CN111688288A - 一种柔性纳米纤维滤膜及其制备方法 - Google Patents

一种柔性纳米纤维滤膜及其制备方法 Download PDF

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CN111688288A
CN111688288A CN202010441293.2A CN202010441293A CN111688288A CN 111688288 A CN111688288 A CN 111688288A CN 202010441293 A CN202010441293 A CN 202010441293A CN 111688288 A CN111688288 A CN 111688288A
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flexible
filter membrane
membrane
nanofiber filter
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代云茜
王云鹏
徐婉琳
邹茜茜
孙岳明
吴敏
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Nanjing Jinsibo Nano Technology Co ltd
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Abstract

一种柔性纳米纤维滤膜及其制备方法,S1、提供电纺和电喷前驱液以及非织造基布;S2、将电纺和电喷前驱液在环境温度为20‑30℃,湿度不高于50%的条件下,通过静电纺丝和静电喷雾得到纳米纤维膜;S3、将得到的纳米纤维膜在马弗炉经600℃煅烧2 h,升温速度为2℃/min,得到柔性纳米纤维膜。S4、将所制备的柔性纳米纤维膜与非织造基布进行压印,得到柔性纳米纤维滤膜,其中,柔性纤维膜设置在两层非织造基布之间。该制备方法通过简单的静电纺丝和静电喷雾法一步制成柔性纳米纤维滤膜,其工艺简单、成本较低,能制备得到物理化学性能优异的柔性纳米纤维滤膜,具有较大的应用前景。

