CN117004176B - 一种超双疏液泡棉及其制备方法 - Google Patents
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Abstract
本发明涉及一种超双疏液泡棉，该超双疏液泡棉是利用聚二甲基硅氧烷将P25二氧化钛纳米颗粒粘合在多孔蜜胺泡棉表面及内部，并由全氟辛基三氯硅烷不饱和修饰制得。同时，本发明还公开了该超双疏液泡棉的制备方法。本发明所得超双疏液泡棉在空气中具有超疏水性；其通过水预润湿，在水下具有超疏油性；通过空气预润湿，在水下具有超亲油性，对乳液可实现高效、快速分离。
Description
技术领域
本发明涉及油水分离和海洋防污技术领域，尤其涉及一种超双疏液泡棉及其制备方法。
背景技术
近年来，研究者们受大自然的启发，设计了多种具有不同超润湿性的功能材料。由于众多超润湿材料对水和油的亲和力截然相反，它们在油水分离技术的应用展现出明显的优势。多孔材料被人们广泛应用于油水分离，这些材料包括分离膜、海绵、纤维、气凝胶等。其中，超润湿膜材料利用尺寸筛分效应可对分层油水混合物和油水乳液实现高纯度、低能耗、便捷的分离。然而在分离过程中，膜的孔洞很容易堵塞阻挡了分离的进行。特别是对于分离含有高粘度油的乳液，此现象更为明显，甚至有些膜无法实现分离。而诸如海绵等具有大孔径的超润湿三维多孔材料可通过强吸附作用提高分离速度，为解决此问题开辟新的途径。由于乳液中乳化的液滴表面存在界面活性成分，油水界面膜稳固，导致液滴较为稳定不易合并，对其分离难度增加。目前大孔径超润湿吸附材料主要用于分层油水混合物的分离，但很少能够实现乳液分离。
为了拓宽超润湿材料的功能和应用场景，研究者们在同一表面上实现了多种不同介质中的超润湿性，如兼具超疏水性和水下超疏油性表面。然而，超疏水-水下超疏油表面的表面能所处范围狭窄，且表面粗糙度较高，因此实现该润湿性较为困难。人们开发出多种超疏水-水下超疏油性二维材料，而制备具有超疏水-水下超疏油性的三维材料还未曾报道。在多相介质中具有超润湿性的表面通常通过作为介质相的水或油的预润湿诱导实现在介质中超润湿性质的转换，而空气作为残留相用于诱导介质中超润湿性的转换却鲜有报道。
发明内容
本发明所要解决的技术问题是提供一种可用于高效乳液分离的超双疏液泡棉。
本发明所要解决的另一个技术问题是提供该超双疏液泡棉的制备方法。
为解决上述问题，本发明所述的一种超双疏液泡棉，其特征在于：该超双疏液泡棉是利用聚二甲基硅氧烷（PDMS）将P25二氧化钛纳米颗粒（TiO2）粘合在多孔蜜胺泡棉表面及内部，并由全氟辛基三氯硅烷（FOTS）不饱和修饰制得。
所述超双疏液泡棉在空气中具有超疏水性；其通过水预润湿，在水下具有超疏油性；通过空气预润湿，在水下具有超亲油性。
如上所述的一种超双疏液泡棉的制备方法，包括以下步骤：
⑴分别将聚二甲基硅氧烷（PDMS）和固化剂加入正己烷中，使其充分溶解并均匀混合，形成试剂A；
⑵将P25二氧化钛纳米颗粒（TiO2）加入试剂A中，超声处理并搅拌10 min，形成试剂B；
⑶市售的蜜胺泡棉清洗后浸入试剂B中反复挤压并超声处理10 min；之后取出泡棉，将多余的液体挤出并在150 ℃固化10 min；将上述浸涂及固化过程循环三次制得TiO2-PDMS泡棉；
⑷将全氟辛基三氯硅烷（FOTS）溶于正己烷中，形成试剂C；
⑸将TiO2-PDMS泡棉浸入试剂C中2 h后取出，用无水乙醇清洗并烘干，即得具有超双疏液性的TiO2@FOTS-PDMS泡棉。
所述步骤⑴试剂A中聚二甲基硅氧烷（PDMS）和固化剂的浓度分别为16.67 mg/mL、1.67 mg/mL。
所述步骤⑵试剂B中P25二氧化钛纳米颗粒（TiO2）的浓度为6.67 mg/mL。
所述步骤⑶试剂C中全氟辛基三氯硅烷（FOTS）的体积浓度为0.06%。
