CN107119457B - 一种超疏水材料以及利用原位热聚合法制备该材料的方法 - Google Patents

一种超疏水材料以及利用原位热聚合法制备该材料的方法 Download PDF

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CN107119457B
CN107119457B CN201710452427.9A CN201710452427A CN107119457B CN 107119457 B CN107119457 B CN 107119457B CN 201710452427 A CN201710452427 A CN 201710452427A CN 107119457 B CN107119457 B CN 107119457B
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杨华伟
张宏杰
张吕鸿
杨娜
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Abstract

本发明涉及一种通过原位热聚合法制备的超疏水材料及其制备方法；该制备方法包括如下步骤：将带有苯乙烯基团的疏水性离子液体或离子型化合物溶解到有机溶剂中，并和微纳米颗粒充分混合分散，将基底材料浸渍在所述溶液中，然后将基底取出置于烘箱中，在一定的温度下发生原位热聚合反应，在一定反应时间后即得所述超疏水材料。本发明制备工艺简单，原料廉价易得，不需要特殊仪器设备，原子利用率为100％，可广泛用于任何基底上，具有极高的耐用性，可用于复杂的分离环境中。所制备的超疏水材料同时具有超亲油的特点，可以大规模的制备并应用于油水分离。

Description

一种超疏水材料以及利用原位热聚合法制备该材料的方法
技术领域
本发明具体涉及一种基于带有苯乙烯基团的疏水性离子液体或离子型化合物的原位热聚合制备超疏水材料的方法。
背景技术
随着石油需求量的增加和工业化程度的升高，油水分离技术的研究对于提高水和油的质量有着重要的意义。近年来，仿生超疏水材料由于其表面特殊的润湿性引起了人们的广泛关注。超疏水性是表面润湿性中的特殊的一种。超疏水表面是指对水及水溶液有排斥性的表面，水滴在其表面无法滑动铺展而保持球型滚动状，从而达到滚动自清洁的效果。自然界当中的荷叶是该种材料的典型代表。超疏水材料因具有自清洁性，抗污性，低粘附等特点使其在生活中多种用途，这种特殊的润湿性不仅能赋予固体表面优异的抗水性，而且在油水分离、自清洁材料、减阻、抗结冰等领域具有巨大的应用价值。
目前已被公开的方法有等离子体技术结合喷涂方法，在表面基底上形成涂层(中国专利CN 105969174 A)，用聚阳离子电解质水溶液以及聚二甲基硅氧烷溶液浸渍表面(中国专利CN 106215461 A)，沉积聚多巴胺和纳米银颗粒(中国专利CN 104562709 A)，采用氟化物等昂贵的低表面能物质(中国专利CN 104213108 A)，溶胶-凝胶法(中国专利CN105544187 A)等，但是目前这些制备超疏水材料的方法存在制备工艺复杂，成本昂贵，耐用性差等问题。
综上所述，为了处理水污染和降低燃油含水量，本专利研究了一种制备过程简单的，制备成本较低的，具有高耐用性的，并能连续用于油水分离过程的超疏水金属丝网和其制备方法。
发明内容
本发明的目的在于针对目前超疏水材料的制备缺陷，提供原位热聚合法制备超疏水材料，其工艺简单，原子利用率100％，耐用性强且适用于大规模工业化生产。本发明提及的超疏水材料的表面是由离子液体单体作为前躯体在氧气高温环境中原位热聚生成的高分子聚合物包裹基底，及被高分子聚合物包裹在材料表面的微纳米颗粒所构成。高分子聚合物均匀的包裹在基底的表面同时将微纳米颗粒也固定在其表面，使得材料表面同时拥有了粗糙性和低表面能的特性，从而使其拥有了超疏水的能力。
本发明的目的是通过如下措施来达到：
本发明所涉及一种超疏水材料，其特征在于，包括基底材料，所述基底材料上设有疏水性高分子聚合物包裹膜，以及被所述高分子聚合物包裹膜包裹在所述基底材料表面的微纳米颗粒。
进一步的，所述的超疏水材料，其中
所述基底材料包括但不限于多孔材料、膜材料、海绵、棉布织物、涤纶、不锈钢网、铜网、玻璃中的一种。
所述疏水性高分子聚合物包裹膜是由带有苯乙烯基团的离子液体或离子型化合物原位热聚合生成。
所述微纳米颗粒为粒径在50～300nm的无机颗粒，包括氧化铝，二氧化硅，二氧化钛，四氧化三铁，球形金纳米颗粒，球形铜纳米颗粒，球形银纳米颗粒，金纳米棒，银纳米棒，单层或多层碳纳米管等。
进一步的，所述的带有苯乙烯基团的离子液体或离子型化合物，其通式为：
式中，R1为碳原子数为1～4的烷基，R2至R4相同或不同，R2至R4为烷基或氟代烷烃，R3为碳原子数为12～18的烷基或氟代烷基；X为Cl-、Br-、BF4 -、PF6 -中的一种或多种。
进一步的，所述通过原位热聚合法制备的超疏水材料，其制备方法包含如下步骤：
(1)将带有苯乙烯基团的离子液体或离子型化合物溶解到有机溶剂中，并和微纳米颗粒混合分散；
(2)将基底材料浸渍在所述溶液中；
(3)然后将所述基底材料取出置于烘箱或其他反应装置中，在一定的反应温度下发生原位热聚合反应，一定反应时间后即得所述超疏水材料。
