CN111925555A - 一种基于金属协同配合物构建超疏水涂层的方法 - Google Patents

一种基于金属协同配合物构建超疏水涂层的方法 Download PDF

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CN111925555A
CN111925555A CN202010795303.2A CN202010795303A CN111925555A CN 111925555 A CN111925555 A CN 111925555A CN 202010795303 A CN202010795303 A CN 202010795303A CN 111925555 A CN111925555 A CN 111925555A
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王艳青
丁丽萍
刘霞
何昊晨
曹泽雨
苏建民
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Abstract

本发明公开了一种基于金属协同配合物构建超疏水涂层的方法，通过采用一种简便、通用的逐层自组装方法可以在不同衬底表面构建超疏水涂层。具体是先在基体表面螯合酚羟基和金属离子配合物，形成具有微/纳米粗糙度的牢固表面，然后用浸泡法将长链烷基硫醇锚定在表面，达到表面超疏水改性的目的。该方法具有成本低、普遍适用性和稳定性好的特点，且无需加热和复杂设备，超疏水涂层经过强碱、强酸和盐溶液的长期处理后，仍然表现出优异的疏水性能，这种简单的策略为工业应用特别是处理和回收大规模溢油奠定了基础。

Description

一种基于金属协同配合物构建超疏水涂层的方法
技术领域
本发明属于油水分离技术领域，具体涉及一种基于金属协同配合物构建超疏水涂层的方法。
背景技术
原油泄漏对全球环境造成了巨大的破坏，造成了严重的经济损失。 原油中含有石油气体，苯，芳香烃和硫化氢，不仅对人和生物有毒，还导致大量的鱼、虾和鸟失去了生命。然而，面对原油泄漏，最常见的方法是直接燃烧，不仅造成石油资源的浪费，而且造成严重的空气污染。
为了解决溢油造成的环境污染，越来越多的新的除油技术和吸油材料被应用于油水分离领域。油水分离的材料一般为超疏水材料，超疏水材料具有优异的吸油、防水、防冰、耐腐蚀等性能，在处理大规模海洋污染及废油再利用方面具有潜在的应用前景。超疏水表面有两个基本条件：一是表面被疏水基团覆盖，二是表面具有微/纳米的粗糙度。基于这两个条件，目前已经出现了带有超疏水表面的各种材料。然而，探寻一种工艺简单、低成本的超疏水涂层构建方法仍然是挑战。
发明内容
本发明的目的是提供一种基于金属协同配合物构建超疏水涂层的方法，利用酚羟基与金属离子螯合，制备得到微/纳米粗糙表面，疏水烷基烃通过化学键牢固地吸附在微/纳米粗糙表面从而得到超疏水涂层。
为了实现上述发明目的，本发明采用以下技术方案：
一种基于金属协同配合物构建超疏水涂层的方法，包括以下步骤：
步骤1，将基材洗干净后烘干；
步骤2，将含有酚羟基且易氧化的物质溶于去离子水中，制备A液；
步骤3，将金属盐溶于去离子水中，制备B液；
步骤4，将尾端含有硫醇基团的长链烷烃溶于乙醇溶液中，制备C液；
步骤5，将步骤1的基材浸没到A液中浸泡15min，取出基材除去多于的液体后再浸没到B液中浸泡15min，取出基材除去多余的液体，此步骤可以反复循环多次，烘干；
步骤6，将步骤5中烘干后的基材浸没到C液中浸泡24小时，取出基材烘干，即可得到具有超疏水涂层的基材；
其中，所述含有酚羟基易氧化物质为单宁酸（TA）、没食子酸（GA）、左旋多巴（LCD）、邻苯二酚、鞣花酸或多巴胺（DA）中的一种或几种的混合物，所述金属盐为含有Mg2+、Zn2+、Fe3+、Cu2+、Ag+或Zr4+中的一种或几种可溶盐的混合物，所述尾端含有硫醇基团的长链烷烃为十二烷基硫醇、十六烷基硫醇或十八烷基硫醇中的一种或者几种的混合物。
进一步地，A液中溶质的浓度为1mg/ml~5mg/ml。
进一步地，B液中溶质的浓度为10 mg/ml~30mg/ml。
进一步地，C液中溶质浓度为10mg/ml~60mg/ml。
进一步地，所述基材为二维亲水网格材料或三维多孔材料。
在本发明中，所述二维亲水网格材料包括但不仅限于工业滤布，还可以是聚合物薄膜、金属网格材料等，三维多孔材料包括但不仅限于三聚氰胺海绵或聚氨酯海绵。
