体的拒液效果照片，从左到右四种液体依次为蜂蜜水、牛奶、咖啡水和茶水；
图3是通过本发明方法制备超疏水织物经过270天放置后的水接触角图；
图4是通过本发明方法制备的亲/疏水Janus织物的效果展示图片；
图5是通过本发明方法制备的双面异色超疏水织物效果展示图片，其中正面为红色，背面为蓝色；
图6是通过本发明方法制备的单面多色超疏水织物效果展示图片；
图7是通过本发明方法制备的基于不同基材的超疏水织物效果展示图片，所选基材依次为普通A4纸（左上）、滤纸（右上）、涤纶面料（左下）和三聚氰胺海绵（右下）。
具体实施方式
下面结合具体实施例对本发明做进一步说明，但本发明不仅仅限于这些实施例。
实施例1
1）制备疏水整理液：将0.6 g的聚二甲基硅氧烷和0.06g的配套固化剂加入到去离子水中，超声振荡并剧烈搅拌，然后加入0.1 g的十二烷基硫酸钠和0.04 g的十二烷醇，继续加入0.6 g的气相二氧化硅纳米颗粒，在超声振荡作用下剧烈搅拌，得到疏水整理液；
2）施加泡沫整理织物：上述制备好的疏水整理液用搅拌器在2500 r/min转速下搅拌180 s至发泡，将疏水泡沫施加到涤纶面料上并放入150℃烘箱中干燥120 min，由此便获得长效持久的多功能超疏水织物。
处理后的涤纶面料通过扫描电子显微镜观察其表面结构，扫描电子显微镜照片如图1所示。将涤纶面料平放，向涤纶面料的超疏水处理面上滴加去离子水，得到的水接触角图如图1右上角所示。将织物在阴凉干燥环境中放置270天后，再次向超疏水处理面滴加去离子水，得到的水接触角图如图3所示，水接触角为153.1°。通过电镜图可以看出，通过本发明处理后的织物表面的线状纤维表面附着形成了一层不规则的表面结构，而水接触角图证实了该表面结构具有良好的疏水性，且该疏水结构在经过长时间存放后依然与最初时的疏水性相当，具有良好的稳定性。
配制蜂蜜水、牛奶水、咖啡水和茶水四种常见的饮料液体，将制得的超疏水织物平放，依次向疏水面滴加上述四种液体，得到的效果图如图2所示。根据图2可以看出，对四种常见的饮料，本发明制得的超疏水织物均具有优异的抗拒效果，证实了本发明具有良好的泛用性。
实施例2
1）制备疏水整理液：将1.5 g的聚二甲基硅氧烷和0.15g的配套固化剂加入去离子水中，超声振荡并剧烈搅拌，然后加入0.3 g的十二烷基硫酸钠和0.1 g的十二烷醇，再加入1.5 g的气相二氧化硅纳米颗粒，继续在超声振荡作用下剧烈搅拌，得到疏水整理液；
2）施加泡沫整理织物：上述制备好的疏水整理液用搅拌器在2000 r/min转速下搅拌240 s至发泡，将疏水泡沫施加到涤纶面料上，通过控制疏水泡沫的量，使涤纶面料的一面整理上疏水泡沫，另一面尽量保留其原本浸润性。将上述整理好的织物放入150℃烘箱中干燥100 min，由此便获得长效持久的亲/疏水Janus织物表面。
将制备得到的亲/疏水Janus织物表面平放，疏水面朝上，侧边部分折叠使非疏水处理面部分暴露在上，分别向疏水面和非疏水面滴加带有墨水的水滴，效果图如图4所示，其超疏水面的接触角为153.8°，亲水面的接触角为50.4°。
由于添加了墨水，水滴的浸润效果可以较为直观的看到，根据图4可以看到，左侧滴加在非疏水面的水滴扩散开来，被布料吸收，而右侧滴加在疏水面的水滴则保持抗拒状态，没有被布料吸收。通过该图，可以证实本发明能够完成对织物的单面疏水处理，使其非处理面依旧保持良好的吸水性能，因此可以用于贴身衣物的防水处理，既保证外侧具有防水效果，又能保证内侧具有吸汗功能。
实施例3
1）制备疏水整理液：将1.2 g的聚二甲基硅氧烷和0.15g的配套固化剂加入去离子水中，超声振荡并剧烈搅拌，然后加入0.2 g的十二烷基硫酸钠和0.12 g的十二烷醇，再加入0.8 g的气相二氧化硅纳米颗粒，继续超声振荡作用下剧烈搅拌，得到疏水整理液。将疏水整理液分成A和B两份，A中添加蓝色染料亚甲基蓝，B中添加红色染料赤藓红B钠盐。
