CN108867064A - 一种以氧化镁为原料制备廉价稳定超疏水织物的方法 - Google Patents
一种以氧化镁为原料制备廉价稳定超疏水织物的方法 Download PDFInfo
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Abstract
本发明属于疏水材料制备技术领域,具体涉及一种以氧化镁为原料制备廉价稳定超疏水织物的方法。本发明制作过程简单,反应条件温和,易于实现,不需要复杂的反应设备,直接使用廉价易得的材料,通过简单的操作步骤,温和的反应条件便可得到超疏水织物。采用本发明的方法制备的超疏水织物接触角可达152°以上,极大地降低了液滴与织物接触面积。
Description
技术领域
本发明属于疏水材料制备技术领域,具体涉及一种以氧化镁为原料制备廉价稳定超疏水织物的方法。
背景技术
纳米氧化镁在电子、催化剂、陶瓷、涂料等领域有广泛的应用。在市场上,已经实现纳米氧化镁的产业化,纳米氧化镁的价格也相对较低,这为大量使用该材料提供了可能。因此加强氧化镁超疏水材料的研发与制备,既可以拓展氧化镁的研究和应用领域,同时也丰富了超疏水材料的制备方法。
超疏水材料发展了许多年,但是由于其制作成本高昂、稳定性不足、制备方法复杂等因素限制了应用,因此用低廉的成本、简单的方法制作出稳定的超疏水材料越来越受到关注。
超疏水织物常见的制备方法包括:
1.对织物进行酸碱刻蚀,构建微纳米级别的粗糙度,然后用聚二甲基硅氧烷等低表面能质复合修饰,得到超疏水织物。
这类方法的缺点是制作方法复杂,且破坏织物的表面。
2.利用化学气相沉积法制备SiO2溶胶,将织物浸泡在溶液中,微纳米级别的SiO2沉积在织物表面,达到构建粗糙度的效果。然后用聚二甲基硅氧烷等低表面能质复合修饰,得到超疏水织物。
这类方法的缺点是沉积在表面的纳米颗粒易脱落,很容易失去超疏水性能。
3.利用静电纺丝法可以将制备的高浓度溶液拉伸形成纤维状,而制备的低浓度溶液可以将溶液收缩形成颗粒状,使得表面形成粗糙结构,从而具有超疏水性。
这类方法的缺点是利用该方法制备的超疏水织物表面不均匀,在操作过程中对设备的要求比较高,不易控制,且成本高昂。
发明内容
为了解决现有技术中存在的不足,一种以氧化镁为原料制备廉价稳定超疏水织物的方法,该方法简单,成本低廉,易于实现,不需要苛刻的反应条件和复杂的反应设备,直接使用低成本的氧化镁粉体为基准原料,通过简单的操作步骤,温和的反应条件便可得到廉价超疏水织物,且该疏水织物具有耐磨损、稳定的优点,在水中有较好的浮力。
为实现上述目的,本发明采用的技术方案是:
本发明提供的一种以氧化镁为原料制备廉价稳定超疏水织物的方法,
S1、称取环氧树脂、聚酰胺树脂、十二醇和乙醇,环氧树脂:乙醇的比例为1g:10mL,将环氧树脂和聚酰胺树脂以2:1的质量比例相混合,得到混合物A,以十二醇和乙醇的体积比为1:10~25向混合物A中依次加入十二醇和乙醇超声溶解10~30min,放入干净的织物,浸泡5~15min后取出,60~80℃干燥4~6min,备用;
S2、称取氧化镁和乙醇,氧化镁:乙醇的比例为0.1g:5mL,将氧化镁在乙醇中超声溶解30~60min,放入S1处理后的织物,继续超声20~60min后取出,60~80℃干燥5~10min,备用;
S3、将S2处理后的织物放入铝酸酯溶液中,45~60℃加热搅拌2~3h,然后取出织物,室温干燥即得超疏水织物。
优选的,上述的高抗水耐蚀的三维纳米结构钢板膜的制备方法,S1中,所述的织物为棉、毛、麻、涤纶、黏胶或尼龙织物。
优选的,上述的高抗水耐蚀的三维纳米结构钢板膜的制备方法,S1中,超声时间15min,浸泡时间10min,干燥温度为80℃,干燥时间为5min。
优选的,上述的高抗水耐蚀的三维纳米结构钢板膜的制备方法,S2中,氧化镁在乙醇中超声溶解30min,放入S1处理后的织物,继续超声30min,80℃干燥5min。
