CN114517405B - 一种耐久超疏水棉织物及其制备方法 - Google Patents
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Abstract
本发明提供了一种耐久超疏水棉织物及其制备方法，将高碘酸钠氧化后的棉织物常温下置于硝酸银中30‑60min，接下来浸渍在十八胺‑KH560改性Ti3C2Tx/TiO2分散液中进行浸轧整理，两浸两轧，控制轧余率100％，80℃烘干2min，120℃定型5min，最终制备得到一种具有耐水洗、耐超声、耐弯折、耐强酸/碱等特性的耐久超疏水棉织物。十八胺‑KH560改性Ti3C2Tx/TiO2与棉织物之间的附着力牢固，不易从棉织物表面脱落，从而使得超疏水性能具有长效性。此外，耐久超疏水棉织物还具备抗菌/抗病毒、抗紫外、电磁屏蔽、导电等功能。
Description
技术领域
本发明涉及纳米材料和纺织领域，具体涉及一种耐久超疏水棉织物及其制备方法。
背景技术
超疏水表面通常是通过低表面能物质的修饰以及微纳粗糙结构的构筑来实现的。由于其特殊的表面润湿性，不仅在自清洁、表面防腐、油水分离和防结冰等领域表现出诱人的前景，而且在日常生活、生物医学和军事等领域也具有潜在的应用价值。但是在实际应用过程中，低表面能物质容易受到温度、光照和强氧化剂等作用的刺激发生分解，微纳粗糙结构也容易在机械摩擦或磨损等物理作用下受到破坏，从而影响涂层的黏附力和润湿性，导致超疏水性能下降或丧失，限制其应用。因此，制备耐久型超疏水表面是超疏水材料能够真正得以应用的关键。一般来说，超疏水表面耐磨性差的主要原因是超疏水表面与基材间的附着力差，易从基材表面脱落(化工进展,2020,39(12):5148-5160)。
过渡金属碳化物、氮化物和碳氮化物(通常称为MXenes)是自2011年YuryGogotsi等发现碳化钛(Ti3C2Tx)以来的一类新型二维材料。这些材料的一般公式为Mn+1XnTx(n＝1、2或3)，其中M是早期过渡金属，X是碳和/或氮，T是从合成过程中继承的表面基团，通常为-OH、-O和-F。MXenes通常由三元碳化物或氮化物的MAX相选择性地刻蚀A原子层制得，其中A主要是IIIA族和IVA族元素。迄今为止报道的MAX相有70多种，目前20多种基于Ti、V、Nb、Mo、Ta和Zr等的MXenes被成功合成。这种化学和结构上的多功能性使得MXenes在高导电性、大表面积等方面具有与石墨烯等其它二维纳米材料的竞争优势，在多种应用领域特别是在电池、超级电容器和催化等能量转换和储能领域有着广阔的应用前景(Advanced FunctionalMaterials,2020,2000712；Advanced optical Materials,2020,2001120；材料导报,2022,36(04):19-28；复合材料学报,2022,39(02):467-477；材料工程,2022,50(01):43-55；人工晶体学报,2021,50(11):2183-2191；复合材料学报,2022,39(02):460-466)。
目前，基于MXene的超疏水纺织品的文献很少。而且绝大部分超疏水纺织品都是将纺织品直接浸泡在低表面能物质如聚二甲基硅氧烷(PDMS)中，低表面能物质与纺织品之间缺乏牢固的结合。例如Li采用逐层组装的方法开发了一种多功能纺织品，该纺织品具有优越的不对称超疏水性、优异的电磁干扰(EMI)屏蔽、出色的光热转换性能和太阳能水蒸发性能。SiO2纳米颗粒/聚二甲基硅氧烷(PDMS)和1H、1H、2H、2H全氟辛基三乙氧基硅烷(PFOTES)的协同效应使纺织品具有高达160°的水接触角。MXene则为多功能纺织品提供了高导电性(1200S/m)和EMI屏蔽效果(36dB)(ACS Applied Materials&Interfaces,2021,13(24):28996-29007)。