Description

一种柔性纳米纤维滤膜及其制备方法
技术领域
本发明属于纳米材料膜技术,具体涉及一种通过静电纺丝和静电喷雾法得到的柔性纳米纤维滤膜及其制备方法。
背景技术
通过静电纺丝和静电喷雾法制备的纳米纤维膜具有一系列独有的特征和性质,比如高比表面积、孔隙率高、孔径分布小等,是种理想的高效过滤材料,为过滤技术的开发与设计开辟了新的思路。此外,另一方面显著特点是这些纳米纤维可以被方便地制备成为膜状,从而使其非常适合于一些基于膜的应用,包括过滤膜、分离。然而,传统的纳米纤维滤膜只能过滤固定粒径范围的颗粒,因此不能满足人们的生产需求。当人们需要过滤的颗粒的粒径大小发生变化时,就需要更换不同的纳米纤维膜,这样就使得人力成本和时间成本大大增加。此外,传统无机纳米纤维经焙烧后整体较脆,柔韧性较差,难以长时间使用。基于上述情况,本发明提出一种柔性纳米纤维膜过滤材料及其制备方法。
发明内容
解决的技术问题:本发明的目的在于提供一种柔性纤维滤膜及其制备方法,能通过简单的工艺和较低的成本制备得到柔性纳米纤维滤膜。
技术方案:一种柔性纳米纤维滤膜的制备方法,包括以下步骤:S1、提供电纺和电喷前驱液以及非织造基布;S2、将电纺和电喷前驱液在环境温度为20-30℃,湿度不高于50%的条件下,通过静电纺丝和静电喷雾得到纳米纤维膜;S3、将得到的纳米纤维膜在马弗炉经600℃煅烧2h,升温速度为2℃/min,得到柔性纳米纤维膜。S4、将所制备的柔性纳米纤维膜与非织造基布进行压印,得到柔性纳米纤维滤膜,其中,柔性纤维膜设置在两层非织造基布之间。
优选的,上述S1中,电纺前驱液中含有0.6g聚乙烯吡咯烷酮(PVP)、4.5mL乙醇、5mL丙酮、3mL乙酸以及一定量的乙酰丙酮铝和钛酸异丙酯。
优选的,上述S1中,取2mL电纺前驱液加入6mL或6.63mL乙醇中稀释得到电喷前驱液。
优选的,上述S1中,聚乙烯吡咯烷酮的分子量为1300000。
优选的,上述S2中,在静电纺丝和静电喷雾过程中,电纺电压为13-15kV,注射器针头和滚筒收集器的距离为10cm,微量注射泵移动速度为0.6mL/h。
优选的,上述S2中,在静电纺丝和静电喷雾过程中,电喷电压为18kV,注射器针头和滚筒接收器距离为10cm,微量注射泵移动速度为0.2mL/h。
上述制备方法制得的柔性纳米纤维滤膜。
有益效果:本发明的柔性纳米纤维滤膜的制备方法通过简单的工艺和较低的成本,能制备得到物理化学性能优异的柔性纳米纤维滤膜,其吸附效率最高达到99.2%以上,另外,该柔性纳米纤维滤膜相对于只由静电纺丝制备得到的普通柔性纳米纤维滤膜的力学性能更好,AT-30柔性纳米纤维滤膜的断裂强度是AT-30普通纳米纤维滤膜的断裂强度的3.9倍,具有较大的应用前景。
附图说明
图1为静电纺丝-静电喷雾双通道结合同轴纺丝装置示意图;
图2为力学测试装置示意图;
图3为AT-10普通和柔性纳米纤维抗拉强度对比图;
图4为AT-20普通和柔性纳米纤维抗拉强度对比图;
图5为AT-30普通和柔性纳米纤维抗拉强度对比图。
具体实施方式
下面结合附图和实例,对本发明的具体实施方式作进一步详细描述。以下实例用于说明本发明,但不用来限制本发明的范围。
实施例1:
a.采用静电纺丝-静电喷雾法制备铝质量分数为10%的AT-10柔性纤维滤膜:
首先,制备静电纺丝前驱液。将0.6g PVP粉末与4.5mL乙醇混合,搅拌过夜得到均匀透明的溶液,将5mL丙酮,0.46g乙酰丙酮铝,3mL乙酸和2.5mL钛酸异丙酯依次加入上述溶液中,室温搅拌使其完全溶解,得到黄色透明的前驱体溶液。
其次,制备静电喷雾前驱液。取2mL上述电纺前驱液,加入6.0mL乙醇进行稀释,室温搅拌得到浅黄色透明均匀的电喷前驱液。
再次,利用两台微量注射泵和两台高压直流电源分别接在一台转鼓上,同时独立工作,互不干扰。电纺和电喷前准备时每次分别用注射器吸入约3mL前驱液,并在上部预留1mL左右的空气空间,防止纺丝液被注射器污染。电纺电压为13kV-15kV,注射器针头与滚筒接收器之间的距离为10cm,微量注射泵推动速度为0.6mL/h;电喷电压为18kV,注射器针头与滚筒接收器之间距离为10cm,微量注射泵推动速度为0.2mL/h,收集由上述前驱体溶液制得的纤维,要求纺丝环境温度为20-30℃,湿度50%以下。
最后,将所得的纤维膜在马弗炉中于600℃焙烧120min,升温速率为2℃/min,得到氧化铝/二氧化钛纤维膜,用非织造基布封装得到AT-10柔性纳米纤维滤膜。
b.PM 2.5吸附性能测试:
把试验测试样品裁为25mm×50mm的滤膜,设置流速为85L/min,实验结果表明,AT-10柔性纳米纤维滤膜对PM 2.5的去除率如下表所示。
粒径 上游 下游 效率
0.3μm 402958 34347 91.4763%
0.5μm 321436 23536 92.6779%
1.0μm 134836 8 100.0000%
3.0μm 70195 0 100.0000%
5.0μm 15328 0 100.0000%
10.0μm 15 0 100.0000%
c.力学性能测试:
另外制备一组只通过静电纺丝法制得的AT-10普通纤维滤膜,将AT-10普通纤维滤膜和AT-10柔性纤维滤膜都裁成5mm×30mm的条状,固定于25mm×30mm的双层纸框架中。利用力学拉伸仪器从零开始增加拉力,将纤维向两边拉伸,直至纤维断裂。装置如图2所示。实验结果表明,AT-10柔性纤维滤膜的力学性能远远高于AT-10普通纤维滤膜。
