CN108097223A - 一种超声辅助相转化法制备多壁碳纳米管/聚偏氟乙烯多孔膜材料方法 - Google Patents

一种超声辅助相转化法制备多壁碳纳米管/聚偏氟乙烯多孔膜材料方法 Download PDF

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CN108097223A
CN108097223A CN201711040826.0A CN201711040826A CN108097223A CN 108097223 A CN108097223 A CN 108097223A CN 201711040826 A CN201711040826 A CN 201711040826A CN 108097223 A CN108097223 A CN 108097223A
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李广芬
李志鹏
郇洋洋
蒋策
李万盛
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Tianjin Polytechnic University
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Abstract

本发明涉及一种利用超声辅助相转化法制备多壁碳纳米管/聚偏氟乙烯多孔膜材料的方法。该制备方法包括以下步骤：1.将MWCNTs加入DMF中超声分散直至分散完全均匀；将PVDF粉末加入到MWCNT/DMF体系中加热搅拌得到均匀铸膜液；将所得铸膜液密封，静置在室温下隔夜脱泡；2.在玻璃板上用刮膜棒刮膜，然后将膜和玻璃板一同放入超声仪器中分别以不同功率、频率和超声时间进行超声处理，再放入蒸馏水水浴中，溶剂挥发，形成MWCNT/PVDF多孔膜材料；3.最后放置于真空烘箱中干燥，并保存。

Description

一种超声辅助相转化法制备多壁碳纳米管/聚偏氟乙烯多孔 膜材料方法
技术领域
本发明涉及一种超声辅助相转化法制备多壁碳纳米管/聚偏氟乙烯多孔膜材料，属于功能材料技术领域。
背景技术
PVDF膜具有高机械强度、抗紫外线、耐气候老化性、耐冲击性、耐磨性、耐热，耐酸、碱及卤素等化学试剂等多种优良性能，近年来，PVDF膜已被广泛应用于化工、环保、食品、医药和生化等诸多领域。然而，PVDF膜本身仍然存在一些问题限制了其在其他领域中的应用，尤其是在废水处理、生物分离、水的净化和分离等领域。
碳纳米管是碳原子组成的一维管状纳米材料，具有优异的力学性能和独特的传导性能。采用碳纳米管作为聚合物材料的增强体，不仅可以显著提高聚合物的力学性能，同时能够赋予聚合物材料许多新的功能，实现多功能高强复合材料。
超声法目前广泛用于材料清洗、溶液制备及高分子聚合过程等方面。超声波的介入可以促进物理或化学过程，并且在多孔膜形成过程中协助溶剂和非溶剂之间的质量传递，实现在结晶生长和聚合物膜分相期间的结构演化。当超声波照射的液体时，超声波化被视为声化学效应的主要机制，其中气泡塌陷产生强烈的局部加热，高压，微喷射，湍流，声流等。超声的物理效应包括增强传质，乳化，体热加热以及对固体的其他各种影响。此外，超声波被证明是聚合、降解聚合物和分散纳米颗粒的有力工具，并且它被广泛用于聚合物的本体或表面改性。
本发明介绍了一种通过超声波辅助相转化技术来制备多壁碳纳米管/聚偏氟乙烯多孔膜材料的方法。除了溶剂和非溶剂之间的相互扩散带来的相转化外，超声空化对相转化和所得膜形态具有显着影响。采用超声法制备多壁碳纳米管/聚偏氟乙烯多孔膜材料具有用时短、效果好且操作方便等优点。且可以通过控制超声功率、频率和时间来改变膜孔的形态。
发明内容
本发明的目的是多壁碳纳米管/聚偏氟乙烯多孔膜材料的制备。
本发明采用的技术方案是超声辅助相转化法制备多壁碳纳米管/聚偏氟乙烯多孔膜材料，该方法步骤如下：
(1)制备铸膜液
称取一定量的MWCNTs，以N，N_二甲基甲酰胺(DMF)为溶剂，超声使MWCNTs分散均匀。聚偏氟乙烯(PVDF)粉末在使用前置于烘箱中干燥一段时间，去除水分。将PVDF粉末加入到MWCNT/DMF体系中配成铸膜液，加热搅拌，使PVDF粉末充分溶解，得到均一溶液。将所得铸膜液密封，静置在室温下隔夜脱泡。
(2)超声辅助相转化法制备MWCNT/PVDF多孔膜材料
在玻璃板上用刮膜棒刮膜，然后将膜和玻璃板一同放入超声仪器中分别以不同功率、频率和超声时间进行超声处理，再放入蒸馏水水浴中，溶剂挥发，形成MWCNT/PVDF多孔膜材料。
所述复合膜通过超声辅助相转化法制得。
所述溶剂要选择一种能溶解聚偏氟乙烯的溶剂。
所述多壁碳纳米管质量分数为1％。
所述MWCNTs在DMF中超声40min。
所述铸膜液在70℃的恒温水浴中剧烈搅拌4h。
所述铸膜液密封，静置在室温下隔夜脱泡。
所述膜连同玻璃板浸入超声仪器中进行超声处理，取出再放入蒸馏水水浴中，溶剂挥发，形成MWCNT/PVDF多孔膜材料。
本发明的有益效果是：
(1)通过在聚合物中添加具有不同改性MWCNTs可有效地控制膜材料的孔结构，拓宽其应用领域。
(2)实验过程中膜的制备分三个阶段进行，操作较简单且所用时间短，大大降低了能耗和时间。
附图说明
图1是实施例制备的多壁碳纳米管/聚偏氟乙烯多孔膜材料扫描电子显微镜图片及多壁碳纳米管/聚偏氟乙烯多孔膜材料对亚甲基蓝染料的吸附曲线。
具体实施方式
采用超声辅助相转化法，制备多壁碳纳米管/聚偏氟乙烯多孔膜材料。
下面结合实施例对本发明作进一步的描述，以使本领域的技术人员可以更好的理解本发明并能予以实施，但所举实施例不作为对本发明的限定。
实施例1
多壁碳纳米管/聚偏氟乙烯多孔膜材料的制备，步骤如下：
(1)制备铸膜液
称取一定量的MWCNTs，以N，N_二甲基甲酰胺(DMF)为溶剂，超声使MWCNTs分散均匀。聚偏氟乙烯(PVDF)粉末在使用前置于烘箱中干燥一段时间，去除水分。将PVDF粉末加入到MWCNT/DMF体系中配成铸膜液，加热搅拌，使PVDF粉末充分溶解，得到均一溶液。将所得铸膜液密封，静置在室温下隔夜脱泡。
(2)超声辅助相转化法制备MWCNT/PVDF多孔膜材料
在玻璃板上用刮膜棒刮膜，然后将膜和玻璃板一同放入超声仪器中，在频率为45KHz下分别以不同功率60，80，100W和不同超声时间20，60s进行超声处理，随后放入蒸馏水水浴中，待溶剂挥发，形成MWCNT/PVDF多孔膜材料。
(3)最后将膜放置于真空烘箱中干燥，并保存。
图1是在频率为45KHz下分别以不同功率和超声时间进行超声处理制备的多壁碳纳米管/聚偏氟乙烯多孔膜的SEM图及对亚甲基蓝染料的吸附曲线图。由图可见，超声功率为60W，超声时间为60s条件下所制备的MWCNT/PVDF多孔膜材料断面出现了规整的大指孔、孔隙率高、对亚甲基蓝的吸附效果最好。

