CN114232342B - 一种超疏水自清洁可用于油水分离棉织物的制备方法 - Google Patents

一种超疏水自清洁可用于油水分离棉织物的制备方法 Download PDF

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CN114232342B
CN114232342B CN202010941335.9A CN202010941335A CN114232342B CN 114232342 B CN114232342 B CN 114232342B CN 202010941335 A CN202010941335 A CN 202010941335A CN 114232342 B CN114232342 B CN 114232342B
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林绍建
刘鸿宇
兰建武
杨林
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Sichuan University
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Abstract

本发明公开了一种可用于油水分离的超疏水自清洁棉织物，以多巴胺改性棉织物为载体，在其表面负载Ag/AgCl纳米颗粒，再将该织物通过PDMS修饰。本发明公开了上述织物的制备方法，包括以下步骤：1.首先，用水和乙醇清洗棉织物。2.将棉织物浸入盐酸多巴胺的Tris溶液中，使多巴胺在织物上自聚合。3.将Ag/AgCl纳米颗粒负载到多巴胺改性的棉织物上。4.在织物表面修饰低表面能物质PDMS。本发明所得织物性质稳定，在各种溶剂、不同pH、超声以及砂纸摩擦等条件下均保持良好的超疏水性；对不同油水混合物均具有优异的分离性能，分离效率最高可达99.90％；并且能够在可见光条件下光催化降解染料和表面黏附的油污。