发明内容
针对上述不足，本发明提供了一种耐久超疏水棉织物及其制备方法。
本发明通过如下的技术方案实现：
使用乙醇反复超声棉织物，真空烘干，使用高碘酸钠对上述棉织物在避光条件下进行轻度氧化，去离子水反复清洗，真空烘干后，常温下置于1-100g/L硝酸银中30-60min，取出后真空烘干，接下来浸渍在十八胺-KH560改性Ti3C2Tx/TiO2分散液中进行浸轧整理，两浸两轧，控制轧余率100％，80℃烘干2min，120℃定型5min，最终制备得到耐久超疏水棉织物。
详细制备步骤如下：
(1)使用十八胺改性KH560制备十八胺-KH560：配置体积分数为1-10％的硅烷偶联剂KH560乙醇溶液，混合均匀后，再加入十八胺，所述十八胺与硅烷偶联剂KH560的质量比为0.1-1，70-90℃加热回流反应6-12h，得到十八胺-KH560。
(2)高温煅烧氧化Ti3C2Tx制备Ti3C2Tx/TiO2纳米复合材料：将9mol/L体积40mL的HCl缓慢倒入聚四氟乙烯烧杯中，加入2g的LiF，常温下400rpm磁力搅拌30min，以完全溶解LiF；随后将2g的Ti3AlC2粉末缓慢加入到蚀刻溶液中，室温下磁力搅拌24h；待反应结束后，使用去离子水清洗数次，3500rpm离心，直至pH值≥6；然后将黑色沉淀物重新分散到1:1水/乙醇混合溶剂中，10000rpm离心10min；使用去离子水洗涤所得沉淀物，3500rpm继续离心数次后，收集上清液，通过离心和冷冻干燥，得到单层Ti3C2Tx粉末；将所述单层Ti3C2Tx纳米片粉末放入管式炉中，氩气氛围中60℃持续干燥24h，然后以5℃/min的升温速率升到500℃-600℃，保温2h，冷却至室温，得到Ti3C2Tx/TiO2纳米复合材料。
(3)将Ti3C2Tx/TiO2纳米复合材料缓慢加入十八胺-KH560溶液中反应24h，即可制备得到十八胺-KH560改性Ti3C2Tx/TiO2。
(4)使用乙醇反复超声棉织物，真空烘干。将上述棉织物浸渍在2g/L高碘酸钠水溶液中，浴比1：50，避光条件下60-80℃氧化10-30min，去离子水反复清洗，真空烘干。然后常温下置于1-100g/L硝酸银中30-60min，取出后真空烘干，接下来浸渍在十八胺-KH560改性Ti3C2Tx/TiO2分散液中进行浸轧整理，两浸两轧，控制轧余率100％，80℃烘干2min，120℃定型5min，最终制备得到耐久超疏水棉织物。
本发明的有益效果：(1)表面自由能和表面几何结构是材料表面润湿性的两个决定性的影响因素，因此设计制备超疏水表面的途径有2条：一是在材料表面构建微纳粗糙结构；二是在材料表面修饰低表面能物质。本发明的微纳粗糙结构由TiO2和纳米银共同赋予，低表面能则由十八胺提供。(2)绝大部分超疏水纺织品都是将纺织品直接浸泡在低表面能物质如聚二甲基硅氧烷(PDMS)中，低表面能物质与纺织品之间缺乏牢固的结合。因而制备的超疏水纺织品耐久性能较差。本发明另辟蹊径，直接使用低表面能物质十八胺改性硅烷偶联剂KH560，使得硅烷偶联剂KH560表面附有低表面能物质十八胺，末端的环氧基团也相应转变为十八胺的氨基基团。十八胺-KH560通过硅烷偶联剂KH560的化学键合作用偶联在Ti3C2Tx/TiO2表面。