本发明的构建方法先在基体表面螯合酚羟基和金属离子配合物，形成具有微/纳米粗糙度的牢固表面，然后用浸泡法将长链烷基硫醇锚定在表面，达到表面超疏水改性的目的。该方法成本低，无需加热和复杂设备，对各种基材具有普遍适用性，制得的涂层经过强碱、强酸和盐溶液的长期处理后，仍然表现出优异的疏水性能，该疏水涂层为石油污染废水的大规模连续处理，水质净化以及废油在复杂环境中的再利用提供了新的方法。
附图说明
图1为实施例1中聚氨酯海绵改性前后的水接触角和扫描电子显微镜图片。
图2为实施例2中三聚氰胺海绵改性前后的水接触角和扫描电子显微镜图片。
图3为实施例3中聚氨酯海绵改性前后的水接触角和扫描电子显微镜图片。
图4为实施例4中棉布改性前后的水接触角和扫描电子显微镜图片。
图5为实施例5中三聚氰胺海绵改性前后的水接触角和扫描电子显微镜图片。
具体实施方式
下面结合具体实施例和附图对本发明的技术方案作进一步说明。
实施例1
聚氨酯海绵依次用乙醇和去离子水洗干净后烘干，浸没到2mg/ml的TA溶液中15min，取出海绵挤压出多余的TA溶液，浸没到10mg/ml 的FeCl3溶液中15min，取出海绵挤压出多余的FeCl3溶液，再次浸没到2mg/ml的TA溶液中15min后浸没到10mg/ml 的FeCl3溶液中15min，取出海绵挤压出多余的FeCl3溶液，反复循环5次，60℃鼓风烘箱烘干后浸没到20mg/ml的十八烷基硫醇溶液中24小时，取出改性海绵，烘干得到超疏水海绵。
图1为聚氨酯海绵改性前后的水接触角和扫描电子显微镜图片。由图片可知，改性后的聚氨酯海绵由亲水变成超疏水，且改性后涂层赋予基材微/纳米粗糙表面，进一步增强了疏水性。
实施例2
三聚氰胺海绵依次用乙醇和去离子水洗干净后烘干，浸没到2mg/ml的GA溶液中15min，取出海绵挤压出多余的GA溶液，浸没到10mg/ml 的MgCl2溶液中15min，取出海绵挤压出多余的MgCl2溶液，再次浸没到2mg/ml的GA溶液中15min后浸没到10mg/ml 的MgCl2溶液中15min，取出海绵挤压出多余的MgCl2溶液，反复循环2次，60℃鼓风烘箱烘干后浸没到20mg/ml的十八烷基硫醇醇溶液中24小时，取出改性海绵，烘干得到超疏水海绵。
图2为三聚氰胺海绵改性前后的水接触角和扫描电子显微镜图片。由图片可知，改性后的三聚氰胺海绵由超亲水变成超疏水性，改性涂层赋予基材微/纳米粗糙表面，进一步增强了疏水性。
实施例3
聚氨酯海绵依次用乙醇和去离子水洗干净后烘干，浸没到2mg/ml的TA溶液中15min，取出海绵挤压出多余的TA溶液，浸没到10mg/ml 的FeCl3溶液中15min，取出海绵挤压出多余的FeCl3溶液，再次浸没到2mg/ml的TA溶液中15min后浸没到10mg/ml 的FeCl3溶液中15min，取出海绵挤压出多余的FeCl3溶液，反复循环5次，60℃鼓风烘箱烘干后浸没到20mg/ml的十二烷基硫醇醇溶液中24小时，取出改性海绵，烘干得到超疏水海绵。
图3为聚氨酯海绵改性前后的水接触角和扫描电子显微镜图片。由图片可知，改性后的聚氨酯海绵由亲水变成超疏水，且改性后涂层赋予基材微/纳米粗糙表面，进一步增强了疏水性。
实施例4
棉布依次用乙醇和去离子水洗干净后烘干，浸没到4mg/ml的LCD溶液中15min，取出棉布挤压出多余的LCD溶液，浸没到10mg/ml 的FeCl3溶液中15min，取出棉布挤压出多余的FeCl3溶液，再次浸没到2mg/ml的LCD溶液中15min后浸没到10mg/ml 的FeCl3溶液中15min，取出海绵挤压出多余的FeCl3溶液，反复循环5次，60℃鼓风烘箱烘干后浸没到20mg/ml的十八烷基硫醇醇溶液中24小时，取出改性海绵，烘干得到超疏水棉布。
图4为棉布改性前后的水接触角和扫描电子显微镜图片。改性后的棉布由超亲水变成超疏水性，改性涂层赋予基材微/纳米粗糙表面，进一步增强了疏水性。
实施例5
三聚氰胺海绵依次用乙醇和去离子水洗干净后烘干，浸没到2mg/ml的邻苯二酚溶液中15min，取出海绵挤压出多余的邻苯二酚溶液，浸没到10mg/ml 的MgCl2溶液中15min，取出海绵挤压出多余的MgCl2溶液，再次浸没到2mg/ml的邻苯二酚溶液中15min后浸没到10mg/ml 的MgCl2溶液中15min，取出海绵挤压出多余的MgCl2溶液，反复循环2次，60℃鼓风烘箱烘干后浸没到20mg/ml的十六烷基硫醇醇溶液中24小时，取出改性海绵，烘干得到超疏水海绵。
图5为三聚氰胺海绵改性前后的水接触角和扫描电子显微镜图片。改性后的三聚氰胺海绵由超亲水变成超疏水性，改性涂层赋予基材微/纳米粗糙表面，进一步增强了疏水性。

