Pretreatment Influence on Hexane Permeability in Nanofiltration and ReverseOsmosis Commercial Polymeric MembranesKatia Rezzadori, Frederico M. Penha, Mariane C. Proner, Lara Fogaça, José C. C. Petrus,Marco Di Luccio*Departamento de Engenharia Química e de Alimentos, Universidade Federal de SantaCatarina, UFSC, Florianópolis, SC, 88040-900.e-mail: katia.rezzadori@gmail.com; *diluccio@enq.ufsc.brMembrane technology application in non-aqueous systems is not yet fully established, although itspotential for technological innovations in the food, chemical and pharmaceutical industry isrecognized [1]. The development of this technological alternative is related to the chemical stabilityof the membranes, since the exposition of these to organic solvents can cause physicochemicaland/or morphological changes on the membranes, affecting process performance. Studies indicatethat pre-treatment of polymer membranes, by immersion in organic solvents, can ensure themembrane’s contact with the solvent and modification of the selective surface, providing bettersolvent permeation and increasing the performance of the membrane [2].In this context, the aim of this study was to define a pretreatment for commercial polymericmembranes and to characterize these membranes, before and after the pretreatment, usingdifferent techniques. Two reverse osmosis (RO) membranes (BW30 and ORAK, BW30 e ORAK –rejections of 99,5 e 99 % to NaCl, respectively) and two nanofiltration (NF) membranes (NF270 –rejection of 97 % to MgSO 4 and NP030 rejection of 80-97% to Na 2 SO 4 ) were characterized by contactangle, FTIR (Fourier Transform Infrared Spectroscopy) and SEM (Scanning Electronic Microscopy). Themembrane conditioning was studied using distinct solvents (n-hexane, ethanol, n-propanol, isopropanoland n-butanol) in intervals of 2, 8, 12, and 24 hours. After the pretreatment, the n-hexaneflux was measured on each pressure (0-35 bar), at room temperature. A resistance test on n-hexanewas performed for 8 hours at 15 bar for the NF and 20 bar for the RO membranes.The conditioning with ethanol enabled higher hexane fluxes in the membranes ORAK, NF270 andBW30, while NP030 did not presented increases in permeability after the different conditionings. Theconditioning time has no significant effect (p > 0.05) on the process. Thus, a pretreatment for 2 hourswas chosen for further essays. An increase in the contact angle after the conditioning of themembranes was detected, which reflects changes in hydrophilicity of the surface. The FTIR spectraindicated the presence of polyamide and polysulfone of the membranes ORAK, BW30 and NF270.The membrane NP030 showed consecutive and sharp peaks of sulfone. After hexane permeation, adecrease in FTIR transmittance was noticed, which suggest the occurrence of swelling. SEM analysisdid not show any visible changes in membrane structure, except for the NF270 membrane, whichpresented pore compaction, probably due to applied pressure or to the solvent’s action.The results obtained in this work with commercial membranes of RO and NF, normally used inaqueous solutions separations, indicate that these membranes can be used in separation of nonaqueousmixtures without structural degradation, measurable with the techniques applied in thepreliminary tests.[1] S. Darvishmanesh, J. Degrève, B. Van Der Bruggen (2010), Ind. Eng. Chem. Res., 49, 9330-9338.[2] M.S. Araki, C.M. Coutinho, L.A.G. Gonçalves, L.A Viotto (2010), Sep. Purif. Technol., 71, 13-21.Acknowledgements: CAPES and CNPq
Effect of Dense CO 2 on Polymeric Commercial MembranesKatia Rezzadori, Josamaique G. Veneral, Lucas Pires, J. Vladimir Oliveira, José C. C. Petrus,Marco Di Luccio*Departamento de Engenharia Química e de Alimentos, Universidade Federal de SantaCatarina – UFSC – Florianópolis/SC - 88040-900.e-mail: katia.rezzadori@gmail.com; *diluccio@enq.ufsc.brCoupling supercritical CO 2 (SC-CO 2 ) extraction with membrane separation can lead to energy savings.Also, when pressurized fluids are considered for oil extraction, membrane separation could beprofitably used for minimizing the need of solvent recompression [1]. However, high pressureconditions may cause physicochemical and morphological changes in polymeric membranes, whichcan negatively affect membrane performance [2]. Moreover, since most of the information oncommercial membranes is provided by manufacturers, further investigation on their structure wouldbe beneficial for the selection of proper membranes, especially for processes involving non-aqueoussolvents, as SC-CO 2 .In this context, the aim of the present work was to study the behavior of two commercialmembranes, one reverse osmosis (RO) membrane (BW30 – rejections of 99 % to NaCl) and onenanofiltration (NF) membrane (NP030 rejection of 80-97% to Na 2 SO 4 ) upon static exposure toSC-CO 2 . The static process was carried out with dense CO 2 in two subcritical and two supercriticalconditions (80 bar and 100 bar/20°C; 100 bar and 200 bar/ 80°C) for 8 hours. The performance wasinvestigated based on changes in physicochemical and morphological properties. These propertieswere studied using contact angle, ATR-FTIR (Fourier Transform Infrared Spectroscopy) and SEM(Scanning Electronic Microscopy).Dense CO 2 exposure caused an increase in contact angle, which was higher in elevated pressures,indicating changes in membrane hydrophilicity. The FTIR spectra indicated the presence of polyamideand polysulfone, proving the thin film composite formation of the membrane BW30. The membraneNP030 showed consecutive and sharp peaks of sulfone. After dense CO 2 permeation, a decrease inFTIR transmittance was noticed, which suggests the occurrence of swelling. After contact with denseCO 2 , membrane BW30 showed structural changes on the active layer, while the membrane NP030remained unchanged.The results obtained in this work suggest that the commercial RO and NF membranes can be appliedin the permeation of dense CO 2 , with small changes in their properties, which did not causestructural degradation, measurable with the techniques applied in these preliminary tests.[1] C.B. Sprícigo, A. Bolzan, R.A.F. Machado, L.H.C. Carlson, J.C.C. Petrus (2001), J. Membr. Sci., 188, 173-178.[2] O. Akin, F. Temelli (2011), J. Supercrit. Fluids, 60, 81-88.Acknowledgements: CAPES and CNPq
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