CN111335038A - 一种耐水洗光催化超疏水棉织物及其制备、应用 - Google Patents
一种耐水洗光催化超疏水棉织物及其制备、应用 Download PDFInfo
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Abstract
本发明公开了一种耐水洗光催化超疏水棉织物,以表面负载有β‑FeOOH纳米粒子的多巴胺改性棉织物为载体,在载体表面修饰有十二硫醇。本发明公开了上述耐水洗光催化超疏水棉织物制备方法,将除杂后的棉织物进行多巴胺改性处理,以铁盐为前驱体,在多巴胺织物表面原位生长β‑FeOOH纳米粒子;再在粗糙织物表面修饰低表面能物质十二硫醇,获得具有耐水洗和光催化性能的超疏水棉织物。本发明所得织物在可见光照射下180min内可以完全降解亚甲基蓝溶液,而且耐水洗性能优良,经5次循环后,降解亚甲基蓝溶液的稳定性和可靠性均达到90%;而且棉织物表面水滴静态接触角大于150°,经不同油液的油水分离后,分离率大于98%。
Description
技术领域
本发明涉及棉织物改性技术领域,尤其涉及一种耐水洗光催化超疏水棉织物及其制备、应用。
背景技术
光催化氧化是一种操作简单、成本低、无二次污染的环保技术,已被广泛应用于解决工业废水中有机污染物超标问题。绝大多数传统的光催化剂都会受到紫外线的影响,而紫外线占太阳能的比例很小,仅为4%左右,对太阳光的利用率很低。而可见光占太阳光能的43%左右,因此可见光驱动光催化剂的研究受到广大科学家的关注与研究。
而超疏水性表面通常是指水接触角大于150°和接触角滞后很低的表面,而润湿性能主要取决于表面能和表面粗糙度。已有研究表明,表面粗糙度与粒子的粘附存在相关性,表面能可以用化学改性加以控制。因此要想达到超疏水的效果,在纺织品表面修饰低表面能的防水整理剂的同时,还要降低织物的表面能。超湿性材料由于其结构和性能的新颖性,在水质净化中发挥了重要作用。近年来,很多科学家利用某些材料对水和油的不同润湿性来实现油水分离已经进行了大量的研究。
申请号为201811493414.7的中国专利《一种耐磨超疏水织物及其制备方法》中,采用氧化锌纳米粒子负载在棉纤维内部,所得织物耐水洗、抗菌和防紫外线性能优良。但其缺点是:由于氧化锌禁带宽度为3.37eV,且对太阳能的利用率低,光催化效果不明显,同时氧化锌纳米粒子在织物表面负载不牢固,使用过程中易掉落。
现有文献(冯静,杜英英,邢彦军.钨杂二氧化钛负载棉织物的微波法制备及光催化性能[J].纺织学报,2014,35(7):88-93.)中,将钨酸钠和钨酸铵作为钨源,采用微波辅助法将二氧化钛负载在棉织物表面,得到具有光催化性能的W-TiO2/棉织物。但上述所得织物耐水洗性能差,同时二氧化钛禁带宽度高,只能利用太阳能中4%的紫外光。
β-FeOOH作为一种半导体材料,其小禁带宽度仅为2.1eV,可见光响应高,具有小粒径和高比表面积。由于β-FeOOH在制备过程中操作简单、成本低、反应温和、环境友好等优点,在环境领域得到了广泛的应用。
然而,β-FeOOH往往作为粉末状催化剂,很难分散和回收,有时不可避免地会产生二次污染。同时粉末状的羟基氧化铁易产生沉淀,不易溶于水,不易重复利用等缺点,因此很难在织物表面负载,所以将光催化颗粒粘附在织物表面成为广大学者研究的热点。
发明内容
本发明提出了一种耐水洗光催化超疏水棉织物及其制备、应用,既克服了超疏水织物制备工艺繁琐、能耗大、耐久性差的缺点,又使所得棉织物耐水洗和光催化性能。
一种耐水洗光催化超疏水棉织物,以表面负载有β-FeOOH纳米粒子的多巴胺改性棉织物为载体,在载体表面修饰有十二硫醇。