优选的,上述的高抗水耐蚀的三维纳米结构钢板膜的制备方法,S3中,将S2处理后的织物放入铝酸酯溶液中,50℃加热搅拌2h。
优选的,上述的高抗水耐蚀的三维纳米结构钢板膜的制备方法,S1中,所述环氧树脂和十二醇的比例为5g:3ml。
优选的,上述的高抗水耐蚀的三维纳米结构钢板膜的制备方法,S3中,溶解铝酸酯的溶剂为乙醇,其中,铝酸酯与乙醇的比例为0.4~0.6g:9~15mL。
与现有技术相比,本发明的制备方法具有以下有益效果:
1、本发明中采用成本低廉的胶黏剂,将织物和纳米氧化镁粒紧密枝接在一起,使它的稳定性提高。
2、本发明中环氧树脂和聚酰胺树脂混合后加入十二醇,避免了制成的织物放黄、变硬的问题,尽量不改变织物的柔软度和颜色。
3、本发明制作过程简单,反应条件温和,易于实现,不需要苛刻的反应条件和复杂的反应设备。
4、本发明没有使用有毒有害的溶剂,对环境友好,没有使用硅烷,与大多数超疏水材料的制备方法有别。
5、本发明使得超疏水织物的发展在实际应用中有了进一步的发展,服装、户外运动、油水分离等许多领域。
6、本发明直接使用廉价易得的材料,通过简单的操作步骤,温和的反应条件便可得到超疏水织物。采用本发明的方法制备的超疏水织物接触角可达152°以上,极大地降低了液滴与织物接触面积。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
附图说明:
图1为本发明实施例1制备的超疏水织物静态接触角测量图;
图2为本发明实施例1制备的超疏水织物扫描电镜图;
图3为本发明实施例1制备的超疏水织物耐酸碱图;
图4为本发明实施例1制备的超疏水织物胶带粘附次数与接触角关系图;
图5为本发明实施例1制备的超疏水织物折叠次数与接触角关系图;
图6为本发明实施例1制备的超疏水织物洗涤测试图(用乙醇、丙酮和环己烷洗涤,每4小时循环一次);
图7为本发明实施例1制备的超疏水织物自清洁图(将织物浸入染色的水中,由a、b、c的顺序放入);
图8为本发明实施例1制备的超疏水织物的油水分离效率图(分离水和四氯化碳、三氯甲烷、二氯甲烷、环己烷、正己烷以及葵花籽油的混合液);
图9为本发明实施例1制备的超疏水织物在水中(染色)负重照片。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。下列实施例中未注明具体条件的试验方法,通常按照常规条件,或者按照各制造商所建议的条件,本发明中的药品均为化学纯试剂。
实施例1
在本实施例中,一种以氧化镁为原料制备廉价稳定超疏水织物的方法,包括以下步骤:
S1、称取0.5g环氧树脂和0.25g的聚酰胺树脂,再加入0.3mL十二醇,溶于5mL的乙醇,超声分散15min,将干净织物放入其中浸泡10min后取出,80℃干燥5min,备用,其中干净的织物大小为2.5cm×2.5cm;
S2、称取0.5g的纳米氧化镁(50nM)溶于5mL乙醇,超声30min,将S1的织物放入其中超声浸泡10min,80℃干燥5min,取出备用;
S3、在搅拌条件下向S2处理后的织物放入溶解于铝酸酯的乙醇溶液中,其中铝酸酯的乙醇溶液是将0.5g铝酸酯溶解于15mL乙醇得到的,60℃加热搅拌2h,然后取出织物,室温干燥即得超疏水织物。
对本实施例1制备的超疏水织物进行接触角测量表征,本发明实施例1中所制备的超疏水织物的接触角测量图如图1所示,由图中可以看出,水滴在处理过的织物上呈现较完整的球形,织物表面的水滴静态接触角大于150°,水滴在织物表面可以自由滚动,表明成功的制备出超疏水织物。
本发明实施例1中所制备的超疏水织物的扫描电镜图如图2所示,从图中可以看出,织物的表面修饰了诸多的粗糙物质,本实验中只用了氧化镁来增强其粗糙度,所以,从该图可以得出,氧化镁修饰在了织物上,增强了粗糙度,使其达到超疏水的状态。我们所采用的氧化镁按照预期的设计起到了效果。
