CN107164947A - 一种耐用超疏水织物及其制备方法 - Google Patents
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Abstract
本发明公开了一种耐用超疏水织物及其制备方法。该制备方法是将织物浸入正硅酸乙酯和含端羟基的聚二甲基硅氧烷的混合溶液中,取出后置于装有盐酸溶液的密闭容器中且位于盐酸溶液液面之上,在30‐60℃温度下反应0.5‐2h,制得耐用超疏水织物。本发明制备的织物表面水滴静态接触角大于150°,水滴在其表面极易滚动,同时该织物具有优异的化学稳定性和力学耐久性,且制备工艺简单,无污染。
Description
技术领域
本发明涉及一种超疏水材料,具体涉及一种耐用超疏水织物及其制备方法。
背景技术
受自然界中荷叶表面、蝴蝶翅膀、动物羽毛等的启发,人们设计并发明了超疏水织物,其静态液滴接触角大于150°,且水滴在其表面极易发生滚动。超疏水织物在自清洁、防覆冰、防污染、阻燃、油水分离等方面具有重要的应用价值,已引起了人们的广泛关注。
目前关于超疏水织物的制备方法已有较多报道,如化学刻蚀法、溶胶凝胶法、气相沉积法、紫外光固化法等,但仍存在如下问题:制备工艺繁琐,反应条件苛刻,需要用到特殊的昂贵仪器,只能局限于实验室研究;采用含氟的低表面能物质修饰织物以期构造超疏水表面,但长链含氟单体容易在自然环境中氧化分解,对人体健康和生态环境会造成严重的危害;制备过程中四氢呋喃、甲苯、丙酮等有毒溶剂的使用也违背了“绿色化学”的宗旨;构造出的微纳粗糙结构由于与织物、低表面能物质间微弱的结合力容易遭到破坏,导致织物抵抗外界破坏能力差,在洗涤或摩擦后易丧失超疏水性,耐用性较差。因此,发展一种制备方法简便、经济高效、绿色环保和耐用性强的超疏水织物显得尤为重要。
发明内容
本发明针对目前超疏水织物制备工艺繁琐、反应条件苛刻和耐久性较差等现有技术存在的问题,提供一种工艺简单、成本低廉和环境友好的超疏水织物及其制备方法,所得织物具有优异的化学稳定性和力学耐久性,能长期保持超疏水性。
本发明采用一步气‐液溶胶凝胶法,首先将普通织物浸入含正硅酸乙酯和含端羟基的聚二甲基硅氧烷的混合溶液中,取出后置于充满挥发性盐酸气体的密闭容器中;将该密闭容器在恒定温度下保持一定时间,正硅酸乙酯通过水解和缩聚在织物表面原位生成二氧化硅,进而二氧化硅上的硅羟基与聚二甲基硅氧烷上的端羟基之间发生交联反应,制得表面呈微纳粗糙结构的超疏水织物。本发明在盐酸气体的催化下,利用正硅酸乙酯水解和缩聚在织物上原位生成二氧化硅,进而二氧化硅上的硅羟基与聚二甲基硅氧烷的端羟基之间发生缩聚反应,形成具有交联结构的呈微纳粗糙结构的耐用超疏水织物。本发明方法具有成本低廉、绿色环保、操作简便等优点,且制备的超疏水织物具有优异的化学稳定性和力学耐久性,即使在严苛的环境下也能长期保持超疏水性。该耐用超疏水织物在制备过程中的发生的反应如下式所示:
本发明目的通过如下技术方案实现:
一种耐用超疏水织物的制备方法,包括以下步骤:将织物浸入正硅酸乙酯和含端羟基的聚二甲基硅氧烷的混合溶液中,取出后置于装有盐酸溶液的密闭容器中且位于盐酸溶液液面之上,在30‐60℃温度下反应0.5‐2h,制得耐用超疏水织物。
为进一步实现本发明目的,优选地,所述含端羟基的聚二甲基硅氧烷的分子量为400‐8000。
优选地,所述正硅酸乙酯和含端羟基的聚二甲基硅氧烷的质量比为2:1‐5:1。
优选地,所述盐酸溶液的质量百分比为10‐20wt%。