Description

一种超疏水自清洁可用于油水分离棉织物的制备方法
技术领域
本发明涉及油水分离技术领域，尤其涉及一种超疏水自清洁可用于油水分离棉织物的制备、应用。
背景技术
近年来，由于世界经济的飞速发展和工业化水平的日益提高，来自纺织、石化、金属/钢铁等行业的含油废水以及溢油事故严重威胁着我们的生活环境。因此，开发先进高效的除油处理技术已经迫在眉睫，具有科学和现实意义。传统的油水分离方法，如气浮、蒸馏、离心、电泳、化学分散剂降解等，具有很多缺点：其效率低、选择性低、操作成本高、能耗大。为了寻找能够解决上述问题的替代方法，基于特殊润湿性表面的油水分离材料引起了人们广泛的关注和研究。
油水分离的实质是界面问题。通过在基材上构造微纳结构调控表面粗糙度和降低表面自由能，我们可以获得超疏水-超亲油材料。当油水混合物接触超疏水超亲油膜表面时，油滴可以迅速在膜表面扩散并渗透。而水则因为不能湿润膜表面所以无法渗透到膜下，从而达到油水分离的目的。
Ag/AgCl是一种光催化材料，可在见光条件下可分解染料和有机污染物。将光催化和油水分离这两种技术复合可得到理想的水处理材料。
发明内容
为解决上述技术现存的问题，本发明提出了一种超疏水自清洁可用于油水分离的棉织物及其制备方法。该织物既具有超疏水性和良好的油水分离性能，又可利用可见光催化将污水中的染料以及黏附在织物表面的有机污物去除。
上述超疏水自清洁可用于油水分离棉织物的制备方法包括如下步骤：
步骤1：首先，将棉织物浸入超纯水中，并加热搅拌。在此期间，不断更换水以保持液体澄清。然后在超声波辐射下用乙醇洗涤棉织物。
步骤2：将三(羟甲基)氨基甲烷溶解在超纯水中，并用稀盐酸将溶液的pH值调节至碱性，以制备Tris缓冲液。然后将多巴胺盐酸盐溶解在Tris缓冲溶液中，并将经过预处理的棉织物浸入该溶液中，并在室温下轻轻摇动，以使多巴胺在织物上自聚合。最后，用超纯水漂洗织物，然后在真空烘箱中干燥。
步骤3：首先，将AgNO3溶解在超纯水中，然后向其中加入ZnCl2，发生化学反应以获得AgCl。同时，溶液中出现白色沉淀。磁力搅拌后，用氙气灯照射混合物以将氯化银还原成金属银。最初的白色悬浮液在辐照后变成紫黑色。然后将混合物抽滤，用超纯水洗涤，然后在真空烘箱中干燥。将干燥的紫黑色粉末球磨，然后获得非常小粒径的Ag/AgCl颗粒。
步骤4：通过超声波照射将上述制备好的Ag/AgCl颗粒分散在超纯水中。之后，将多巴胺改性的棉织物浸入悬浮液中。将反应混合物磁力搅拌。最后，将织物在真空烘箱中干燥。
步骤5：本发明中使用的PDMS可以由SYLGARD 184(双组分有机硅弹性体套件)制成。首先，将含有氢化硅基的A组分和含有乙烯基固化剂的B组分按10:1混合在一起，然后在搅拌下溶解于四氢呋喃中。之后，将用多巴胺改性的沉积Ag/AgCl的棉织物在该溶液中浸泡20分钟。最后，在100℃下干燥2小时完成涂覆。
附图说明
图1所示为本发明的实施例1中所制得的超疏水自清洁棉织物的SEM图，左上为未经任何处理的棉织物，右上为经过多巴胺改性处理后的棉织物，左下为沉积了Ag/AgCl的多巴胺改性棉织物，右下为在多巴胺改性棉织物上沉积Ag/AgCl之后再以PDMS修饰的超疏水自清洁可用于油水分离棉织物。
图2所示为本发明的实施例1中所制得的超疏水自清洁棉织物在空气中15微升水的静态接触角。
图3所示为本发明的实施例1中所制得的超疏水自清洁棉织物针对不同油水混合物的分离效率。其中Hexane是正己烷，Dichloromethane为二氯甲烷，Petroleum ether指石油醚，Toluene是甲苯，Chloroform为三氯甲烷。
图4所示为本发明的实施例1中所制得的超疏水自清洁棉织物利用可见光降解亚甲基蓝染液的的紫外吸收光谱图。
图5所示为本发明的实施例1中所制得的超疏水自清洁棉织物表面被油污黏附到降解去除整个过程中接触角的变化。
具体实施方式
下面结合具体实施例对本发明做进一步的解释说明。
本发明的最关键构思在于:通过多巴胺修饰棉织物将其功能化，然后在表面沉积具有光催化效果的Ag/AgCl，再将低表面能物质聚二甲基硅氧烷(PDMS)整理织物上，制备一种分离效果优异、化学稳定性好、机械强度高、可自清洁的油水分离材料。
实施例1
本发明公开的超疏水自清洁可用于油水分离棉织物的制备方法，制备步骤如下：
步骤1：棉织物预处理：
首先，将棉织物浸入超纯水中，并在80℃磁力搅拌4小时。在此期间，不断更换水以保持液体清澈。然后在超声波辐射下用乙醇将棉织物洗涤30分钟。
步骤2：用多巴胺修饰棉织物：
将三(羟甲基)氨基甲烷溶解在超纯水(10mmol/L)中，并用稀盐酸将溶液的pH值调节至8.5，以制备三缓冲液。然后将0.4g的多巴胺盐酸盐溶解在200mL的Tris缓冲溶液中，并将经过预处理的棉织物浸入该溶液中，并在室温下轻轻摇动24h，以使多巴胺在织物上自聚合。最后，用超纯水漂洗织物，然后在60℃的真空烘箱中干燥。
步骤3：Ag/AgCl颗粒的制备：
首先，将7.48g AgNO3溶解在440ml超纯水中，然后添加2.6g ZnCl2，以获得AgCl。同时，溶液中出现白色沉淀。磁力搅拌1h后，用氙气灯照射混合物30分钟以将氯化银还原成金属银。最初的白色悬浮液在辐照后变成紫黑色。然后将混合物抽滤，用超纯水洗涤3次，然后在60℃的真空烘箱中干燥。将干燥的紫黑色粉末球磨1h，然后获得非常小粒径的Ag/AgCl颗粒。
步骤4：在多巴胺改性织物上沉积Ag/AgCl：
通过超声波照射将0.4g的Ag/AgCl颗粒分散在200ml的超纯水中。之后，将多巴胺改性的棉织物浸入悬浮液中。将反应混合物磁力搅拌4小时。最后，将织物在60℃的真空烘箱中干燥。因此，通过这种方式，Ag/AgCl颗粒将牢固而均匀地沉积在织物上。
步骤5：用聚二甲基硅氧烷(PDMS)修饰织物：
本实验中使用的PDMS可以由SYLGARD 184(双部分有机硅弹性体套件)制成。首先，将3g的含有氢化硅基的A组分和0.3g的含有乙烯基固化剂的B部分混合在一起，然后在搅拌下溶解于100ml的四氢呋喃中。之后，我们将用多巴胺改性后沉积有Ag/AgCl的棉织物在该溶液中浸泡20分钟。最后，在100℃下干燥2小时后，成功制备该织物。
实验例：
1.水接触角测试
用Theta Lite光学接触角仪(瑞典Biolin)在空气中对织物进行水接触角测试，液滴大小为15微升。所测得的超疏水油水分离棉织物的接触角均在150°以上。
2.油水分离测试
分别选取正己烷、二氯甲烷、石油醚、甲苯以及氯仿与水(体积比1:1)形成油水混合物。将实施例1中制得的超疏水自清洁可用于油水分离棉织物置于油水分离装置中并用夹子固定好，然后倒入油水混合物进行油水分离，同时记录分离前后油的质量和所需时间。
油水分离效率通过以下公式计算：
分离效率＝(Mb/Ma)×100％
其中，Ma为分离前油的初始质量，Mb为经油水分离后油的质量。油水分离效率均为多次测量后取平均值得到。图3所示为分离不同有油水混合物的分离效率。可以看出，对于各种不同的油水混合物，本发明所制得的超疏水自清洁棉织物的分离效率均接近100％.
3.光催化降解染料性能测试
选用亚甲基蓝作为代表性染料，将其配成染液。将按照实施例1所制得的超疏水自清洁棉织物浸入染液中，置于能发出可见光的氙灯下照射，数小时后亚甲基蓝被Ag/AgCl降解，染液由蓝色变为无色。从开始照射到染液无色的过程中定时取样，之后用紫外可见分光光度计测量染液浓度。
4.油污黏附降解测试
首先将油酸溶解在丙酮中，然后吸取一定量的该溶液滴加到按实施例1所制备的超疏水自清洁棉织物上来模拟油污黏附。然后先用紫外光照射该织物四个小时，以使油污被Ag/AgCl催化降解成小分子易挥发物质。最后在140℃烘箱中处理4h，使油污降解成的小分子物质完全挥发。