实施例2:
a.采用静电纺丝-静电喷雾法制备铝质量分数为10%的AT-20柔性纤维滤膜:
首先,制备静电纺丝前驱液。将0.6g PVP粉末与4.5mL乙醇混合,搅拌过夜得到均匀透明的溶液,将5mL丙酮,1.04g乙酰丙酮铝,3mL乙酸和2.5mL钛酸异丙酯依次加入上述溶液中,室温搅拌使其完全溶解,得到黄色透明的前驱体溶液。
其次,制备静电喷雾前驱液。取2mL上述电纺前驱液,加入6.0mL乙醇进行稀释,室温搅拌得到浅黄色透明均匀的电喷前驱液。
再次,利用两台微量注射泵和两台高压直流电源分别接在一台转鼓上,同时独立工作,互不干扰。电纺和电喷前准备时每次分别用注射器吸入约3mL前驱液,并在上部预留1mL左右的空气空间,防止纺丝液被注射器污染。电纺电压为13kV-15kV,注射器针头与滚筒接收器之间的距离为10cm,微量注射泵推动速度为0.6mL/h;电喷电压为18kV,注射器针头与滚筒接收器之间距离为10cm,微量注射泵推动速度为0.2mL/h,收集由上述前驱体溶液制得的纤维,要求纺丝环境温度为20-30℃,湿度50%以下。
最后,将所得的纤维膜在马弗炉中于600℃焙烧120min,升温速率为2℃/min,得到氧化铝/二氧化钛纤维膜,用非织造基布封装得到AT-20柔性纳米纤维滤膜。
b.PM 2.5吸附性能测试:
把试验测试样品裁为25mm×50mm的滤膜,设置流速为85L/min,实验结果表明,AT-20柔性纳米纤维滤膜对PM 2.5的去除率如下表所示。
粒径 上游 下游 效率
0.3μm 625830 35869 94.2686%
0.5μm 598673 29385 95.0916%
1.0μm 10847 1 100.0000%
3.0μm 61294 0 100.0000%
5.0μm 9482 0 100.0000%
10.0μm 19 0 100.0000%
c.力学性能测试:
另外制备一组只通过静电纺丝法制得的AT-20普通纤维滤膜,将AT-20普通纤维滤膜和AT-20柔性纤维滤膜都裁成5mm×30mm的条状,固定于25mm×30mm的双层纸框架中。利用力学拉伸仪器从零开始增加拉力,将纤维向两边拉伸,直至纤维断裂。装置如图2所示。实验结果表明,AT-20柔性纤维滤膜的力学性能远远高于AT-20普通纤维滤膜。
实施例3:
a.采用静电纺丝-静电喷雾法制备铝质量分数为10%的AT-30柔性纤维滤膜:
首先,制备静电纺丝前驱液。将0.6g PVP粉末与4.5mL乙醇混合,搅拌过夜得到均匀透明的溶液,将5mL丙酮,1.0g乙酰丙酮铝,3mL乙酸和1.40mL钛酸异丙酯依次加入上述溶液中,室温搅拌使其完全溶解,得到黄色透明的前驱体溶液。
其次,制备静电喷雾前驱液。取2mL上述电纺前驱液,加入6.63mL乙醇进行稀释,室温搅拌得到浅黄色透明均匀的电喷前驱液。
再次,利用两台微量注射泵和两台高压直流电源分别接在一台转鼓上,同时独立工作,互不干扰。电纺和电喷前准备时每次分别用注射器吸入约3mL前驱液,并在上部预留1mL左右的空气空间,防止纺丝液被注射器污染。电纺电压为13kV-15kV,注射器针头与滚筒接收器之间的距离为10cm,微量注射泵推动速度为0.6mL/h;电喷电压为18kV,注射器针头与滚筒接收器之间距离为10cm,微量注射泵推动速度为0.2mL/h,收集由上述前驱体溶液制得的纤维,要求纺丝环境温度为20-30℃,湿度50%以下。
最后,将所得的纤维膜在马弗炉中于600℃焙烧120min,升温速率为2℃/min,得到氧化铝/二氧化钛纤维膜,用非织造基布封装得到AT-30柔性纳米纤维滤膜。
b.PM 2.5吸附性能测试:
把试验测试样品裁为25mm×50mm的滤膜,设置流速为85L/min,实验结果表明,AT-30柔性纳米纤维滤膜对PM 2.5的去除率如下表所示。
粒径 上游 下游 效率
0.3μm 698381 7821 98.8801%
0.5μm 659149 3497 99.4695%
1.0μm 106834 1 100.0000%
3.0μm 51068 0 100.0000%
5.0μm 8573 0 100.0000%
10.0μm 16 0 100.0000%
c.力学性能测试:
另外制备一组只通过静电纺丝法制得的AT-30普通纤维滤膜,将AT-30普通纤维滤膜和AT-30柔性纤维滤膜都裁成5mm×30mm的条状,固定于25mm×30mm的双层纸框架中。利用力学拉伸仪器从零开始增加拉力,将纤维向两边拉伸,直至纤维断裂。装置如图2所示。实验结果表明,AT-30柔性纤维滤膜的力学性能远远高于AT-30普通纤维滤膜。
综上所述:本发明的柔性纳米纤维滤膜的制备方法通过简单的工艺和较低的成本制备,能制备得到物理化学性能优异的复合纳米纤维滤膜,具有较大的应用前景。
以上所述仅表达了本发明的一种实施方式,其描述较为具体和详细,但并不能因此而理解对发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以作出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。