优选地,所述30‐60℃温度下反应0.5‐2h是该密闭容器放入烘箱中,控制温度为30‐60℃。
优选地,所述织物为聚酯、棉、羊毛、腈纶、聚氨酯和尼龙中的任意一种为原料的织物。
一种耐用超疏水织物,由上述的制备方法制得。
优选地,该耐用超疏水织物接触角达到150‐165°,在经过168h以上的有机溶剂浸泡、112次的洗涤(AATCC测试方法61‐2006的2A条件)或600次的耐磨测试后仍可保持超疏水性质。
本发明所述的耐用超疏水涂层的制备方法,与现有技术相比,具有如下优点:
(1)通过一步气‐液溶胶凝胶法制备出超疏水织物,具有操作简单、条件温和、无需使用含氟物质和有毒溶剂、无需特定的仪器设备等优点,可应用于大规模的工业生产。
(2)本发明制备的超疏水织物中二氧化硅堆积形成微纳粗糙结构,与聚二甲基硅氧烷通过羟基缩水脱合形成化学键链接的交联结构,在不同溶剂中长时间浸泡也能保持较高的疏水性能,且织物经多次洗涤和磨损后,其疏水性也基本不变,具有优异的化学稳定性和力学耐久性。
附图说明
图1为实施例1制备的耐磨超疏水织物的扫描电镜图(图像放大倍数为1000倍,右上角插图放大倍数为5000倍,右下角插图为水接触角照片)。
图2为实施例1中纯织物和浸泡正硅酸乙酯和聚二甲基硅氧烷混合物后45℃反应不同时间得到的织物的红外谱图。
图3为各实施例中制备的耐磨超疏水织物用于磨损测试的示意图。
具体实施方式
为更好地理解本发明,下面结合实施例对本发明作进一步说明,但是本发明的实施方式不限于此。
实施例1
将聚酯织物浸入正硅酸乙酯和分子量为400的聚二甲基硅氧烷的质量比为3:1的混合溶液中,取出后置于装有盐酸溶液(质量分数为20wt%)的密闭容器中且位于盐酸溶液液面之上,将该密闭容器放入烘箱于45℃下反应1h,即可制得耐用超疏水织物。
图1是如何得到的要有一个简要的说明,包括放大倍数。图1为本实施例耐用超疏水织物放大1000倍的扫描电镜图,其中右上角的插图为放大5000倍的扫描电镜图,右下角为水接触角的照片。从图1可以看出,在超疏水织物表面形成二氧化硅堆积的微纳粗糙结构,水接触角为160°,具有超疏水性能。
图2为本实施例中纯织物和浸泡正硅酸乙酯和聚二甲基硅氧烷混合物后45℃反应不同时间得到的织物的红外谱图。从图2可以看出,与纯织物相比,浸泡了正硅酸乙酯和聚二甲基硅氧烷混合物后的织物在3330cm‐1的羟基振动峰和1719cm‐1的羰基振动峰强度减弱,而在2972cm‐1的CH3振动峰和2896cm‐1的CH2振动峰强度增强,并且在1068cm‐1和787cm‐1出现了Si‐O‐Si和Si‐C的新峰。随反应的进行,3200‐3400cm‐1的羟基吸收峰先出现后消失,CH3峰峰强略微降低,而CH2峰峰强大幅度下降,但后期均保持不变。并且Si‐O‐Si峰位向高波数位置移动,900‐1100cm‐1处的峰宽也逐渐变大。这说明反应前期正硅酸乙酯发生水解缩合反应,生成的二氧化硅后期与两端带羟基的聚二甲基硅氧烷发生交联反应。
为了评价超疏水织物的化学稳定性,将其分别浸泡在装有30mL丙酮、乙醇、甲苯、己烷的50mL烧杯中,并用保鲜膜密封,在室温下浸泡168h后取出用乙醇洗涤,并在50℃的鼓风干燥箱中干燥1h,对其接触角进行测试。表1列出了本实施例耐用超疏水织物分别浸泡在丙酮、乙醇、甲苯、己烷中168h后,取出后干燥所测得的接触角。从表1可以看出,本实施例所制备的耐用超疏水织物在不同溶剂中长时间浸泡后,其水接触角变化不大,表明其具有优异的化学稳定性。