Claims (6)

1.一种基于金属协同配合物构建超疏水涂层的方法，其特征在于：包括以下步骤：
步骤1，将基材洗干净后烘干；
步骤2，将含有酚羟基且易氧化的物质溶于去离子水中，制备A液；
步骤3，将金属盐溶于去离子水中，制备B液；
步骤4，将尾端含有硫醇基团的长链烷烃溶于乙醇溶液中，制备C液；
步骤5，将步骤1的基材浸没到A液中浸泡，取出基材除去多于的液体后再浸没到B液中浸泡，取出基材除去多余的液体，此步骤可以反复循环多次，烘干；
步骤6，将步骤5中烘干后的基材浸没到C液中浸泡，取出基材烘干，即可得到具有超疏水涂层的基材；
其中，所述含有酚羟基易氧化物质为单宁酸、没食子酸、左旋多巴、邻苯二酚、鞣花酸或多巴胺中的一种或几种的混合物，所述金属盐为含有Mg2+、Zn2+、Fe3+、Cu2+、Ag+或Zr4+中的一种或几种可溶盐的混合物，所述尾端含有硫醇基团的长链烷烃为十二烷基硫醇、十六烷基硫醇或十八烷基硫醇中的一种或者几种的混合物。
2.根据权利要求1所述的方法，其特征在于：所述A液中溶质的浓度为1mg/ml~5mg/ml。
3.根据权利要求1所述的方法，其特征在于：所述B液中溶质的浓度为10 mg/ml~30mg/ml。
4.根据权利要求1所述的方法，其特征在于：所述C液中溶质浓度为10mg/ml~60mg/ml。
5.根据权利要求1所述的方法，其特征在于：所述基材为二维亲水网格材料或三维多孔材料。
6.根据权利要求1所述的方法，其特征在于：步骤5中基材在A液中的浸泡时间为10-20min，基材在B液中的浸泡时间为10-20min；步骤6中基材在C液中的浸泡时间为24小时。
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