CN114452841A - 一种PVDF/PDMS@TiO2自清洁微纳米滤膜的制备方法 - Google Patents
一种PVDF/PDMS@TiO2自清洁微纳米滤膜的制备方法 Download PDFInfo
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Abstract
本发明公开了一种PVDF/PDMS@TiO2微纳米滤膜制备方法，所述的微纳米滤膜是由静电纺丝制备的直径分布在微纳米级别的PVDF/PDMS纤维内部镶嵌的平均粒径25nm的TiO2纳米颗粒构成的复合空气过滤膜。本发明属于空气过滤器技术领域，微纳米滤膜的高过滤性能、超疏水性能和光催化性能的协同作用保证对颗粒物高过滤的同时，实现对颗粒物的绿色降解，使微纳米滤膜具有自清洁功能，极大的延长了微纳米滤膜的使用寿命，在环境保护和空气污染防治具有很高的应用前景和理论指导价值。本发明采用的制备方法简单、可操作性强，成本低廉、环境友好、PM过滤效率较高，可作为PVDF/PDMS@TiO2微纳米滤膜大规模批量生产的方法，制备方法易于工业化生产，方法普适性强。
Description
技术领域
本发明涉及空气过滤器技术领域，具体是一种自清洁微纳米滤膜的制备方法。
背景技术
聚偏氟乙烯Poly(vinylidene fluoride)，英文缩写PVDF，主要是指偏氟乙烯均聚物或者偏氟乙烯与其他少量含氟乙烯基单体的共聚物，具有氟树脂和通用树脂的特性，具有良好的耐化学腐蚀性、耐高温性、耐氧化性、耐候性、耐射线辐射等性能。PVDF微纳米膜表面可以永久储存电荷而且具有较高的偶极矩，对空气中的PM颗粒具有较好的过滤性能。自从PVDF 材料作为空气过滤材料以来，为提高其过滤性能和使用寿命，很多相关研究者对其进行了表面改性。为了提高PVDF微纳米滤膜的过滤性能和使用寿命，本发明引入了PDMS(聚二甲基硅氧烷)和纳米TiO2。PDMS具有透明度高，耐热性、耐寒性好，疏水性好，可以有效改善纤维膜表面形貌具有超疏水性能。纳米TiO2有优异的紫外线吸收、光催化杀菌、分解有机污染物等性能，可以使纳米纤维表面更加粗糙，增强过滤性能，也实现对微纳米滤膜所吸附颗粒物中有机碳的光降解。
发明内容
一种PVDF/PDMS@TiO2自清洁微纳米滤膜的制备方法。所制备的微纳米滤膜对空气中的 PM2.5过滤性能达到99％以上、阻力压降56Pa，通过水滴可以表面的灰尘冲洗干净，利用光催化作用降解吸附的PM颗粒，实现了自清洁性能脱附效率可达到80％，极大的延长微纳米滤膜使用寿命降低PM颗粒带来的危害。
本发明通过以下技术方案实现：
一种PVDF/PDMS@TiO2自清洁微纳米滤膜，所述微纳米滤膜有PVDF、PDMS、TiO2按质量比7：3：0.5静电纺丝而成，PVDF膜的高滤低阻的性能协同PDMS的超疏水性能和纳米TiO2的光降解性能实现对PM2.5高过滤的同时完成自我清洁功能。
制备PVDF/PDMS@TiO2自清洁微纳米滤膜的制备详细过程如下：
步骤一：称取一定量的PVDF(聚偏氟乙烯)和纳米TiO2溶解在DMF(N,N-二甲基甲酰胺) 进行超声分散20min，超声分散结束后将溶液进行磁力搅拌，以800r/min速度搅拌6h；
步骤二：称取一定量的PDMS(聚二甲基硅氧烷)溶解到THF(四氢呋喃中)，进行磁力搅拌，以800r/min速度搅拌1h；
步骤三：将制备PVDF溶液和PDMS溶液混合，进行磁力搅拌至混合均匀，将混合溶液进行超声分散10min排出气泡；