上述耐水洗光催化超疏水棉织物的制备方法,将除杂后棉织物进行多巴胺改性处理,接着将β-FeOOH纳米粒子负载在多巴胺改性棉织物表面得到载体,然后在载体表面采用十二硫醇进行修饰。
优选地,棉织物除杂的具体操作如下:向圆底烧瓶中加入丙酮至丙酮体积占烧圆底瓶容积的三分之一,将棉织物置于索氏提取器中,将该索氏提取器与上述盛有丙酮的圆底烧瓶联通,然后水浴加热,取出干燥。
优选地,棉织物除杂过程中,水浴加热温度为80-100℃,水浴加热时间为4.5-5.5h。
优选地,所述多巴胺改性处理的具体操作如下:对Tris-HCl缓冲液调节pH值,然后向所述缓冲液溶液中加入多巴胺,再加入除杂后棉织物,将体系置于20-40℃水浴中震荡,取出干燥。
优选地,多巴胺改性处理过程中,水浴震荡时间为15-20h。
优选地,多巴胺改性处理过程中,对Tris-HCl缓冲液调节pH值至8.5。
优选地,多巴胺改性处理过程中,多巴胺与所述缓冲液溶液的质量体积比(g/mL)为0.1-0.2:100。
优选地,所述将β-FeOOH纳米粒子负载在多巴胺改性棉织物表面的具体操作如下:将铁盐溶液和盐酸混合后,再浸入多巴胺改性棉织物,50-80℃水浴处理5-10h,干燥。
优选地,铁盐溶液浓度为0.055-0.074mol/L,盐酸浓度为0.005-0.01mol/L。
优选地,所述在载体表面采用十二硫醇进行修饰的具体操作如下:将十二硫醇超声分散在无水乙醇中,然后加入载体进行静置15-20h。
优选地,十二硫醇表面修饰过程中,十二硫醇与无水乙醇的质量体积比(g/mL)为0.1-0.5:50-200。
上述耐水洗光催化超疏水棉织物在光催化剂或水油分离的应用。
本发明具有以下有益效果:
(1)采用棉织物进行多巴胺改性之后,由于多巴胺在聚合过程中会产生大量的氨基、邻苯二酚等基团,可赋予棉织物超强的粘附力;
(2)经过多巴胺修饰的棉织物有强大的粘附力,采用铁盐在多巴胺改性棉织物表面原位生长β-FeOOH纳米粒子,能强有力地将β-FeOOH纳米粒子负载在织物表面,提高织物表面微观粗糙度;同时β-FeOOH纳米粒子的禁带宽度仅为2.1eV,可见光响应高,具有小粒径和高比表面积,大幅提高所得棉织物的光催化性能,扩大应用领域;
(3)由于织物表面微观粗糙度被提高,接着采用十二硫醇对载体表面进行表面修饰,一方面加强十二硫醇与载体表面之间的结合强度,避免十二硫醇脱落,另一方面十二硫醇可与具有大量活性官能团的聚多巴胺结合,进一步增强十二硫醇与载体表面之间的结合强度,同时十二硫醇对载体表面进行修饰,不仅可以提高所得棉织物的疏水亲油性能,而且在棉织物表面形成保护膜,减少甚至避免β-FeOOH纳米粒子的脱落。
经检测,本发明所得棉织物的性质如下:
(1)在可见光照射下,180min内可以完全降解亚甲基蓝溶液;
(2)经5次循环后,降解亚甲基蓝溶液的稳定性和可靠性仍然均可达90%;
(3)对棉织物表面水滴静态接触角进行测试,其接触角大于150°;
(4)经不同油液的油水分离后,其分离率仍大于98%。
附图说明
图1为实施例3所得耐水洗光催化超疏水棉织物的SEM图,左侧为原始棉织物,右侧为实施例3所得耐水洗光催化超疏水棉织物。
图2为实施例3所得耐水洗光催化超疏水棉织物的XRD图,其中CF为原始棉织物,CF@PDA为多巴胺改性棉织物,CF@PDA@FeOOH为表面负载有β-FeOOH纳米粒子的多巴胺改性棉织物。
图3为图2中虚线框中局部放大图。
图4为实施例4所得耐水洗光催化超疏水棉织物在可见光照射下亚甲基蓝溶液的吸收光谱图。
