For H2 separation by Pd-based composite membranes, the pore mouth size distribution of the porous support immediately affects the quality of the deposited layer, including continuity and defect/pinhole formation. However, there is a lack of convenient and effective methods for characterization of pore mouth size of porous supports as well as of defect distribution of dense Pd-based composite membranes. Here we introduce a novel method by modifying conventional liquid–liquid displacement porometry. When the pore tunnels are filled with Liquid B and the outer surface is occupied by Liquid A, the reopening of the pore mouth depends on the pressure of Liquid B and the interfacial tension at the position of the pore mouth, from which the pore mouth size can be determined according to the Young–Laplace equation. Our experimental tests using this method with model samples show promising results, which are well supported by those obtained using FESEM (fild emission scanning electron microscope), AFM (atomic force microscope), and conventional liquid–liquid displacement porometry. This novel method can provide useful information for not only surface coatings on porous substrates but also for modification of dense membrane defects; thus, broad utilizations of this technique can be expected in future study.
Water condensation is a possible cause of membrane wetting in the operation of membrane contactors, especially under high-temperature conditions. In this study, water condensation in pores of polytetrafluoroethylene (PTFE) hollow fiber membranes was investigated during high-pressure CO2 absorption around 70 °C. It was found that the liquid accumulation rate in the treated gas knock-out drum was constant during continuous operation for 24 h when all experimental conditions were fixed, indicating a stable degree of membrane wetting. However, as the operating parameters were changed, the equilibrium vapor pressure of water within membrane pores could change, which may result in a condensation-conducive environment. Water condensation in membrane pores was detected and proven indirectly through the increase in liquid accumulation rate in the treated gas knock-out drum. The Hagen–Poiseuille equation was used to correlate the liquid accumulation rate with the degree of membrane wetting. The degree of membrane wetting increased significantly from 1.8 × 10−15 m3 to 3.9 × 10−15 m3 when the feed gas flow rate was reduced from 1.45 kg/h to 0.40 kg/h in this study due to water condensation in membrane pores. The results of this study provide insights into potential operational limitations of membrane contactor for CO2 absorption under high-temperature conditions.