本发明与现有技术相比具有以下优点：
1、本发明利用聚二甲基硅氧烷将二氧化钛纳米颗粒粘合在多孔蜜胺泡棉表面及内部，并由全氟辛基三氯硅烷不饱和修饰制得，所得的超双疏液泡棉，孔径在100 μm左右，相比现有的乳液分离滤膜，其孔径更大。
2、本发明所述超双疏液泡棉是一种兼具超疏水性和水下超疏油性的三维多孔材料。当泡棉被水预润湿时，在水下展现出超疏油性；而当被空气预润湿时，则在水下展现出超亲油性，实现了水下超疏油和超亲油的转换，拓宽了超润湿材料的功能，可用于防污和油水分离。
3、本发明所述材料具有较大孔径，通过在水下对油滴强吸附作用提高分离速度，实现对多种水包油乳液，尤其对含有高粘度油乳液的快速、高效分离，分离后水的化学需氧量（COD）均在120 mg/L以下。
4、本发明在使用时仅需改变预润湿相，即可分别实现防污和快速、高效的乳液分离，克服了现有技术中乳液分离材料在实际应用时分离流速慢，孔易污染的缺陷。
5、本发明工艺简单，易操作，普适性强，不仅适用于市售的泡棉，还可以应用到其他多孔基底，制备超双疏液材料。
附图说明
下面结合附图对本发明的具体实施方式作进一步详细的说明。
图1为本发明实施例1制备的超双疏液泡棉的扫描电镜照片。
图2为本发明实施例1制备的超双疏液泡棉的光学照片和润湿性质的照片。
图3为本发明实施例1制备的超双疏液泡棉（a）分别经水和被空气预润湿后水下润湿性质的光学照片（b，c），并用于抗污（d，e）和油水分离（f，g）。
图4为本发明实施例1制备的超双疏液泡棉经空气预润湿后用于乳液分离，乳液分离前（左侧）后（右侧）的光学照片。
图5为本发明实施例1制备的超双疏液泡棉经空气预润湿后用于乳液分离，分离后滤液的化学需氧量（COD）。
具体实施方式
一种超双疏液泡棉，该超双疏液泡棉是利用聚二甲基硅氧烷（PDMS）将P25二氧化钛纳米颗粒（TiO2）粘合在多孔蜜胺泡棉表面及内部，并由全氟辛基三氯硅烷（FOTS）不饱和修饰制得。
超双疏液泡棉在空气中具有超疏水性；其通过水预润湿，在水下具有超疏油性；通过空气预润湿，在水下具有超亲油性。
一种超双疏液泡棉的制备方法，包括以下步骤：
⑴分别将聚二甲基硅氧烷（PDMS）和固化剂加入正己烷中，使其充分溶解并均匀混合，形成试剂A。
试剂A中聚二甲基硅氧烷（PDMS）和固化剂的浓度分别为16.67 mg/mL、1.67 mg/mL。这是因为：较低的浓度容易导致P25与基底的结合力降低，进而容易从基底表面脱落。较高的浓度容易导致泡棉表面及内部粗糙度降低，难以达到超双疏液效果。
⑵将P25二氧化钛纳米颗粒（TiO2）加入试剂A中，超声处理并搅拌10 min，形成试剂B。
试剂B中P25二氧化钛纳米颗粒（TiO2）的浓度为6.67 mg/mL。这是因为：较低的浓度容易导致泡棉表面及内部粗糙度降低，难以达到超双疏液效果。较高的浓度容易导致P25颗粒团聚，从而不能均匀包覆在基底表面及内部，团聚的颗粒与基底的结合力较弱，容易从基底表面脱落。
⑶市售的蜜胺泡棉清洗后浸入试剂B中反复挤压并超声处理10 min；之后取出泡棉，将多余的液体挤出并在150 ℃固化10 min；将上述浸涂及固化过程循环三次制得TiO2-PDMS泡棉。
⑷将全氟辛基三氯硅烷（FOTS）溶于正己烷中，形成试剂C。
试剂C中全氟辛基三氯硅烷（FOTS）的体积浓度为0.06%，该浓度会大大影响材料的表面能从而影响超双疏液性。
⑸将TiO2-PDMS泡棉浸入试剂C中2 h后取出，用无水乙醇清洗并烘干，即得具有超双疏液性的TiO2@FOTS-PDMS泡棉。
实施例1 一种超双疏液泡棉的制备方法，包括以下步骤：
⑴分别将1 g PDMS和0.1 g固化剂加入60 mL正己烷中，使其充分溶解并均匀混合。
⑵称取0.4 g的P25加入上述溶液中，超声处理并搅拌10 min，形成均一的TiO2-PDMS悬浊液。