为了评价超疏水织物的耐洗涤性,照AATCC测试方法61‐2006的2A条件对其进行洗涤,具体方法为:调节水洗色牢度仪(SW‐12A,温州方圆仪器有限公司)水温达到49℃,向大小为90×200mm的钢杯中加入150mL的去离子水,0.015g的洗涤剂和50颗直径6mm、质量1g的钢球。预热钢杯两分钟后,将尺寸为50×150mm的织物放入钢杯,再启动仪器,以40±2rpm的转速运转45min。最后取出试样用乙醇清洗三次,在60℃烘箱中干燥。表2列出了本实施例耐用超疏水织物按照AATCC测试方法61‐2006的2A条件洗涤112次所测得的接触角。
为了评价超疏水织物的耐磨性,采用了如图3所示的装置对其进行测试,耐磨测试装置由280目的砂纸和200g的砝码组成,将砂纸放在平整的桌子上并固定,再将织物试样放在砂纸上面,并用200g的砝码压在织物试样上面,以4cm/s的速度将织物试样拉动20cm,视为1次摩擦,经过600次摩擦后,测试织物试样的接触角。
表2列出了织物磨损600次后的水接触角。从表2可以看出,本实施例所制备的耐用超疏水织物即使经过112次洗涤和600次磨损,其水接触角均可保持在150°以上,表明其具有优良的耐洗涤和耐磨损性能。
结合图1、图2、表1和表2,本实施例制备的耐用超疏水织物接触角大于150°,这主要归因于正硅酸乙酯水解生成的二氧化硅在聚二甲基硅氧烷链段的作用下堆积形成微纳粗糙结构以及聚二甲基硅氧烷链段的疏水性;而超疏水织物优良的化学稳定性和力学耐久性主要是由于二氧化硅上的羟基进一步与聚二甲基硅氧烷上的羟基缩合形成了化学交联结构。
实施例2
将棉织物浸入正硅酸乙酯和分子量为8000的聚二甲基硅氧烷的质量比为2:1的混合溶液中,取出后置于装有盐酸溶液(质量分数为10wt%)的密闭容器中且位于盐酸溶液液面之上,将该密闭容器放入烘箱于30℃下反应2h,即可制得耐用超疏水织物。
表1列出了本实施例耐用超疏水织物分别浸泡在丙酮、乙醇、甲苯、己烷中168h后,取出洗涤干燥所测得的接触角,表2列出了本实施例耐用超疏水织物分别按照AATCC测试方法61‐2006的2A条件洗涤112次后、按照3示意图磨损600次后(垂直压强为2.5kPa,拉伸速度为4cm/s,拉伸距离为20cm,砂纸为280目)的水接触角。从表1可以看出,本实施例所制备的耐用超疏水织物在不同溶剂中浸泡168h,其水接触角均保持在150°以上,表明其具有优良的化学稳定性。从表2可以看出,本实施例所制备的耐用超疏水织物即使经过112次洗涤和600次磨损,其水接触角均可保持在150°以上,表明其具有优良的耐洗涤和耐磨损性能。
实施例3
将尼龙织物浸入正硅酸乙酯和分子量为2000的聚二甲基硅氧烷的质量比为5:1的混合溶液中,取出后置于装有盐酸溶液(质量分数为15wt%)的密闭容器中且位于盐酸溶液液面之上,将该密闭容器放入烘箱于45℃下反应1.5h,即可制得耐用超疏水织物。
表1列出了本实施例耐用超疏水织物分别浸泡在丙酮、乙醇、甲苯、己烷中168h后,取出洗涤干燥所测得的接触角,表2列出了本实施例耐用超疏水织物分别按照AATCC测试方法61‐2006的2A条件洗涤112次后、按照图3示意图磨损600次后(垂直压强为2.5kPa,拉伸速度为4cm/s,拉伸距离为20cm,砂纸为280目)的水接触角。从表1可以看出,本实施例所制备的耐用超疏水织物在不同溶剂中浸泡168h,其水接触角均保持在150°以上,表明其具有优良的化学稳定性。从表2可以看出,本实施例所制备的耐用超疏水织物即使经过112次洗涤和600次磨损,其水接触角均可保持在150°以上,表明其具有优良的耐洗涤和耐磨损性能。