由于十八胺-KH560改性Ti3C2Tx/TiO2表面有氨基基团，和氧化棉织物发生席夫碱反应，通过-C＝N-共价键提升了超疏水表面与棉织物之间的附着力，最终制备得到的耐久超疏水棉织物耐水洗、耐超声、耐弯折、耐强酸/碱等性能优异。(3)本发明将高碘酸钠氧化后的棉织物常温下置于硝酸银中，然后利用Ti3C2Tx/TiO2的自还原性将硝酸银直接还原为单质银，纳米银除了增加棉织物表面的粗糙度之外，还提供了协同抗菌和导电性能。原位生成整理的优势在于：能够更多的在织物的内部生成，有利于提高其耐洗性。将初始液吸收到织物中后再整理，整理后织物即干燥，无任何残留物质，并且初始液可以继续使用，有利于节约成本。反应快，效率高，而且安全、方便。纳米材料的制备和对棉织物的整理可同时进行，避免了纳米材料在整理过程中团聚的问题。
附图说明
图1为不同超声时间下耐久超疏水棉织物接触角的变化。
图2为不同弯折次数下耐久超疏水棉织物接触角的变化。
具体实施方式
下面结合具体实施方式，进一步阐述本发明。
实施例1：
(1)配置体积分数为1％的硅烷偶联剂KH560乙醇溶液，混合均匀后，再加入十八胺，所述十八胺与硅烷偶联剂KH560的质量比为0.1，70℃加热回流反应6h，得到十八胺-KH560。
(2)将9mol/L体积40mL的HCl缓慢倒入聚四氟乙烯烧杯中，加入2g的LiF，常温下400rpm磁力搅拌30min，以完全溶解LiF；随后将2g的Ti3AlC2粉末缓慢加入到蚀刻溶液中，室温下磁力搅拌24h；待反应结束后，使用去离子水清洗数次，3500rpm离心，直至pH值≥6；然后将黑色沉淀物重新分散到1:1水/乙醇混合溶剂中，10000rpm离心10min；使用去离子水洗涤所得沉淀物，3500rpm继续离心数次后，收集上清液，通过离心和冷冻干燥，得到单层Ti3C2Tx粉末；将所述单层Ti3C2Tx粉末放入管式炉中，氩气氛围中60℃持续干燥24h，然后以5℃/min的升温速率升到500℃，保温2h，冷却至室温，得到Ti3C2Tx/TiO2纳米复合材料。
(3)将Ti3C2Tx/TiO2纳米复合材料缓慢加入十八胺-KH560溶液中反应24h，即可制备得到十八胺-KH560改性Ti3C2Tx/TiO2。
(4)使用乙醇反复超声棉织物，真空烘干。将上述棉织物浸渍在2g/L高碘酸钠水溶液中，浴比1：50，避光条件下60℃氧化30min，去离子水反复清洗，真空烘干。然后常温下置于1g/L硝酸银中60min，取出后真空烘干。接下来浸渍在十八胺-KH560改性Ti3C2Tx/TiO2分散液中进行浸轧整理，两浸两轧，控制轧余率100％，80℃烘干2min，120℃定型5min，最终制备得到耐久超疏水棉织物。
实施例2：
(1)配置体积分数为5％的硅烷偶联剂KH560乙醇溶液，混合均匀后，再加入十八胺，所述十八胺与硅烷偶联剂KH560的质量比为0.5，80℃加热回流反应9h，得到十八胺-KH560。
(2)将9mol/L体积40mL的HCl缓慢倒入聚四氟乙烯烧杯中，加入2g的LiF，常温下400rpm磁力搅拌30min，以完全溶解LiF；随后将2g的Ti3AlC2粉末缓慢加入到蚀刻溶液中，室温下磁力搅拌24h；待反应结束后，使用去离子水清洗数次，3500rpm离心，直至pH值≥6；然后将黑色沉淀物重新分散到1:1水/乙醇混合溶剂中，10000rpm离心10min；使用去离子水洗涤所得沉淀物，3500rpm继续离心数次后，收集上清液，通过离心和冷冻干燥，得到单层Ti3C2Tx粉末；将所述单层Ti3C2Tx粉末放入管式炉中，氩气氛围中60℃持续干燥24h，然后以5℃/min的升温速率升到550℃，保温2h，冷却至室温，得到Ti3C2Tx/TiO2纳米复合材料。