图5为实施例4所得耐水洗光催化超疏水棉织物经1-5次循环后,降解亚甲基蓝溶液的稳定性谱图。
图6为实施例5所得耐水洗光催化超疏水棉织物的接触角测试图。
图7为实施例6所得耐水洗光催化超疏水棉织物在不同油液的油水分离效率图,其中hexane为正己烷,kerosene为煤油,toluene为甲苯,chloroform为氯仿,dichloroethane为二氯乙烷。
图8为实施例6所得耐水洗光催化超疏水棉织物在不同循环次数的油水分离效率图。
图9为油/水混合物经本发明所得耐水洗光催化超疏水棉织物接触后的模拟示意图。
具体实施方式
下面结合具体实施例对本发明作进一步解说。
实施例1
一种耐水洗光催化超疏水棉织物的制备方法,包括如下步骤:
(1)向圆底烧瓶中加入丙酮至丙酮体积占烧圆底瓶容积的三分之一,将棉织物置于索氏提取器中,将该索氏提取器与上述盛有丙酮的圆底烧瓶联通,然后80℃水浴加热4.5h,取出干燥;
(2)对100mL Tris-HCl缓冲液调节pH值至8.5,然后向所述缓冲液溶液中加入0.1g多巴胺,再加入除杂后棉织物,将体系置于20℃水浴中震荡20h,取出干燥。
(3)将浓度为0.055mol/L的硝酸铁溶液和浓度为0.005mol/L的盐酸混合后,再浸入多巴胺改性棉织物,50℃水浴处理8h,干燥。
(4)将0.5g十二硫醇超声分散在200mL无水乙醇中,然后加入载体进行静置15h。
实施例2
一种耐水洗光催化超疏水棉织物的制备方法,包括如下步骤:
(1)向圆底烧瓶中加入丙酮至丙酮体积占烧圆底瓶容积的三分之一,将棉织物置于索氏提取器中,将该索氏提取器与上述盛有丙酮的圆底烧瓶联通,然后100℃水浴加热5.5h,取出干燥;
(2)对100mL Tris-HCl缓冲液调节pH值至8.5,然后向所述缓冲液溶液中加入0.2g多巴胺,再加入除杂后棉织物,将体系置于30℃水浴中震荡17h,取出干燥。
(3)将浓度为0.074mol/L的硫酸铁溶液和浓度为0.008mol/L的盐酸混合后,再浸入多巴胺改性棉织物,80℃水浴处理5h,干燥。
(4)将0.1g十二硫醇超声分散在50mL无水乙醇中,然后加入载体进行静置18h。
实施例3
一种耐水洗光催化超疏水棉织物的制备方法,包括如下步骤:
(1)向圆底烧瓶中加入丙酮至丙酮体积占烧圆底瓶容积的三分之一,将棉织物置于索氏提取器中,将该索氏提取器与上述盛有丙酮的圆底烧瓶联通,然后85℃水浴加热5h,取出干燥;
(2)对100mL Tris-HCl缓冲液调节pH值至8.5,然后向所述缓冲液溶液中加入0.15g多巴胺,再加入除杂后棉织物,将体系置于40℃水浴中震荡20h,取出干燥。
(3)将质量分数为20mg/mL的六水合氯化铁溶液和浓度为0.01mol/L的盐酸混合后,再浸入多巴胺改性棉织物,60℃水浴处理10h,干燥。
(4)将0.5g十二硫醇超声分散在200mL无水乙醇中,然后加入载体进行静置20h。
将本实施例所得耐水洗光催化超疏水棉织物置于日本生产的JSM-5600型喷金仪中,对样品进行喷金处理240s,然后将喷金处理后的样品进行电镜扫描,在温度为20℃、相对湿度为65%的恒温恒湿环境中,选取不同的放大倍数,不同的区域进行微观结构观察,并拍照存储。其结果如图1所示,其中左侧为原始棉织物的SEM图,右侧为本实施例所得耐水洗光催化超疏水棉织物的SEM图。
由图1可以看出,原始棉织物呈现出干净的白色外观,具有光滑的纤维表面和凹槽;而本实施例所得耐水洗光催化超疏水棉织物中,多巴胺棉织物在负载一层纳米β-FeOOH棒后,可以明显的看出光滑的织物表面有一层厚厚的纳米层,并且表面粗糙。