Claims (7)

1.一种柔性纳米纤维滤膜的制备方法,其特征在于包括以下步骤:
S1、提供电纺和电喷前驱液以及非织造基布;
S2、将电纺和电喷前驱液在环境温度为20-30 ℃,湿度不高于50%的条件下,通过静电纺丝和静电喷雾得到纳米纤维膜;
S3、将得到的纳米纤维膜在马弗炉经600 ℃煅烧2 h,升温速度为2 ℃/min,得到柔性纳米纤维膜;
S4、将所制备的柔性纳米纤维膜与非织造基布进行压印,得到柔性纳米纤维滤膜,其中,柔性纤维膜设置在两层非织造基布之间。
2.根据权利要求1所述的柔性纳米纤维滤膜的制备方法,其特征在于所述S1中,电纺前驱液中含有0.6 g聚乙烯吡咯烷酮(PVP)、4.5 mL乙醇、5 mL丙酮、3 mL乙酸以及一定量的乙酰丙酮铝和钛酸异丙酯。
3.根据权利要求1所述的柔性纳米纤维滤膜的制备方法,其特征在于所述S1中,取2 mL电纺前驱液加入6 mL或6.63 mL乙醇中稀释得到电喷前驱液。
4.根据权利要求2所述的柔性纳米纤维滤膜的制备方法,其特征在于所述S1中,聚乙烯吡咯烷酮的分子量为1300000。
5.根据权利要求1所述的柔性纳米纤维滤膜的制备方法,其特征在于所述S2中,在静电纺丝和静电喷雾过程中,电纺电压为13-15 kV,注射器针头和滚筒收集器的距离为10 cm,微量注射泵移动速度为0.6 mL/h。
6.根据权利要求1所述的柔性纳米纤维滤膜的制备方法,其特征在于所述S2中,在静电纺丝和静电喷雾过程中,电喷电压为18 kV,注射器针头和滚筒接收器距离为10 cm,微量注射泵移动速度为0.2 mL/h。
7.权利要求1至6任一项所述制备方法制得的柔性纳米纤维滤膜。
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