进一步的，所述的制备方法，其特征在于：所述有机溶剂为带有苯乙烯基团的离子液体或离子型化合物的良性溶剂，具体可为甲醇，乙醇，二氯甲烷，氯仿，N，N-二甲基甲酰胺，四氢呋喃，乙醚，丙酮中至少一种。
进一步的，所述的制备方法，其特征在于：所述离子液体单体在溶液中的浓度为1wt％～20wt％。
进一步的，所述的制备方法，其特征在于：所述微纳米颗粒在溶液中的浓度为 0.5～5wt％。
进一步的，所述的制备方法，其特征在于：所述步骤(2)中的浸渍时间为 0.1min～60min。
进一步的，所述的制备方法，其特征在于：所述步骤(3)中的反应温度为100～200℃。
进一步的，所述的制备方法，其特征在于：：所述步骤(3)中的反应时间为12～72h。
本发明通过带有苯乙烯基团的离子液体或离子型化合物在有氧环境下原位热聚合，得到高分子聚合物交联体包裹基底材料表面，并连同纳米颗粒一起为材料表面带来了复合的微纳米粗糙结构，并在高分子聚合物低表面能特征的共同作用下，使基底材料拥有了超疏水的特性。
本发明与现有技术相比，具有如下优点：
(1)制备工艺简单，仅为一步法制备，不需要特殊仪器设备。
(2)所用改性原料廉价易得，材料制备成本低。
(3)原子利用率为100％。
(4)所制备的超疏水材料具有超高耐用性，在超声震荡和重复使用50次后，其微观形貌和接触角值仍在150°以上；不溶于任何有机溶剂，适用于复杂的分离环境中。
(5)本发明制备方法可在基底表面形成极强的粘附作用，可广泛应用于任何基底上，不受类型所限。
(6)本发明所制备的超疏水材料同时具有超亲油性，可用于油水分离中。
附图说明
图1：原始金属网放大倍数为2000倍的扫描电镜图。
图2：所制备的超疏水金属网放大倍数为2500倍的扫描电镜图。
具体实施方式
为更好的理解本发明，下面结合实施例对本发明作进一步的说明，但是本发明的实施方式不限于此。应当知晓的是，所有的数字标识，例如pH、温度、时间、浓度，包括范围，都是近似值。要了解，虽然不总是明确的叙述所有的数字标识之前都加上术语“约”。同时也要了解，虽然不总是明确的叙述，本文中描述的试剂仅仅是示例，其等价物是本领域已知的。
实施例1：
将一种分子式如下式的离子液体前躯体
溶解于二氯甲烷中，形成浓度为1wt％的溶液，再加入0.5wt％的20nm的二氧化硅颗粒，超声分散30min，形成均一的溶液；将棉布织物浸泡在此溶液中1min后取出，然后放置到120℃烘箱中反应24h。所得超疏水材料的接触角为155°。
实施例2：
将一种分子式为下式的离子液体前躯体
溶解于甲醇中，形成浓度为5wt％的溶液，再加入1wt％的200nm的氧化铝颗粒，超声分散30min，形成均一的溶液；将铜网浸泡在此溶液中0.5min后取出，然后放置到110℃烘箱中反应12h。所得超疏水材料的接触角为158°。
本实施例与实施例1不同之处在于离子液体单体阴离子改为Br-，阳离子集团上最长碳链长度改为16，用量改为5wt％，溶剂改为甲醇，微纳米颗粒改成1wt％的200nm的氧化铝颗粒，基底材料换成铜网，浸泡时间有所缩短，烘箱温度为有所降低，反应时间减半，但最终制成的超疏水材料的接触角依旧很大。
实施例3：
将一种分子式为下式的离子液体前躯体
溶解于乙醇中，形成浓度为10wt％的溶液，再加入1wt％的300nm的二氧化钛颗粒，超声分散30min，形成均一的溶液；将不锈钢网浸泡在此溶液中30min后取出，然后放置到150℃烘箱中反应60h。所得超疏水金属网放大2500倍的电镜图如附图2所示，其接触角值为157°。
本实施例与实施例2不同之处在于离子液体单体的阴离子改成BF4 -，用量改为10wt％，溶剂改为乙醇，基底材料换成不锈钢网，微纳米颗粒改成300nm的二氧化钛颗粒，浸泡时间有所增加，烘箱温度为有所增加，反应时间增长。
实施例4：
将一种结构式为下式的离子型化合物单体
溶解于N，N-二甲基甲酰胺中，形成浓度为2wt％的溶液，再加入0.5wt％的50nm的球形银纳米颗粒，超声分散30min，形成均一的溶液；将海绵浸泡在此溶液中10min后取出，然后放置到160℃烘箱中反应72h。所得超疏水材料的接触角为156°。
本实施例与实施例3不同之处在于离子液体单体为全氟长碳链，阴离子改成Cl-，用量改为2wt％，微纳米颗粒改成0.5wt％的50nm的球形银纳米颗粒，基底材料换成海绵，浸泡时间有所减少，烘箱温度为有所升高，反应时间增长。
实施例5：
采用的离子型化合物，结构式为下式：
溶解于氯仿中，形成浓度为5wt％的溶液，再加入0.5wt％的直径为50nm的碳纳米管，超声分散30min，形成均一的溶液；将载玻片浸泡在此溶液中5min后取出，然后放置到140℃烘箱中反应36h。所得超疏水材料的接触角为156°。
本实施例与实施例4不同之处在于采用了含偏氟长碳链的离子液体单体，阴离子改成PF6 -，用量改为5wt％，微纳米颗粒改成0.5wt％的50nm的碳纳米管，基底材料换成载玻片，浸泡时间有所减少，烘箱温度为有所降低，反应时间减少。
上述具体实施例仅是为了说明本发明制备过程，并非是对实施方式的限定，所属领域专业人员可以在实施例的基础上变动或扩展来制得超疏水材料，因此无需穷举所有的实施例，而由此所引出的明显变动仍属于本发明的保护范围之内。