步骤四：将制备的混合溶液转移到注射器中，用静电纺丝设备制膜，实验参数为：注射速率1.0mL/h；电压18kV；纳米纤维接收距离12cm；温度25℃；湿度40％，控制不同纺丝时间制备微纳米滤膜；
步骤五：将制备的微纳米滤膜在真空干燥箱内60℃内干燥24h，去除未挥发的溶剂。将制备的微纳米滤膜进行各项测试。
优异效果：一种PVDF/PDMS@TiO2自清洁微纳米滤膜的制备方法，本发明技术相对于现有技术具有如下优点：
PVDF/PDMS@TiO2自清洁微纳米滤膜的制备方法。所制备的微纳米滤膜对空气中的PM2.5过滤性能达到99％以上、阻力压降56Pa；微纳米滤膜的水接触角达到153°具有超疏水性能，通过水滴可以表面的灰尘冲洗干净；利用光催化作用降解吸附的PM颗粒，实现了自清洁功能脱附效率可达到80％以上，极大的延长微纳米滤膜使用寿命降低PM颗粒带来的危害。本发明方法选用的原材料价格便宜、制备工艺流程简易，可重复性较强，稳定性较好，在空气污染防治和环境保护领域有较高的应用价值。
附图说明
图1为微纳米滤膜过滤PM颗粒机理示意图；
图2为本发明PVDF/PDMS@TiO2自清洁微纳米滤膜过滤前后扫描电镜图；
图3为本发明PVDF/PDMS@TiO2自清洁微纳米滤膜光降解前后实物图；
图4为本发明PVDF/PDMS@TiO2自清洁微纳米滤膜自清洁测试图；
图5为本发明PVDF/PDMS@TiO2自清洁微纳米滤膜过滤示意图。
具体实施方式
下面结合附图和实施例来详细描述本发明。
取一个小烧杯称量0.7gPVDF和0.05gTiO2粉末分散到6.265gDMF中，并在100W功率超声分散20min，然后进行磁力搅拌在800r/min转速下搅拌6h。取一个等规格的烧杯，称取0.3gPDMS溶解到2.685gTHF溶液中，在800r/min转速下搅拌2h。然后将两个均匀进行混合，置于磁力搅拌器上在800r/min转速下搅拌6h至充分混合均匀。前驱液搅拌制备完成后置于100W功率超声分散20min去除溶解的气泡。将前驱液装入注射器内进行静电纺丝，电放参数为注射速率1.0mL/h；电压18kV；纳米纤维接收距离12cm；温度25℃；湿度40％；以中心位置摆动，摆动距离40mm，纺丝时间90min；将制备的微纳米滤膜在真空干燥箱内60℃下干燥24h，去除未挥发的溶剂。过滤性能检测采用自制设备对微纳米滤膜的过滤性能检测，自制的检测设备组成为由两个密封的箱体组成，将过滤膜夹在中间，一侧放入颗粒源(点燃的艾条)另一侧安装排风***往外排风形成负压，两个箱体内各放置一个PM颗粒检测器，通过两个检测器的比值来计算出过滤效率，本发明制备的微纳米滤膜过滤性能达到99％以上。另外在膜连接处的上风口和下风口连接差压计来测试阻力压降本发明制备的微纳米滤膜阻力压降56Pa。评判过滤空气滤膜过滤性能的主要依据，除过滤效率外还要考虑气体在纤维表面发生滑移前后的压力损失。故通常用质量因数QF来评价空气滤膜的综合过滤性能，Q＝[- ln(1-η)/ΔP]，其中η为过滤效率，ΔP为压降。跟传统过滤材料相比，本发明制备的微纳米滤膜具有较高的过滤效率同时具备较低的阻力压降，因此有较高的质量因数QF，QF可以达到0.083。自清洁性能的测试中，先测试微纳米的水接触角，测试水接触角平均为153°，实际测试当表面落满灰尘，随着水流的滑动，如图4所示可以将灰尘清理干净。对过滤后的纳米滤膜进行光催化测试，先称取空白膜的质量计为mc，然后进行过滤测试将过滤后的膜进行称重计为m0，将过滤后的纤维膜进行光照降解，隔一定时间间隔称去滤膜重量计为mi，降解效率ηd＝(m0-mi)/(m0-mc)*100％，通过四个小时的光降解，降解后颜色明显变浅，如图3所示，降解效率可以达到80％以上。
