CN111809252A - 复合陶瓷纳米纤维膜及其制备方法和应用 - Google Patents

复合陶瓷纳米纤维膜及其制备方法和应用 Download PDF

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CN111809252A
CN111809252A CN202010521037.4A CN202010521037A CN111809252A CN 111809252 A CN111809252 A CN 111809252A CN 202010521037 A CN202010521037 A CN 202010521037A CN 111809252 A CN111809252 A CN 111809252A
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nanofiber membrane
ceramic nanofiber
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代云茜
徐婉琳
孙岳明
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Nanjing Jinsibo Nano Technology Co ltd
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Abstract

复合陶瓷纳米纤维膜及其制备方法和应用，将聚乙烯吡咯烷酮溶解在乙醇中作为纺丝前驱液；向前驱液中添加陶瓷材料的物质源以及相应的溶剂、助剂，利用微流体喷气纺丝设备，保持金属针头与接收器之间距离为10‑50 cm，液体流速为0.5‑4 mL/h，气压0.2‑3 MPa的条件下，采用卷对卷方式收集所得纤维膜，其中转轴速度为100‑300 r/min。在高温空气中焙烧后得到疏松多孔的陶瓷纳米纤维膜。本发明制备的陶瓷纤维膜比表面积大、孔隙率高、光催化性能及抗菌性能良好，可用于空气过滤及个人抗菌防护等领域。