采用日本Rigaku公司生产的D/max 2500型X射线衍射仪对本实施例所得耐水洗光催化超疏水棉织物进行织物晶体结构测试,其中Cu Kα为放射源,管电压为40kV,管电流为200mA,波长扫描范围40-80°,扫描速度3°/min;其结果如图2和图3所示。
由图2和图3可以看出,原始棉织物的衍射峰分别为15.1°、16.7°、23.0°和34.5°,而本实施例所得耐水洗光催化超疏水棉织物在26.7°、34.0°、35.1°、39.2°、46.4°、52.2°和55.9°处分别检测到一系列新的峰,进一步证实纳米β-FeOOH在棉织物表面的成功负载。
实施例4
一种耐水洗光催化超疏水棉织物的制备方法,包括如下步骤:
(1)向圆底烧瓶中加入丙酮至丙酮体积占烧圆底瓶容积的三分之一,将棉织物置于索氏提取器中,将该索氏提取器与上述盛有丙酮的圆底烧瓶联通,然后90℃水浴加热5h,取出干燥;
(2)对100mL Tris-HCl缓冲液调节pH值至8.5,然后向所述缓冲液溶液中加入0.15g多巴胺,再加入除杂后棉织物,将体系置于40℃水浴中震荡15h,取出干燥。
(3)将质量分数为15mg/mL的六水合氯化铁溶液和浓度为0.01mol/L的盐酸混合后,再浸入多巴胺改性棉织物,60℃水浴处理10h,干燥。
(4)将0.5g十二硫醇超声分散在50mL无水乙醇中,然后加入载体进行静置20h。
将本实施例所得耐水洗光催化超疏水棉织物置于质量分数为10mg/mL的亚甲基蓝溶液中,仅在可见光照射下通过搅拌溶液,观察溶液在0min,30min,60min,90min,120min,150min,180min的颜色变化并测其荧光强度。其结果如图4所示。将本实施例所得耐水洗光催化超疏水棉织物经1-5次循环,置于质量分数为10mg/mL的亚甲基蓝溶液中,仅在可见光照射下通过搅拌溶液,观察溶液在0min,30min,60min,90min,120min,150min,180min的颜色变化并测其荧光强度。其结果如图5所示。
由图4可以看出,随着可见光照射时间的增加,亚甲基蓝溶液在665nm处的吸光度明显降低;当光照时间达到180min时,图谱中没有明显的吸收峰,说明大部分亚甲基蓝已经被分解。由图5可以看出,本实施例所得耐水洗光催化超疏水棉织物经1-5次循环后,其对亚甲基蓝降解极为稳定。
实施例5
一种耐水洗光催化超疏水棉织物的制备方法,包括如下步骤:
(1)向圆底烧瓶中加入丙酮至丙酮体积占烧圆底瓶容积的三分之一,将棉织物置于索氏提取器中,将该索氏提取器与上述盛有丙酮的圆底烧瓶联通,然后90℃水浴加热5h,取出干燥;
(2)对100mL Tris-HCl缓冲液调节pH值至8.5,然后向所述缓冲液溶液中加入0.15g多巴胺,再加入除杂后棉织物,将体系置于40℃水浴中震荡18h,取出干燥。
(3)将质量分数为16mg/mL的六水合氯化铁溶液和浓度为0.01mol/L的盐酸混合后,再浸入多巴胺改性棉织物,60℃水浴处理10h,干燥。
(4)将0.3g十二硫醇超声分散在100mL无水乙醇中,然后加入载体进行静置20h。
将本实施例所得耐水洗光催化超疏水棉织物进行静态水接触角(WCA)测试,采用2μL水滴或油滴在不同区域各测量5次。通过测试发现,织物的拒水性能优异,如图6所示,其接触角达到151.6°。经过20次水洗之后,织物的接触角仍然在150°以上。
实施例6
一种耐水洗光催化超疏水棉织物的制备方法,包括如下步骤:
(1)向圆底烧瓶中加入丙酮至丙酮体积占烧圆底瓶容积的三分之一,将棉织物置于索氏提取器中,将该索氏提取器与上述盛有丙酮的圆底烧瓶联通,然后90℃水浴加热5h,取出干燥;