实施例4
将腈纶织物浸入正硅酸乙酯和分子量为5000的聚二甲基硅氧烷的质量比为4:1的混合溶液中,取出后置于装有盐酸溶液(质量分数为20wt%)的密闭容器中且位于盐酸溶液液面之上,将该密闭容器放入烘箱于60℃下反应0.5h,即可制得耐用超疏水织物。
表1为本发明实施例耐用超疏水织物在不同溶剂中浸泡168h后的水接触角。表1列出了本实施例耐用超疏水织物分别浸泡在丙酮、乙醇、甲苯、己烷中168h后,取出洗涤干燥所测得的接触角,表2列出了本实施例耐用超疏水织物分别按照AATCC测试方法61‐2006的2A条件洗涤112次后、按照图3示意图磨损600次后(垂直压强为2.5kPa,拉伸速度为4cm/s,拉伸距离为20cm,砂纸为280目)的水接触角。从表1可以看出,本实施例所制备的耐用超疏水织物在不同溶剂中浸泡168h,其水接触角均保持在150°以上,表明其具有优良的化学稳定性。从表2可以看出,本实施例所制备的耐用超疏水织物即使经过112次洗涤和600次磨损,其水接触角均可保持在150°以上,表明其具有优良的耐洗涤和耐磨损性能。
表1
注:采用德国KRUSS公司的DSA100接触角测试仪进行测试,每个样品取5个点计算平均值。
表2为本发明实施例耐用超疏水织物按照AATCC测试方法61‐2006的2A条件洗涤112次后、按照图3示意图磨损600次后(垂直压强为2.5kPa,拉伸速度为4cm/s,拉伸距离为20cm,砂纸为280目)的水接触角。
表2
注:耐洗测试按照AATCC测试方法61‐2006的2A条件进行,耐磨测试按照图3示意图(垂直压强为2.5kPa,拉伸速度为4cm/s,拉伸距离为20cm,砂纸为280目)进行。水接触角采用德国KRUSS公司的DSA100接触角测试仪进行,每个样品取5个点计算平均值。
Claims (8)
1.一种耐用超疏水织物的制备方法,其特征在于包括以下步骤:将织物浸入正硅酸乙酯和含端羟基的聚二甲基硅氧烷的混合溶液中,取出后置于装有盐酸溶液的密闭容器中且位于盐酸溶液液面之上,在30‐60℃温度下反应0.5‐2h,制得耐用超疏水织物。
2.根据权利要求1所述的耐用超疏水织物的制备方法,其特征在于:所述含端羟基的聚二甲基硅氧烷的分子量为400‐8000。
3.根据权利要求1所述的耐用超疏水织物的制备方法,其特征在于:所述正硅酸乙酯和含端羟基的聚二甲基硅氧烷的质量比为2:1‐5:1。
4.根据权利要求1所述的耐用超疏水织物的制备方法,其特征在于:所述盐酸溶液的质量百分比为10‐20wt%。
5.根据权利要求1所述的耐用超疏水织物的制备方法,其特征在于:所述30‐60℃温度下反应0.5‐2h是该密闭容器放入烘箱中,控制温度为30‐60℃。
6.根据权利要求1所述的耐用超疏水织物的制备方法,其特征在于:所述织物为聚酯、棉、羊毛、腈纶、聚氨酯和尼龙中的任意一种为原料的织物。
7.一种耐用超疏水织物,其特征在于由权利要求1‐6任一项所述的制备方法制得。
8.根据权利要求7所述的耐用超疏水织物,其特征在于,该织物接触角达到150‐165°,在经过168h以上的有机溶剂浸泡、112次的洗涤或600次的耐磨测试后仍保持超疏水性质。
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