(3)将Ti3C2Tx/TiO2纳米复合材料缓慢加入十八胺-KH560溶液中反应24h，即可制备得到十八胺-KH560改性Ti3C2Tx/TiO2。
(4)使用乙醇反复超声棉织物，真空烘干。将上述棉织物浸渍在2g/L高碘酸钠水溶液中，浴比1：50，避光条件下70℃氧化20min，去离子水反复清洗，真空烘干。然后常温下置于50g/L硝酸银中45min，取出后真空烘干，接下来浸渍在十八胺-KH560改性Ti3C2Tx/TiO2分散液中进行浸轧整理，两浸两轧，控制轧余率100％，80℃烘干2min，120℃定型5min，最终制备得到耐久超疏水棉织物。
实施例3：
(1)配置体积分数为10％的硅烷偶联剂KH560乙醇溶液，混合均匀后，再加入十八胺，所述十八胺与硅烷偶联剂KH560的质量比为1，90℃加热回流反应12h，得到十八胺-KH560。
(2)将9mol/L体积40mL的HCl缓慢倒入聚四氟乙烯烧杯中，加入2g的LiF，常温下400rpm磁力搅拌30min，以完全溶解LiF；随后将2g的Ti3AlC2粉末缓慢加入到蚀刻溶液中，室温下磁力搅拌24h；待反应结束后，使用去离子水清洗数次，3500rpm离心，直至pH值≥6；然后将黑色沉淀物重新分散到1:1水/乙醇混合溶剂中，10000rpm离心10min；使用去离子水洗涤所得沉淀物，3500rpm继续离心数次后，收集上清液，通过离心和冷冻干燥，得到单层Ti3C2Tx粉末；将所述单层Ti3C2Tx粉末放入管式炉中，氩气氛围中60℃持续干燥24h，然后以5℃/min的升温速率升到600℃，保温2h，冷却至室温，得到Ti3C2Tx/TiO2纳米复合材料。
(3)将Ti3C2Tx/TiO2纳米复合材料缓慢加入十八胺-KH560溶液中反应24h，即可制备得到十八胺-KH560改性Ti3C2Tx/TiO2。
(4)使用乙醇反复超声棉织物，真空烘干。将上述棉织物浸渍在2g/L高碘酸钠水溶液中，浴比1：50，避光条件下80℃氧化10min，去离子水反复清洗，真空烘干。然后常温下置于100g/L硝酸银中30min，取出后真空烘干，接下来浸渍在十八胺-KH560改性Ti3C2Tx/TiO2分散液中进行浸轧整理，两浸两轧，控制轧余率100％，80℃烘干2min，120℃定型5min，最终制备得到耐久超疏水棉织物。
分别测试实施例1、实施例2、实施例3制备的耐久超疏水棉织物的接触角和不同水洗次数后的接触角。结果如表1所示。
实施例1、实施例2、实施例3制备的耐久超疏水棉织物的接触角水洗50次，接触角的保留率为92.7％、91.1％、92％，耐水洗性能优异。超疏水材料的表面稳定接触角要大于150°，实施例3制备的耐久超疏水棉织物即使经过了50次水洗，仍然具有超疏水性能。
将实施例1、实施例2、实施例3制备的耐久超疏水棉织物分别浸泡在pH＝2强酸溶液和pH＝12的强碱溶液中10h，测试其接触角的变化情况，结果见表2。可见实施例1、实施例2、实施例3制备的耐久超疏水棉织物具有优异的耐强酸/强碱性能。
将实施例3制备的耐久超疏水棉织物放入盛有超纯水的烧杯中，设定超声功率500W，超声时间0-5h。探讨超声时间对耐久超疏水棉织物接触角的影响，结果见图1，可见长时间超声对耐久超疏水棉织物接触角的影响非常小。即使超声时间长达5h，实施例3制备的耐久超疏水棉织物的接触角仍大于150°，具有超疏水性能。
