膜科学与技术

中空纤维微滤膜孔径检测方法研究

作者：张艳萍，潘献辉，王旭亮，关毅鹏，张召才

单位：国家海洋局天津海水淡化与综合利用研究所，天津 300192

关键词：微滤膜；孔径；泡点压力法；压汞法；氮气吸附法

出版年,卷(期):页码： 2013,33(3):97-102

摘要：

孔径是微滤膜最为重要的表征参数之一，直接影响到微滤膜的分离性能。选用聚偏氟乙烯（PVDF）和聚丙烯（PP）材质的中空纤维微滤膜，研究并优化了泡点压力法测定微滤膜最大孔径的检测条件。以乙醇作为润湿剂，在20 °C、浸润时间30 min的最佳实验条件下，该方法测定PVDF和PP中空纤维微滤膜最大孔径的相对标准偏差分别为5.4%和8.8%。使用泡点压力法、压汞法和氮气吸附法测定四种不同材质的中空纤维微滤膜孔径特征，结果表明，泡点压力法测得的最大孔径和压汞法测得的平均孔径存在显著的线性相关性，氮气吸附法不适用于微滤膜孔径的测定。

Pore size is one of the most important characterization parameter, which directly affects the membrane separation performance. Bubble-point method for analysis of maximum pore diameter of hollow fiber microfiltration membrane was investigated in this study. With polyvinylidene fluoride (PVDF) and polypropylene (PP) microfiltration membrane as the representative examples, the detection conditions were optimized. Optimum bubble-point method was carried out at a temperature of 20 °C for 30 min by using ethanol as the soaking liquid. The relative standard deviations of maximum pore diameter were 5.4% and 8.8% for PVDF and PP microfiltration membrane, respectively. Pore sizes of four hollow fiber microfiltration membranes were determined by bubble-point, mercury porosimetry, and gas adsorption methods, respectively. The results showed that the maximum pore diameters obtained by bubble-point method were strongly correlated with the average pore diameters obtained by mercury porosimetry method. Gas adsorption method was not suitable for the pore size analysis of microfiltration membranes.

张艳萍（1983- ），女，山东淄博人，博士，工程师，从事海水利用膜产品检测技术研究。E-mail: zhangyanping_001@163.com

参考文献：

[1]Hernández A, Calvo J I, Prádanos P, et al. Pore size distributions in microporous membranes. A critical analysis of the bubble point extended method[J]. J Membr Sci, 1996, 112: 1-12.
[2]宫美乐，袁国梁. 我国微孔滤膜研究现状与发展[J]. 膜科学与技术，2003，23（4）：186-189.
[3]吕晓龙. 超滤膜孔径及其分布的测定方法 I. 常用测定方法讨论[J]. 水处理技术，1995，21（3）：137-141.
[4]齐秀聪，王金泉. 多孔滤膜的三种孔径分布及其关联[J]. 膜科学与技术，1993，13（3）：65-68.
[5]吕晓龙，马世虎. 一种多孔分离膜孔径及其分布的测定方法[J]. 天津工业大学学报，2005，24（2）：6-8，15.
[6]Prádanos P, Rodriguez M L, Calvo J I, et al. Structural characterization of an UF membrane by gas adsorption-desorption and AFM measurements[J]. J Membr Sci, 1996, 117: 291-302.
[7]Wyart Y, Georges G, Deumié C, et al. Membrane characterization by microscopic methods: multiscale structure[J]. J Membr Sci, 2008, 315: 82-92.
[8]Ziel R, Haus A, Tulke A. Quantification of the pore size distribution (porosity profiles) in microfiltration membranes by SEM, TEM and computer image analysis[J]. J Membr Sci, 2008, 323: 241-246.
[9]Reingruber H, Zankel A, Mayrhofer C, et al. Quantitative characterization of microfiltration membranes by 3D reconstruction[J]. J Membr Sci, 2011, 372: 66-74.
[10]Calvo J I, Hernández A, Prádanos P, et al. Pore size distributions in microporous membranes. II. Bulk characterization of track-etched filters by air porometry and mercury porosimetry[J]. J Colloid Interface Sci, 1995, 176: 467-478.
[11]Yu J, Hu X J, Huang Y. A modification of the bubble-point method to determine the pore-mouth size distribution of porous materials[J]. Sep and Purif Technol, 2012, 70: 314-319.
[12]Arkhangelsky E, Duek A, Gitis V. Maximal pore size in UF membranes[J]. J Membr Sci, 2012, 394-495: 89-97.
[13]Reichelt G. Bubble point measurements on large areas of microporous membranes[J]. J Membr Sci, 1991, 60: 253-259.
[14]Bechhold H, Schlesinger M, Silbereisen K, et al. Pore diameters of untrafilters[J]. Kolloid Z., 1931, 55:172.
[15]Nunes S P, Peinemann K V. Ultrafiltration membranes from PVDF/PMMA blends[J]. J Membr Sci, 1992, 77: 25-35.
[16]American Society for Testing and Materials. ASTM E1294-1999, Standard test method for pore size characteristics of membrane filters using automated liquid porosimeter[S]. United States: ASTM International, 1999.
[17]American Society for Testing and Materials. ASTM F316-03(2011), Standard test methods for pore size characteristics of membrane filters by bubble point and mean flow pore test[S]. United States: ASTM International, 2011.
[18]国家海洋局. HY/T 051-1999，中空纤维微孔滤膜测试方法[S]. 北京：中国标准出版社，1999.
[19]Castaing J B, Massé A, Pontié M, et al. Investigating submerged ultrafiltration (UF) and microfiltration (MF) membranes for seawater pre-treatment dedicated to total removal of undesirable micro-algae[J]. Desalination, 2010, 253: 71-77.
[20]陈悦，李东旭. 压汞法测定孔结构的误差分析[J]. 硅酸盐通报，2006，25（4）：198-207.
[21]严继民，张启元. 吸附与凝聚[M]. 北京：科学出版社，1979: 101-108.

服务与反馈：

【文章下载】【加入收藏】

《膜科学与技术》编辑部地址：北京市朝阳区北三环东路19号蓝星大厦邮政编码：100029 电话：010-64426130/64433466 传真：010-80485372邮箱：mkxyjs@163.com