ABSTRACT
A resorcinol-formaldehyde precursor was synthesized to fabricate the CO2 selective Carbon Molecular Sieve Membranes (CMSMs) developed in this study. The degree of polymerization (DP) was analyzed via Gel Permeation Chromatography (GPC) and its effect on the CO2/N2 perm-selectivity and CO2 permeance was investigated. The membrane that was polymerized at 80 °C (named R80) was selected as the best performing CMSM after a preliminary test. The post treatment with oxidative atmosphere was performed to increase the CO2 permeance and CO2/N2 perm-selectivity on membrane R80. The gas permeation results and Pore Size Distribution (PSD) measurements via perm-porometry resulted in selecting the membrane with an 80 °C polymerization temperature, 100 min of post treatment in 6 bar pressure and 120 °C with an oxygen concentration of 10% (named R80T100) as the optimum for enhancing the performance of CMSMs. The 3D laser confocal microscopy results confirmed the reduction in the surface roughness in post treatment on CMSMs and the optimum timing of 100 min in the treatment. CMSM R80T100 exhibiting CO2/N2 ideal selectivity of 194 at 100 °C with a CO2 permeability of 4718 barrier was performed higher than Robeson's upper bound limit for polymeric membranes and also the other CMSMs fabricated in this work.
ABSTRACT
Hydrogen permeation performance of palladium membranes supported on porous alpha-alumina and yttria-stabilized zirconia (YSZ) was studied at 300-850 degrees C. The hydrogen permeation flux across the palladium-alpha-alumina membrane decreased markedly during permeation tests conducted at >600 degrees C. The SEM and XPS studies of the post-test membrane revealed the presence of aluminium in the palladium layer. Such migration of aluminium was not observed by heating the palladium-alpha-alumina membrane under an argon atmosphere, indicating that hydrogen is responsible for this phenomenon. Hydrogen-induced strong metal-support interaction might be related to this considerable loss of the hydrogen flux. Reduction of alumina to Al(0) by active hydrogen at the membrane-support interface and subsequent migration of Al(0) into the palladium layer represents the most plausible mechanism for the aluminium diffusion. Actually, Al(0) that migrated into the palladium membrane layer generated less hydrogen-permeable palladium-aluminium alloy or inter-metallic compound phase. In contrast, no such strong interaction was found between the YSZ support and the palladium membrane. This composite membrane exhibited a steady permeation of hydrogen at 650 degrees C for 336 h. Having a remarkably high reduction potential, Y(III) is unlikely to be reduced to Y(0), although Zr(IV) has a comparable reduction potential to that of Al(III). A binary phase diagram shows a liquid alloy phase present for the Pd/Al couple at temperatures greater than 615 degrees C (eutectic point), while an inter-metallic compound or liquid alloy phase in the Pd-Zr binary system is not apparent at temperatures less than 750 degrees C. Consequently, inter-diffusion of zirconium with palladium did not occur during operations at 650 degrees C.
Subject(s)
Aluminum Oxide/chemistry , Hot Temperature , Hydrogen/chemistry , Membranes, Artificial , Palladium/chemistry , Porosity , Surface Properties , Zirconium/chemistryABSTRACT
A Pb(2+) selective membrane filter was fabricated from the fibrous CeO(H(2)PO(4))(2).2H(2)O (CeP) crystals by blending with cellulose fiber. Enrichment of ppb level of Pb(2+) was achieved simply by filtration of aqueous sample solution through the membrane filter. Pb(2+) was strongly retained on the membrane filter by accommodation into the interlayer gallery of a CeP crystal. Visual detection of the enriched Pb(2+) was achieved by subsequent color signaling as PbS deposit upon treatment of the membrane filter with 3% Na(2)S solution. The analytical procedure and sample treatment conditions were optimized with respect to pH of the sample solution, filtration rate and masking of interfering ions. Detection of 20 ppb of Pb(2+) was not interfered by the presence of 1000-fold of Ca(2+), Mg(2+), and up to 100-fold of Fe(3+)and Cu(2+) by masking with 1 x 10(-3) mol dm(-3) of iminodiacetic acid (IDA). Most anions including phosphate (20 000 times) did not interfere with the determination of Pb(2+). The present simple method was applied to the determination of Pb(2+) in real samples like mine valley water.