将实施例3制备的耐久超疏水棉织物以90°的角度分别弯曲0-1000次，通过接触角的变化来表征耐久超疏水棉织物的耐弯折性能即柔性，结果见图2。弯曲实验进行了1000次，耐久超疏水棉织物的接触角变化不大，仍具有超疏水性能。
选用革兰氏阴性菌和革兰氏阳性菌中最具有代表性的两个菌种大肠杆菌和金黄色葡萄球菌作为测试菌种，采用振荡烧瓶法定量测试来表征实施例1、实施例2、实施例3制备的耐久超疏水棉织物的抗菌效果。防紫外线效果使用紫外线防护指数(UPF)表示。结果见表3，可见实施例1、实施例2、实施例3制备的耐久超疏水棉织物具有极其优异的抗紫外、抗菌和电磁屏蔽性能。
显然，本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定。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的变化或变动。这里无法对所有的实施方式予以穷举。凡是属于本发明的技术方案所引申出的显而易见的变化或变动仍处于本发明的保护范围之列。
Claims (7)
1.一种耐久超疏水棉织物的制备方法，其特征在于，使用乙醇反复超声棉织物，真空烘干，使用高碘酸钠对上述棉织物在避光条件下进行轻度氧化，去离子水反复清洗，真空烘干后，常温下置于1-100g/L硝酸银中30-60min，取出后真空烘干，接下来浸渍在十八胺-KH560改性Ti3C2Tx/TiO2分散液中进行浸轧整理，两浸两轧，控制轧余率100％，80℃烘干2min，120℃定型5min，最终制备得到耐久超疏水棉织物；
其中所述十八胺-KH560改性Ti3C2Tx/TiO2的制备方法为：(1)将HCl缓慢倒入聚四氟乙烯烧杯中，加入2g的LiF，常温下400rpm磁力搅拌30min，以完全溶解LiF；随后将2g的Ti3AlC2粉末缓慢加入到蚀刻溶液中，室温下磁力搅拌24h；待反应结束后，使用去离子水清洗数次，3500rpm离心，直至pH值≥6；然后将黑色沉淀物重新分散到1:1水/乙醇混合溶剂中，10000rpm离心10min；使用去离子水洗涤所得沉淀物，3500rpm继续离心数次后，收集上清液，通过离心和冷冻干燥，得到单层Ti3C2Tx粉末；(2)将所述单层Ti3C2Tx粉末放入管式炉中，氩气氛围中60℃持续干燥24h，然后以一定的升温速率升温到500℃-600℃，保温2h，冷却至室温，得到Ti3C2Tx/TiO2纳米复合材料；(3)将上述Ti3C2Tx/TiO2纳米复合材料缓慢加入十八胺-KH560溶液中反应24h，即可制备得到十八胺-KH560改性Ti3C2Tx/TiO2。
2.根据权利要求1所述的一种耐久超疏水棉织物的制备方法，其特征在于，所述HCl为9mol/L体积40mL。
3.根据权利要求1所述的一种耐久超疏水棉织物的制备方法，其特征在于，所述升温速率为5℃/min。
4.根据权利要求1所述的一种耐久超疏水棉织物的制备方法，其特征在于，所述十八胺-KH560的制备方法为：配置体积分数为1-10％的硅烷偶联剂KH560乙醇溶液，混合均匀后，再加入十八胺，70-90℃加热回流反应6-12h，得到十八胺-KH560。
5.根据权利要求4所述的一种耐久超疏水棉织物的制备方法，其特征在于，所述十八胺与硅烷偶联剂KH560的质量比为0.1-1。
6.根据权利要求1所述的一种耐久超疏水棉织物的制备方法，其特征在于，所述轻度氧化是指氧化剂高碘酸钠的浓度为2g/L，氧化温度60-80℃，氧化时间10-30min，浴比1：50。
7.由权利要求1～6中任一项所述的制备方法制备得到的耐久超疏水棉织物。
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