⑶将3块清洗后的蜜胺泡棉（2 cm × 2 cm × 2 cm）浸入TiO2-PDMS悬浊液中反复挤压并超声处理10 min。之后取出泡棉，将多余的液体挤出并在150 ℃固化10 min。将上述浸涂及固化过程循环三次制得TiO2-PDMS泡棉。
⑷将30 μL的FOTS溶于50 mL正己烷中配制成修饰液。
⑸将TiO2-PDMS泡棉浸入修饰液中修饰2 h后，将泡棉取出用无水乙醇清洗并烘干，制得具有超双疏液性的TiO2@FOTS-PDMS泡棉。
对所制备的超双疏液泡棉进行性能测试：
如图1所示，经扫描电镜观察，泡棉纤维表面具有微-纳米多级结构，孔径约为100μm。
该超双疏液泡棉的光学照片如图2所示，其在空气中水的接触角和水下油的接触角为分别为158.9 ± 2.5°和162.1 ± 1.4°。因此，表现出优异的超疏水-水下超疏油性。
如图3所示，在空气中，水滴在制备的超双疏液泡棉上呈球形，而油滴则完全铺展浸润（a）。当超双疏液泡棉被水预润湿时，水下的油滴在制备的超双疏液泡棉上呈球形，在水下展现出超疏油性（b）；而当被空气预润湿时，在水下的油滴则完全铺展浸润，在水下展现出超亲油性（c），实现了水下超疏油性和水下超亲油性的转换。当经水预润湿的泡棉浸入到上层漂浮油的油水混合物中，取出观察其变化（d），其表面没有沾染任何油滴（e）；而当泡棉直接浸入到含有油滴的油水混合物时，其在水中能选择性地快速吸附油滴（f），被油污染的泡棉易冲洗（g）。实验表明分别利用空气和水对超双疏液泡棉预润湿，实现了油水分离和抗污功能的转换。
分别将不同粘度的油（PAO 2、PAO 10、PAO 40）和水以1/100的体积比混合，配制成多种稳定的水包油乳液。将制备的泡棉放入盛有乳液的离心管中剧烈振荡30 s进行乳液分离。分离过程结束后，观察分离前后乳液的变化。如图4所示，分离前所有的乳液均呈乳白色且较为浑浊，其中分布着无数细小的油滴（左侧）。分离后所有得到滤液均透明清澈，并且在光学显微镜下观察不到油滴的存在（右侧）。以上实验结果证明该超双疏液泡棉对多种含有不同粘度油的乳液，实现了有效分离。
进一步通过测量滤液的化学需氧量（COD）来详细评估该泡棉对各种乳液的分离效率，如图5所示，分离水包PAO 2乳液、水包PAO 10乳液和水包PAO 40乳液后所得到的滤液COD值很小，均在120 mg/L以下。
以上实验结果证明了该超双疏液泡棉对于不同的水包油乳液，尤其对含有高粘度油的乳液，实现了高效、快速分离。
Claims (1)
1.一种超双疏液泡棉，其特征在于：该超双疏液泡棉是利用聚二甲基硅氧烷将P25二氧化钛纳米颗粒粘合在多孔蜜胺泡棉表面及内部，并由全氟辛基三氯硅烷不饱和修饰制得；所述超双疏液泡棉在空气中具有超疏水性；其通过水预润湿，在水下具有超疏油性；通过空气预润湿，在水下具有超亲油性；其超双疏液泡棉的制备方法，包括以下步骤：
⑴分别将聚二甲基硅氧烷和固化剂加入正己烷中，使其充分溶解并均匀混合，形成试剂A；所述试剂A中聚二甲基硅氧烷和固化剂的浓度分别为16.67 mg/mL、1.67 mg/mL；
⑵将P25二氧化钛纳米颗粒加入试剂A中，超声处理并搅拌10 min，形成试剂B；所述试剂B中P25二氧化钛纳米颗粒的浓度为6.67 mg/mL；
⑶市售的蜜胺泡棉清洗后浸入试剂B中反复挤压并超声处理10 min；之后取出泡棉，将多余的液体挤出并在150 ℃固化10 min；将上述浸涂及固化过程循环三次制得TiO2-PDMS泡棉；
⑷将全氟辛基三氯硅烷溶于正己烷中，形成试剂C；所述试剂C中全氟辛基三氯硅烷的体积浓度为0.06%；
⑸将TiO2-PDMS泡棉浸入试剂C中2 h后取出，用无水乙醇清洗并烘干，即得具有超双疏液性的TiO2@FOTS-PDMS泡棉。
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