2）施加泡沫整理织物：上述制备好的两份染色疏水整理液分别用搅拌器在2500r/min转速下搅拌120 s至发泡，将少量A中产生的蓝色泡沫施加在厚棉布其中一面上，放入150℃烘箱干燥5 min，取出，再在另一面涂覆少量B中产生的红色泡沫，之后放入150℃烘箱中干燥120 min，由此便获得长效持久的双面异色超疏水织物。
制备得到的双面异色超疏水织物如图5所示，其中左上角为蓝色面疏水效果示意图，右上角为红色面疏水效果示意图。同理，在使用更多种不同染料后，在制备超疏水层时，也可以在单面上形成多种不同颜色的色块和花纹，如图6所示，图中每一块不同的色块区域均代表不同的染色颜色。
实施例4
1）制备疏水整理液：将0.8 g的聚二甲基硅氧烷和0.10g的配套固化剂加入去离子水中，超声振荡并剧烈搅拌，然后加入0.15 g的十二烷基硫酸钠和0.08 g的十二烷醇，再加入0.8 g的气相二氧化硅纳米颗粒，继续超声振荡作用下剧烈搅拌，得到疏水整理液。
2）施加泡沫整理不同基底：上述制备好的疏水整理液用搅拌器在2200 r/min转速下搅拌150 s至发泡，将泡沫分别施加在普通A4纸、滤纸、涤氨面料和三聚氰胺海绵上，放入140℃烘箱中干燥150 min，由此获得各种基底表面的长效持久多功能超疏水材料。
向四种不同基材制得的超疏水产品的疏水面上滴加水滴，得到的效果图如图7所示。根据图7可以看出，对于不同的基材，本发明方法均有良好的适用性，得到的产品也都具有良好的疏水效果。因此本发明方法并不局限于传统的织物表面处理，也可用作其他防水处理，如记事本的封面防水处理等。
综上所述，本发明方法处理得到的产品具有优异的疏水效果，面对多种常见的易造成衣物污染的液体均产生了抗拒作用，达到了防止衣物污染的效果。且本发明方法由于不需要对基材进行浸没，对基材破坏性小，因此对多种不同的基材均具有良好的适用性，甚至纸张这种遇水易破损的基材也可以用该方法处理，达到疏水效果。此外，同样由于无需对基材浸没处理，本发明可以实现单面疏水、双面疏水、双面异色、单面不同区域异色等传统漂染方法难以实现效果，具有较高的生产实用价值。
以上实施例仅仅是对本发明的解释和具体实施方式和实施效果进行举例，其并不是对本发明的限制，本领域技术人员在阅读完本说明书后可以根据需要对发明做出没有创造性贡献的修改，但只要在本发明的权利要求范围内都受到专利法的保护。

Claims (3)

1.一种基于泡沫整理技术的多功能超疏水表面制备方法，其特征在于，该方法包括以下步骤：
S1：将聚二甲基硅氧烷和固化剂加入到去离子水中，进行搅拌，随后加入表面活性剂，再加入气相二氧化硅纳米颗粒，继续搅拌，得到疏水整理液；
S2：上述制备好的疏水整理液通过机械搅拌至发泡，将产生的泡沫施加到织物上，并将织物放入烘箱中干燥，即可获得长效持久的多功能超疏水织物；
表面活性剂中包含十二烷基硫酸钠和十二烷醇，且十二烷基硫酸钠与十二烷醇的配比为1:0.2~1:0.8；
聚二甲基硅氧烷与固化剂的配比为1:0.01~1:1；
聚二甲基硅氧烷与表面活性剂的配比为1:0.2~1:0.4；
聚二甲基硅氧烷和气相二氧化硅纳米颗粒的配比为1:0.4~1:1.2；
机械搅拌的转速为300~3500r/min，搅拌时间为20~1500s；
所述的S1步骤中，搅拌方式为超声波振荡搅拌。
2.根据权利要求1所述的一种基于泡沫整理技术的多功能超疏水表面制备方法，其特征在于，织物在烘箱中的干燥温度为40~200℃，干燥时间为15~240min。
3.根据权利要求1所述的一种基于泡沫整理技术的多功能超疏水表面制备方法，其特征在于，所述的S1步骤中制得的疏水整理液中还添加有织物染料。
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