图3是pH为1~14的水珠滴在本发明实施例1中所制备的超疏水织物上,检测不同的酸碱溶液对超疏水织物的影响,从图中可看出不同的酸碱溶液测得的结果,接触角都在150°以上,保持了超疏水性。该图可说明,制备的超疏水织物对酸碱溶液有耐受性,其稳定性较好。
图4、图5和图6分别为本发明实施例1制备的超疏水织物做的胶带粘附、折叠实验和洗涤实验,从图4中可看出,在用胶带粘附100次后,该织物才丧失超疏水性,但是还是疏水的。从图5可看出,将制备的超疏水织物折叠2000次,织物依旧可保持超疏水性质。从图6可看出,用乙醇、丙酮和正己烷(选用有代表的溶剂)洗涤12次后,织物表面仍然有很高的接触角,没有使其失效。这表明,制备的超疏水织物很稳定,在一些物理破坏中,能保持超疏水性。
图7是本发明实施例1制备超疏水织物自清洁测试,将制备好的织物浸入染色的水中图中显示为从a至b的过程,然后再取出,织物表面不被污水污染,依旧光洁。说明该超疏水织物有自清洁性,可在服装、修饰等领域广泛应用。
图8是本发明实施例1制备的超疏织物油水分离效率图,分为轻油和重油。重油和水的混合物用重力做驱动力,通过该织物可轻易分离。轻油浮于水面,用该织物浸入吸收,可使油水分离。如图所示,分离效率在90%以上,说明该织物具有良好的油水分离效率,且该织物可重复使用,增强其实用性。该织物在处理有机溶剂、油水相分离等领域有广阔的应用前景。
图9是对本发明实施例1制备的超疏织物的浮力测试,由图中看出,由于其超疏水性,使原本遇水即沉的织物漂浮于水面,且能负载一定重物。在28cm2的织物上可负载12.36g的重物,这一性质在救生衣、泳衣等服饰上有着良好的应用前景。
实施例2
在本实施例中,一种以氧化镁为原料制备廉价稳定超疏水织物的方法,包括以下步骤:
S1、称取1g环氧树脂和0.5g的聚酰胺树脂,再加入0.6mL十二醇,溶于10mL的乙醇,超声分散15min,将干净织物放入其中浸泡10min后取出,80℃干燥5min,备用,其中干净的织物大小为2.5cm×2.5cm;
S2、称取1g的纳米氧化镁(50nM)溶于10mL乙醇,超声30min,将S1的织物放入其中超声浸泡10min,80℃干燥5min,取出备用;
S3、在搅拌条件下向S2处理后的织物放入溶解于铝酸酯的乙醇溶液中,其中铝酸酯的乙醇溶液是将0.5g铝酸酯溶解于15mL乙醇得到的,60℃加热搅拌2h,然后取出织物,室温干燥即得超疏水织物。
实施例3
在本实施例中,一种以氧化镁为原料制备廉价稳定超疏水织物的方法,包括以下步骤:
S1、称取1g环氧树脂和0.5g的聚酰胺树脂,再加入0.6mL十二醇,溶于10mL的乙醇,超声分散15min,将干净织物放入其中浸泡10min后取出,80℃干燥5min,备用,其中干净的织物大小为2.5cm×2.5cm;
S2、称取1g的纳米氧化镁(50nM)溶于10mL乙醇,超声30min,将S1的织物放入其中超声浸泡10min,80℃干燥5min,取出备用;
S3、在搅拌条件下向S2处理后的织物放入溶解于铝酸酯的乙醇溶液中,其中铝酸酯的乙醇溶液是将0.25g铝酸酯溶解于5mL乙醇得到的,60℃加热搅拌2h,然后取出织物,室温干燥即得超疏水织物。
实施例4
在本实施例中,一种以氧化镁为原料制备廉价稳定超疏水织物的方法,包括以下步骤:
S1、称取1g环氧树脂和0.5g的聚酰胺树脂,再加入0.3mL十二醇,溶于5mL的乙醇,超声分散10min,将干净织物放入其中浸泡15min后取出,80℃干燥5min,备用,其中干净的织物大小为2.5cm×2.5cm;
S2、称取0.5g的纳米氧化镁(50nM)溶于10mL乙醇,超声30min,将S1的织物放入其中超声浸泡15min,80℃干燥5min,取出备用;