Description

复合陶瓷纳米纤维膜及其制备方法和应用
技术领域
本发明属于陶瓷纳米纤维膜技术领域，具体涉及一种复合陶瓷纳米纤维膜及其制备方法和应用。
背景技术
目前生产高质量的陶瓷纤维多采用静电纺丝技术，尽管静电纺丝技术具有多功能性，但仍有一些缺点限制了其在工业上的应用，如需要高压电源、对溶液电导率要求高、产量低、损耗大、耗时长等。而通过微流体气喷纺丝方式制备的陶瓷纤维膜，利用高速压缩空气喷射拉伸聚合物溶液，可以有效避免原料浪费，实验环境及装置更简单便捷，极大缩短了纺丝时间；由于不使用高压电源等危险装置，更加安全。
发明内容
解决的技术问题：本发明提供一种复合陶瓷纳米纤维膜及其制备方法和应用，通过高速压缩空气喷射拉伸聚合物溶液，极大缩短了纺丝时间；同时，对纺丝液没有导电性等的要求，打破原有静电纺丝的限制，为陶瓷纤维的规模化生产和工业推广提供了有益条件。此外，该方法制备的氧化铝/二氧化钛复合陶瓷纤维可利用氧化铝、二氧化钛本征的氧化性、光热性能进行杀菌灭毒，应用于空气过滤和个人防护。
技术方案：复合陶瓷纳米纤维膜的制备方法，步骤为：a.配制10wt.％-20wt.％的聚乙烯吡咯烷酮(PVP)的乙醇溶液，将陶瓷材料物质源及其良溶剂、助剂依次加入上述溶液中，室温搅拌使其完全溶解，得到均匀的前驱体溶液，其中PVP的乙醇溶液、良溶剂、助剂的体积比例为9:(5-15):(2-10)；所述陶瓷材料物质源为钛酸异丙酯和乙酰丙酮铝，其中乙酰丙酮铝的质量分数为5-50wt.％，钛酸异丙酯与乙醇的体积比为(2-5):9；b.利用微流体气喷纺丝装置，将前驱体溶液制成纳米纤维；c.将纳米纤维在马弗炉中600℃焙烧1-2h，升温速率为2.0℃/min，得到氧化铝/二氧化钛复合陶瓷纳米纤维；d.用两层无纺布封装陶瓷纳米纤维，成为陶瓷纳米纤维基复合抗菌膜。
优选的，上述聚乙烯吡咯烷酮的分子量为1300000。
上述乙酰丙酮铝和钛酸异丙酯高温分解后Al2O3和TiO2质量比为(1-19):19。
优选的，上述良溶剂为乙醇和丙酮，所述助剂为乙酸，乙醇、丙酮、乙酸的体积比为9:10:6。
上述微流体气喷纺丝装置的金属针头与接收器之间的距离为30-50cm，液体流速为0.5-4mL/h，气压0.2-3MPa的条件下，采用卷对卷方式收集所得纤维膜，其中转速为100-300rpm，环境温度25℃，湿度不超过30-50wt.％。
优选的，所采用金属针头为不锈钢工业实验加长针，7号22G针头。
优选的，上述无纺布的克重量为60g。
上述制备方法制得的复合陶瓷纳米纤维膜。
上述复合陶瓷纳米纤维膜在制备空气过滤及个人防护产品中的应用。
有益效果：本发明通过微流体气喷纺丝技术所制备的氧化铝/二氧化钛陶瓷纳米纤维，可以实现大面积、规模化、连续生产，突破了原有静电纺丝技术在陶瓷纳米纤维上的限制，有望将其工业化。本发明制备的氧化铝/二氧化钛陶瓷纳米纤维，具有疏松多孔的结构，比表面积大，同时具有良好的光催化性、抗菌性，可将其应用于空气过滤、个人抗菌防护等领域。
附图说明
图1为微流体气喷纺丝技术原理示意图；
图2为氧化铝/二氧化钛复合陶瓷纳米纤维膜SEM图和纤维直径分布图(纺丝液流速为0.5mL/h，气体流速7m/s)；其中a为氧化铝/二氧化钛复合陶瓷纳米纤维膜SEM图，b为氧化铝/二氧化钛复合陶瓷纳米纤维膜SEM图和纤维直径分布图；
图3为氧化铝/二氧化钛复合陶瓷纳米纤维膜纤维直径分布图(纺丝液流速为2mL/h，气体流速7m/s)；
图4为氧化铝/二氧化钛复合陶瓷纳米纤维膜纤维直径分布图(纺丝液流速为2mL/h，气体流速10m/s)；
图5为氧化铝/二氧化钛复合陶瓷纳米纤维膜纤维直径分布图(纺丝液流速为3.5mL/h，气体流速7m/s)；
图6为氧化铝/二氧化钛复合陶瓷纳米纤维膜纤维直径分布图(纺丝液流速为3.5mL/h，气体流速10m/s)；
图7为氧化铝/二氧化钛复合陶瓷纳米纤维膜纤维实物图(纺丝液流速为3.5mL/h，气体流速10m/s，纺丝时间10min)；
图8为空气滤膜颗粒过滤效率检测装置示意图。
具体实施方式
实施例1
a.采用微流体气喷纺丝法制备氧化铝/二氧化钛/无纺布复合吸附材料(液体流速0.5mL/h，气体流速7m/s)：首先，制备前驱液：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，1.00g乙酰丙酮铝，3mL乙酸和1.43mL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，保持金属针头(针头为工业实验加长针，7号22G针头)与接收器之间距离为40cm，液体流速为0.5mL/h，气体流速7m/s的条件下，采用卷对卷方式收集所得纤维膜，其中转速100-300rpm，要求环境温度25℃，湿度不超过30-50％，接收时间1h。最后，将所得的PVP/乙酰丙酮铝/四异丙醇钛纤维在马弗炉中于600℃焙烧120min，升温速率为2.0℃/min，加热过程中PVP和乙酰丙酮铝分解，得到氧化铝/二氧化钛复合陶瓷纤维。用克重量为60g的无纺布上下两层封装氧化铝/二氧化钛膜，得到完整的氧化铝/二氧化钛无纺布复合吸附网。
b.氧化铝/二氧化钛/无纺布复合膜过滤测试：把试验测试样品裁成直径为1±0.2cm的圆形滤膜，置于图8所示的检测台上，设置流速为85L/min，实验结果表明，氧化铝/二氧化钛/无纺布复合吸附网对PM 2.5的去除率如下表所示。
Figure BDA0002532046450000031
实施例2
a.采用微流体气喷纺丝法制备氧化铝/二氧化钛/无纺布复合吸附材料(液体流速2mL/h，气体流速7m/s)：首先，制备前驱液：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，1.00g乙酰丙酮铝，3mL乙酸和1.43mL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，保持金属针头与接收器之间距离为40cm，液体流速为2mL/h，气体流速7m/s的条件下，采用卷对卷方式收集所得纤维膜，其中转速100-300rpm，要求环境温度25℃，湿度不超过30-50％，接收时间1h。最后，将所得的PVP/乙酰丙酮铝/四异丙醇钛纤维在马弗炉中于600℃焙烧120min，升温速率为2.0℃/min，加热过程中PVP和乙酰丙酮铝分解，得到氧化铝/二氧化钛复合陶瓷纤维。用克重量为60g的无纺布上下两层封装氧化铝/二氧化钛膜，得到完整的氧化铝/二氧化钛无纺布复合吸附网。
b.氧化铝/二氧化钛/无纺布复合膜过滤测试：把试验测试样品裁成直径为1±0.2cm的圆形滤膜，置于图8所示的检测台上，设置流速为85L/min，实验结果表明，氧化铝/二氧化钛/无纺布复合吸附网对烟气颗粒的去除率如下表所示。
Figure BDA0002532046450000041
实施例3
a.采用微流体气喷纺丝法制备氧化铝/二氧化钛/无纺布复合吸附材料(液体流速2mL/h，气体流速10m/s)：首先，制备前驱液：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，1.00g乙酰丙酮铝，3mL乙酸和1.43mL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，保持金属针头与接收器之间距离为40cm，液体流速为2mL/h，气体流速10m/s的条件下，采用卷对卷方式收集所得纤维膜，其中转速100-300rpm，要求环境温度25℃，湿度不超过30-50％，接收时间1h。最后，将所得的PVP/乙酰丙酮铝/四异丙醇钛纤维在马弗炉中于600℃焙烧120min，升温速率为2.0℃/min，加热过程中PVP和乙酰丙酮铝分解，得到氧化铝/二氧化钛复合陶瓷纤维。用克重量为60g的无纺布上下两层封装氧化铝/二氧化钛膜，得到完整的氧化铝/二氧化钛无纺布复合吸附网。
b.氧化铝/二氧化钛/无纺布复合膜过滤测试：把试验测试样品裁成直径为1±0.2cm的圆形滤膜，置于图8所示的检测台上，设置流速为85L/min，实验结果表明，氧化铝/二氧化钛/无纺布复合吸附网对烟气颗粒的去除率如下表所示。
Figure BDA0002532046450000042
实施例4
a.采用微流体气喷纺丝法制备氧化铝/二氧化钛/无纺布复合吸附材料(液体流速3.5mL/h,气体流速10m/s)：首先，制备前驱液：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，1.00g乙酰丙酮铝，3mL乙酸和1.43mL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，保持金属针头与接收器之间距离为40cm，液体流速为3.5mL/h，气体流速10m/s的条件下，采用卷对卷方式收集所得纤维膜，其中转速100-300rpm，要求环境温度25℃，湿度不超过30-50％，接收时间1h。可得到如图8所示的烧前尺寸为20cm×60cm纤维膜。最后将所得的PVP/乙酰丙酮铝/四异丙醇钛纤维在马弗炉中于600℃焙烧120min，升温速率为2.0℃/min，加热过程中PVP和乙酰丙酮铝分解，得到氧化铝/二氧化钛复合陶瓷纤维。用克重量为60g的无纺布上下两层封装氧化铝/二氧化钛膜，得到完整的氧化铝/二氧化钛无纺布复合吸附网。
b.氧化铝/二氧化钛/无纺布复合膜过滤测试：把试验测试样品裁成直径为1±0.2cm的圆形滤膜，置于图8所示的检测台上，设置流速为85L/min，实验结果表明，氧化铝/二氧化钛/无纺布复合吸附网对烟气颗粒的去除率如下表所示。
Figure BDA0002532046450000051
氧化铝/二氧化钛/无纺布复合膜纤维直径、膜厚对比
Figure BDA0002532046450000052