Claims (8)

1.一种超声辅助相转化法制备多壁碳纳米管/聚偏氟乙烯多孔膜材料方法，其特征在于，其制备步骤如下：
(1)铸膜液的制备
称取一定量的MWCNTs，以N，N_二甲基甲酰胺(DMF)为溶剂，超声使MWCNTs分散均匀。聚偏氟乙烯(PVDF)粉末在使用前置于烘箱中干燥一段时间，去除水分。将PVDF粉末加入到MWCNT/DMF体系中配成铸膜液，70℃下水浴加热搅拌4小时，使PVDF粉末充分溶解，得到均一溶液。将所得铸膜液密封，静置在室温下隔夜脱泡。
(2)将铸膜液用刮膜棒在玻璃板上刮膜，然后将膜和玻璃板一同放入超声仪器中分别以不同功率、频率和超声时间进行超声处理，再放入蒸馏水水浴中，待溶剂挥发，形成MWCNT/PVDF多孔膜材料。
(3)最后将膜放置于真空烘箱中干燥，并保存。
2.根据权利要求1所述的方法，其特征在于，所述多孔膜材料经过超声辅助相转化法处理。
3.根据权利要求1所述的方法，其特征在于，所述的溶剂要选择一种能溶解聚合物膜材料和分散另外一种添加剂。
4.根据权利要求1所述的方法，其特征在于，所述多壁碳纳米管所占质量分数为1％。
5.根据权利要求1所述的方法，其特征在于，所述MWCNTs在DMF中超声40min。
6.根据权利要求1所述的方法，其特征在于，所述铸膜液在70℃的恒温水浴中剧烈搅拌4h。
7.根据权利要求1所述的方法，其特征在于，所述铸膜液密封，静置在室温下隔夜脱泡。
8.根据权利要求1所述的方法，其特征在于，所述液膜连同玻璃板浸入超声仪器中进行超声处理，取出再放入蒸馏水水浴中，待溶剂挥发形成MWCNT/PVDF多孔膜材料。
CN201711040826.0A 2017-10-30 2017-10-30 一种超声辅助相转化法制备多壁碳纳米管/聚偏氟乙烯多孔膜材料方法 Pending CN108097223A (zh)

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