Claims (8)

1.一种超疏水材料，其特征在于：包括基底材料，所述基底材料上设有疏水性高分子聚合物包裹膜，以及被所述高分子聚合物包裹膜包裹在所述基底材料表面的微纳米颗粒；
所述基底材料为多孔材料、膜材料、海绵、棉布织物、涤纶、不锈钢网、铜网、玻璃中的一种；
所述疏水性高分子聚合物包裹膜是由带有苯乙烯基团的离子液体或离子型化合物原位热聚合生成；
所述带有苯乙烯基团的离子液体或离子型化合物的通式为：
式中，R1为碳原子数为1～4的烷基，R2至R4相同或不同，R2至R4为烷基或氟代烷烃，R3为碳原子数为12～18的烷基或氟代烷基；X为Cl-、Br-、BF4 -、PF6 -中的一种或多种；
所述微纳米颗粒为粒径在50～300nm的无机颗粒，所述无机颗粒为氧化铝、二氧化硅、二氧化钛、四氧化三铁、球形金纳米颗粒、球形铜纳米颗粒、球形银纳米颗粒、金纳米棒，银纳米棒、单层或多层碳纳米管中的一种或多种。
2.利用原位热聚合法制备权利要求1所述的超疏水材料的方法，其特征在于：包括如下步骤：
(1)将带有苯乙烯基团的离子液体或离子型化合物溶解到有机溶剂中，并和微纳米颗粒混合分散；
(2)将基底材料浸渍在所述溶液中；
(3)然后将所述基底材料取出，在一定的反应温度下发生原位热聚合反应。
3.根据权利要求2所述的制备方法，其特征在于：所述有机溶剂为带有苯乙烯基团的离子液体或离子型化合物的良性溶剂。
4.根据权利要求2所述的制备方法，其特征在于：所述离子液体或离子型化合物在所述有机溶剂中的浓度为1wt％～20wt％。
5.根据权利要求2所述的制备方法，其特征在于：所述微纳米颗粒在所述有机溶剂中的浓度为0.5～5wt％。
6.根据权利要求2所述的制备方法，其特征在于：所述步骤(2)中的浸渍时间为0.1min～60min。
7.根据权利要求2所述的制备方法，其特征在于：所述步骤(3)中的反应温度为100～200℃。
8.根据权利要求2所述的制备方法，其特征在于：所述步骤(3)中的反应时间为12～72h。
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