(2)对100mL Tris-HCl缓冲液调节pH值至8.5,然后向所述缓冲液溶液中加入0.15g多巴胺,再加入除杂后棉织物,将体系置于40℃水浴中震荡20h,取出干燥。
(3)将质量分数为18mg/mL六水合氯化铁溶液和浓度为0.01mol/L的盐酸混合后,再浸入多巴胺改性棉织物,60℃水浴处理10h,干燥。
(4)将0.1g十二硫醇超声分散在150mL无水乙醇中,然后加入载体进行静置20h。
采用正己烷、煤油、甲苯、氯仿、二氯乙烷等一系列油水混合物进行重复分离。分离效率计算为分离后收集油的体积占分离前总体积的百分比。
将本实施例所得耐水洗光催化超疏水棉织物固定在两个支撑在锥形烧瓶上的玻璃容器之间,将油/水混合物缓慢地倒在织物表面,并在重力的驱动下分离混合物。通过测量分离溶剂的体积,并通过以下公式计算分离效率(R):
R=M/M0×100%,
其中M0为混合溶剂中原始油的体积,M为分离过程中收集的油的体积。
其结果如图7和图8所示,由图7和图8可知:本实施例所得耐水洗光催化超疏水棉织物的分离效率随着循环次数的增加略有下降,但50次循环后其效率仍保持在98%以上。
油/水混合物经本发明所得耐水洗光催化超疏水棉织物接触后,如图9所示,由于本发明所得棉织物具有优异的疏水亲油性能,将油性物质截留下来,而水可以自由通过棉织物。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (10)
1.一种耐水洗光催化超疏水棉织物,其特征在于,以表面负载有β-FeOOH纳米粒子的多巴胺改性棉织物为载体,在载体表面修饰有十二硫醇。
2.一种如权利要求1所述耐水洗光催化超疏水棉织物的制备方法,其特征在于,将除杂后棉织物进行多巴胺改性处理,接着将β-FeOOH纳米粒子负载在多巴胺改性棉织物表面得到载体,然后在载体表面采用十二硫醇进行修饰。
3.根据权利要求2所述耐水洗光催化超疏水棉织物的制备方法,其特征在于,所述多巴胺改性处理的具体操作如下:对Tris-HCl缓冲液调节pH值,然后向所述缓冲液溶液中加入多巴胺,再加入除杂后棉织物,将体系置于20-40℃水浴中震荡,取出干燥。
4.根据权利要求3所述耐水洗光催化超疏水棉织物的制备方法,其特征在于,水浴震荡时间为15-20h。
5.根据权利要求3所述耐水洗光催化超疏水棉织物的制备方法,其特征在于,对Tris-HCl缓冲液调节pH值至8.5。
6.根据权利要求3所述耐水洗光催化超疏水棉织物的制备方法,其特征在于,多巴胺与所述缓冲液溶液的质量体积比(g/mL)为0.1-0.2:100。
7.根据权利要求2所述耐水洗光催化超疏水棉织物的制备方法,其特征在于,所述将β-FeOOH纳米粒子负载在多巴胺改性棉织物表面的具体操作如下:将铁盐溶液和盐酸混合后,再浸入多巴胺改性棉织物,50-80℃水浴处理,干燥。
8.根据权利要求7所述耐水洗光催化超疏水棉织物的制备方法,其特征在于,铁盐溶液浓度为0.055-0.074mol/L,盐酸浓度为0.005-0.01mol/L。
9.根据权利要求7所述耐水洗光催化超疏水棉织物的制备方法,其特征在于,所述在载体表面采用十二硫醇进行修饰的具体操作如下:将十二硫醇超声分散在无水乙醇中,然后加入载体进行静置;优选地,十二硫醇与无水乙醇的质量体积比(g/mL)为0.1-0.5:50-200。
10.一种如权利要求1所述耐水洗光催化超疏水棉织物在光催化剂或水油分离的应用。
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