本发明PVDF/PDMS@TiO2自清洁微纳米滤膜同时兼具高效过滤效率及较低的阻力压降。本发明生产成本较低应用广泛，可以高效过滤PM颗粒实现空气净化的同时，完成对PM颗粒的绿色降解实现对污染物的自清洁。
实施例对本发明进行了具体描述，但只用于对本发明作进一步说明，不能理解为对本发明保护范围的限制。对于本领域的技术人员在不背离发明精神和保护范围的情况下做出的其它变化和修改，倘若这些修改和变型在本发明权利要求范围内，则本发明也意图包含这些变化和修改。
Claims (7)
1.一种PVDF(聚偏氟乙烯)/PDMS(聚二甲基硅氧烷)@TiO2具有自清洁功能的微纳米空气过滤膜，其特征在于：所述微纳米滤膜由PVDF、PDMS、TiO2按质量比：7:3:0.5混合均匀由静电纺丝技术制备而成。
2.7PVDF:3PDMS:0.5TiO2微纳米滤膜，其特征在于：以PVDF为基材采用静电纺丝制备的微纳米滤膜具有优异的透气性和过滤性能，微纳米滤膜内部纤维直径分布均匀、比表面积较高且孔径分布在微纳米级别可以高效过滤空气中的PM颗粒；PVDF材料和PDMS材料具有较小的表面功能，通过静电纺丝制备的微纳米滤膜表面较为粗糙，制备的微纳米滤膜具有超疏水性能疏水角达到153°，在过滤时表面沉积的灰尘或可溶性无机盐等在水流作用下冲刷干净；另外TiO2具有优异光降解性能，在光的照射下可以将PM颗粒中的对人体有害的有机碳成分进行绿色降解，以水和二氧化碳形式释放不会产生二次污染。微纳米滤膜的高过滤性能、超疏水性能和光降解性能协同作用对吸附的PM颗粒进行及时的降解，降低PM颗粒的危害提高了微纳米膜实验寿命。
3.一种7PVDF:3PDMS:0.5TiO2微纳米滤膜的制备方法，其特征在于，包括以下步骤：步骤一：制备前驱液，称量0.7gPVDF、0.3gPDMS和0.05gTiO2,溶解到6.265gDMF(N,N-二甲基甲酰胺)和2.685gTHF(四氢呋喃)混合溶液中，采用磁力搅拌800r/min搅拌12h使其充分溶解。
4.步骤二：将制好的前驱液进行超声分散10min，去除气泡。然后将前驱液转到注射器中，采用静电纺丝装置制备微纳米滤膜，实验参数：注射速率1.0mL/h；电压18kV；纳米纤维接收距离12cm；温度25℃；湿度40％；将制备的微纳米滤膜在真空干燥箱内60℃下干燥24h，去除未挥发的溶剂。
5.根据权利要求3所述的7PVDF:3PDMS:0.5TiO2微纳米滤膜的制备方法，其特征在于，步骤一中PVDF、PDMS、TiO2按照质量比为7:3:0.5混合。
6.根据权利要求3所述的7PVDF:3PDMS:0.5TiO2微纳米滤膜的制备方法，其特征在于，步骤二中超声分散和实验参数：注射速率1.0mL/h；电压18kV；纳米纤维接收距离12cm；温度25℃；湿度40；真空干燥箱内60℃下干燥12h。
7.一种自清洁空气过滤膜，其特征在于具有权利要求1所述的成分比7PVDF:3PDMS:0.5TiO2或采用权利要求3中制备步骤得到的自清洁空气过滤膜。
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