Claims (9)

1.复合陶瓷纳米纤维膜的制备方法，其特征在于步骤为：a.配制10 wt.%-20 wt.%的聚乙烯吡咯烷酮（PVP）的乙醇溶液，将陶瓷材料物质源及其良溶剂、助剂依次加入上述溶液中，室温搅拌使其完全溶解，得到均匀的前驱体溶液，其中PVP的乙醇溶液、良溶剂、助剂的体积比例为9:(5-15):(2-10)；所述陶瓷材料物质源为钛酸异丙酯和乙酰丙酮铝，其中乙酰丙酮铝的质量分数为5-50 wt.%，钛酸异丙酯与乙醇的体积比为(2-5):9；b. 利用微流体气喷纺丝装置，将前驱体溶液制成纳米纤维； c. 将纳米纤维在马弗炉中600 ℃焙烧1-2 h，升温速率为2.0 ℃/min，得到氧化铝/二氧化钛复合陶瓷纳米纤维；d. 用两层无纺布封装陶瓷纳米纤维，成为陶瓷纳米纤维基复合抗菌膜。
2.根据权利要求1所述复合陶瓷纳米纤维膜的制备方法，其特征在于所述聚乙烯吡咯烷酮的分子量为1300000。
3.根据权利要求1所述复合陶瓷纳米纤维膜的制备方法，其特征在于所述乙酰丙酮铝和钛酸异丙酯高温分解后Al2O3和TiO2质量比为(1-19):19。
4.根据权利要求1所述复合陶瓷纳米纤维膜的制备方法，其特征在于所述良溶剂为乙醇和丙酮，所述助剂为乙酸，乙醇、丙酮、乙酸的体积比为 9:10:6。
5.根据权利要求1所述复合陶瓷纳米纤维膜的制备方法，其特征在于所述微流体气喷纺丝装置的金属针头与接收器之间的距离为30-50 cm，液体流速为0.5-4 mL/h，气压0.2-3MPa的条件下，采用卷对卷方式收集所得纤维膜，其中转速为100-300 rpm，环境温度25 ℃，湿度不超过30-50wt.%。
6.根据权利要求5所述复合陶瓷纳米纤维膜的制备方法，其特征在于采用金属针头为不锈钢工业实验加长针，7号22G针头。
7.根据权利要求1所述复合陶瓷纳米纤维膜的制备方法，其特征在于所述无纺布的克重量为60 g。
8.权利要求1~7任一所述制备方法制得的复合陶瓷纳米纤维膜。
9.权利要求8所述复合陶瓷纳米纤维膜在制备空气过滤及个人防护产品中的应用。
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