Claims (6)

1.一种超疏水自清洁可用于油水分离的棉织物，其特征在于，以多巴胺对棉织物进行功能性整理，并负载Ag/AgCl纳米颗粒，再修饰低表面能物质PDMS；其制备方法如下：将除杂后的棉织物进行多巴胺功能性整理，接着通过光还原法制备Ag/AgCl纳米颗粒并负载到棉织物表面，最后在该织物表面采用PDMS进行修饰；所述Ag/AgCl纳米颗粒的制备方法为：首先，将AgNO3溶解在440mL超纯水中，然后添加ZnCl2，以获得白色AgCl沉淀；磁力搅拌后，用氙灯照射悬浮物以将AgCl还原成Ag/AgCl，最初的白色悬浮液在辐照后变成紫黑色；然后将悬浮液中黑紫色Ag/AgCl分离，并将其颗粒粒径降低；将颗粒粒径降低的方法为：采用高速球磨法对Ag/AgCl进行球磨，球磨时间为1h；将Ag/AgCl负载到棉织物表面的具体操作是：通过超声波将0.4g的Ag/AgCl颗粒分散在200mL的超纯水中；之后，将多巴胺改性的棉织物浸入悬浮液中，将反应混合物磁力搅拌4h；最后，将织物在60℃的真空烘箱中干燥。
2.一种如权利要求1所述的超疏水自清洁可用于油水分离棉织物的制备方法，其特征在于，将除杂后的棉织物进行多巴胺功能性整理，接着通过光还原法制备Ag/AgCl纳米颗粒并负载到棉织物表面，最后在该织物表面采用PDMS进行修饰；所述Ag/AgCl纳米颗粒的制备方法为：首先，将AgNO3溶解在440mL超纯水中，然后添加ZnCl2，以获得白色AgCl沉淀；磁力搅拌后，用氙灯照射悬浮物以将AgCl还原成Ag/AgCl，最初的白色悬浮液在辐照后变成紫黑色；然后将悬浮液中黑紫色Ag/AgCl分离，并将其颗粒粒径降低；将颗粒粒径降低的方法为：采用高速球磨法对Ag/AgCl进行球磨，球磨时间为1h；将Ag/AgCl负载到棉织物表面的具体操作是：通过超声波将0.4g的Ag/AgCl颗粒分散在200mL的超纯水中；之后，将多巴胺改性的棉织物浸入悬浮液中，将反应混合物磁力搅拌4h；最后，将织物在60℃的真空烘箱中干燥。
3.根据权利要求2所述的超疏水自清洁可用于油水分离棉织物的制备方法，其特征在于，所述棉织物除杂的具体操作如下：首先，将棉织物浸入超纯水中，并在80℃磁力搅拌4h；在此期间，不断更换水以保持液体清澈，然后在超声波辐射下用乙醇将棉织物洗涤30min。
4.根据权利要求2所述的超疏水自清洁可用于油水分离棉织物的制备方法，其特征在于，所述棉织物的多巴胺功能性整理的步骤为：将三(羟甲基)氨基甲烷溶解在超纯水10mmol/L中，并用稀盐酸将溶液的pH值调节至8.5，以制备缓冲液；然后将0.4g的多巴胺盐酸盐溶解在200mL的Tris缓冲溶液中，并将经过预处理的棉织物浸入该溶液中，并在室温下轻轻摇动24h，以使多巴胺在棉织物上自聚合；最后，用超纯水漂洗织物，然后在60℃的真空烘箱中干燥。
5.根据权利要求2所述的超疏水自清洁可用于油水分离棉织物的制备方法，其特征在于，磁力搅拌时间为1h；氙灯照射时间为30min。
6.根据权利要求2所述的超疏水自清洁可用于油水分离棉织物的制备方法，其特征在于，将悬浮液中黑紫色Ag/AgCl分离的具体操作如下：将悬浮液抽滤，所得固体用超纯水洗涤3次，然后在60℃的真空烘箱中干燥。
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