S3、在搅拌条件下向S2处理后的织物放入溶解于铝酸酯的乙醇溶液中,其中铝酸酯的乙醇溶液是将0.5g铝酸酯溶解于15mL乙醇得到的,60℃加热搅拌2h,然后取出织物,室温干燥即得超疏水织物。
实施例5
在本实施例中,一种以氧化镁为原料制备廉价稳定超疏水织物的方法,包括以下步骤:
S1、称取0.5g环氧树脂和0.25g的聚酰胺树脂,再加入0.3mL十二醇,溶于5mL的乙醇,超声分散10min,将干净海绵放入其中浸泡15min后取出,80℃干燥5min,备用,其中干净的海绵大小为2.5cm×2.5cm;
S2、称取0.5g的纳米氧化镁(50nM)溶于5mL乙醇,超声30min,将S1的海绵放入其中超声浸泡10min,80℃干燥5min,取出备用;
S3、在搅拌条件下向S2处理后的海绵放入溶解于铝酸酯的乙醇溶液中,其中铝酸酯的乙醇溶液是将0.5g铝酸酯溶解于15mL乙醇得到的,60℃加热搅拌2h,然后取出织物,室温干燥即得超疏水海绵。
需要说明的是,上述实施例中,超声的功率均为400W。
需要说明的是,本发明权利要求书中涉及数值范围时,应理解为每个数值范围的两个端点以及两个端点之间任何一个数值均可选用,由于采用的步骤方法与实施例相同,为了防止赘述,本发明描述了优选实施例及其效果,但本领域内的技术人员一旦得知了基本创造性概念,则可对这些实施例作出另外的变更和修改。所以,所附权利要求意欲解释为包括优选实施例以及落入本发明范围的所有变更和修改。
显然,本领域的技术人员可以对本发明进行各种改动和变型而不脱离本发明的精神和范围。这样,倘若本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内,则本发明也意图包含这些改动和变型在内。
Claims (7)
1.一种以氧化镁为原料制备廉价稳定超疏水织物的方法,其特征在于,包括以下步骤:
S1、称取环氧树脂、聚酰胺树脂、十二醇和乙醇,环氧树脂:乙醇的比例为1g:10mL,将环氧树脂和聚酰胺树脂以2:1的质量比例相混合,得到混合物A,以十二醇和乙醇的体积比为1:10~25向混合物A中依次加入十二醇和乙醇超声溶解10~30min,放入干净的织物,浸泡5~15min后取出,60~80℃干燥4~6min,备用;
S2、称取氧化镁和乙醇,氧化镁:乙醇的比例为0.1g:5mL,将氧化镁在乙醇中超声溶解30~60min,放入S1处理后的织物,继续超声20~60min后取出,60~80℃干燥5~10min,备用;
S3、将S2处理后的织物放入铝酸酯溶液中,45~60℃加热搅拌2~3h,然后取出织物,室温干燥即得超疏水织物。
2.根据权利要求1所述的一种以氧化镁为原料制备廉价稳定超疏水织物的方法,其特征在于,S1中,所述的织物为棉、毛、麻、涤纶、黏胶或尼龙织物。
3.根据权利要求1所述的一种以氧化镁为原料制备廉价稳定超疏水织物的方法,其特征在于,S1中,超声时间15min,浸泡时间10min,干燥温度为80℃,干燥时间为5min。
4.根据权利要求1所述的一种以氧化镁为原料制备廉价稳定超疏水织物的方法,其特征在于,S2中,氧化镁在乙醇中超声溶解30min,放入S1处理后的织物,继续超声30min,80℃干燥5min。
5.根据权利要求1所述的一种以氧化镁为原料制备廉价稳定超疏水织物的方法,其特征在于,S3中,将S2处理后的织物放入铝酸酯溶液中,50℃加热搅拌2h。
6.根据权利要求1所述的一种以氧化镁为原料制备廉价稳定超疏水织物的方法,其特征在于,S1中,所述环氧树脂和十二醇的比例为5g:3ml。
7.根据权利要求4所述的一种以氧化镁为原料制备廉价稳定超疏水织物的方法,其特征在于,溶解铝酸酯的溶剂为乙醇,其中,铝酸酯与乙醇的比例为0.4~0.6g:9~15mL。
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