Browsing by Author "Fernandez, Ekain"
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Item Catalytic membrane reactor for the production of biofuels(2016-06-15) Liuzzi, Dalia; Pérez-Alonso, Francisco José; Fierro, José Luis G.; Rojas, Sergio; Van Wijk, Frank L.; Roghair, Ivo; Van Sint Annaland, Martin; Fernandez, Ekain; Viviente, Jose Luis; Tanaka, D. A.Pacheco; TECNOLOGÍAS DE HIDRÓGENO; TECNOLOGÍA DE MEMBRANAS E INTENSIFICACIÓN DE PROCESOSThe H2-distributed feeding concept using Pd/Ag-based membranes and an Ru-based catalyst in a Packed Bed Membrane Reactor (H2-PBMR) for the synthesis of biofuels via the so-called Fischer-Tropsch Synthesis has been demonstrated. The most successful approach resulted when H2-poor syngas (H2/CO = 1) typically obtained from the gasification of biomass was fed directly through the reaction chamber, i.e., to the catalyst bed, whereas the H2 needed to reach the proper stoichiometry for the FTS (H2/CO = 2) was admitted, and properly distributed, into the catalyst bed through the Pd/Ag-based membrane by flowing H2/He mixtures at the retentate side of the membrane. Under the optimum reaction conditions, the CO conversion measured with the H2-distributed feeding concept is lower than that obtained in a conventional Packed Bed Reactor with H2/CO = 2 (37.9 vs 50.7%), but significantly higher than that obtained in a conventional reactor with H2/CO = 1 (14.1%). Remarkably, the productivity towards high-molecular hydrocarbons increases by almost 70% and the methane production decreases by one order of magnitude when using the H2-distributed feeding concept in a Packed Bed Membrane Reactor.Item Development of highly permeable ultra-thin Pd-based supported membranes(2016-12-01) Fernandez, Ekain; Sanchez-Garcia, Jose Angel; Melendez, Jon; Spallina, Vincenzo; van Sint Annaland, Martin; Gallucci, Fausto; Pacheco Tanaka, D. A.; Prema, Radha; TECNOLOGÍAS DE HIDRÓGENO; Tecnalia Research & Innovation; TECNOLOGÍA DE MEMBRANAS E INTENSIFICACIÓN DE PROCESOSThis paper reports the preparation and characterization of ultra-thin (∼1 μm thick) Pd-based supported membranes for hydrogen purification. Ultra-thin membranes have been prepared by a combination of PVD magnetron sputtering and electroless plating techniques. The membranes have been characterized for single gas and mix gas permeation at temperatures between 350 and 500 °C and they have shown to exhibit very high hydrogen fluxes combined with a good perm-selectivity (H2/N2 ≈ 500). These results have been compared with the performance of highly permeable membranes reported in the literature. The influence of the morphology of the deposited Pd-based layers on the membrane performance has been investigated and discussed.Item Development of thin Pd-Ag supported membranes for fluidized bed membrane reactors including WGS related gases(2015-03-02) Fernandez, Ekain; Helmi, Arash; Coenen, Kai; Melendez, Jon; Viviente, Jose Luis; Pacheco Tanaka, David Alfredo; Van Sint Annaland, Martin; Gallucci, Fausto; TECNOLOGÍAS DE HIDRÓGENO; Tecnalia Research & Innovation; TECNOLOGÍA DE MEMBRANAS E INTENSIFICACIÓN DE PROCESOSThis paper reports the preparation, characterization and stability tests of Pd-based thin membranes for fluidized bed membrane reactor applications. Various thin membranes have been prepared by simultaneous Pd-Ag electroless plating. A simple technique for sealing of the produced membranes is reported and discussed. The membranes have been characterized for single gas permeation, and afterwards used for permeation of mixtures of gases and under fluidization conditions. The membranes have shown very high permeation rates and perm-selectivity when used as permeators. When applied in fluidized bed reactors it has been found that the membranes are stable as long as no interaction between the fluidization catalyst and the membrane surface occurs. For some catalysts a strong chemical interaction between the catalyst and the membrane surface has been observed which caused a drastic decrease in the membrane flux.Item Fluidized Bed Membrane Reactors for Ultra Pure H2 Production - A Step forward towards Commercialization(2016-03-19) Helmi, Arash; Fernandez, Ekain; Melendez, Jon; Pacheco Tanaka, David A.; Gallucci, Fausto; van Sint Annaland, Martin; TECNOLOGÍAS DE HIDRÓGENO; Tecnalia Research & Innovation; TECNOLOGÍA DE MEMBRANAS E INTENSIFICACIÓN DE PROCESOSIn this research the performance of a fluidized bed membrane reactor for high temperature water gas shift and its long term stability was investigated to provide a proof-of-concept of the new system at lab scale. A demonstration unit with a capacity of 1 Nm3/h of ultra-pure H2 was designed, built and operated over 900 h of continuous work. Firstly, the performance of the membranes were investigated at different inlet gas compositions and at different temperatures and H2 partial pressure differences. The membranes showed very high H2 fluxes (3.89E 6 mol m 2 Pa 1 s 1 at 400 C and 1 atm pressure difference) with a H2/N2 ideal perm-selectivity (up to 21,000 when integrating five membranes in the module) beyond the DOE 2015 targets. Monitoring the performance of the membranes and the reactor confirmed a very stable performance of the unit for continuous high temperature water gas shift under bubbling fluidization conditions. Several experiments were carried out at different temperatures, pressures and various inlet compositions to determine the optimum operating window for the reactor. The obtained results showed high hydrogen recovery factors, and very low CO concentrations at the permeate side (in average <10 ppm), so that the produced hydrogen can be directly fed to a low temperature PEM fuel cell.Item Long-Term Stability of Thin-Film Pd-Based Supported Membranes(2019-02-01) Nooijer, Niek; Arratibel Plazaola, Alba; Meléndez Rey, Jon; Fernandez, Ekain; Pacheco Tanaka, David; Sint Annaland, Martin; Gallucci, Fausto; Tecnalia Research & Innovation; TECNOLOGÍA DE MEMBRANAS E INTENSIFICACIÓN DE PROCESOS; TECNOLOGÍAS DE HIDRÓGENOMembrane reactors have demonstrated a large potential for the production of hydrogen via reforming of different feedstocks in comparison with other reactor types. However, the long-term performance and stability of the applied membranes are extremely important for the possible industrial exploitation of these reactors. This study investigates the long-term stability of thin-film Pd-Ag membranes supported on porous Al2O3 supports. The stability of five similarly prepared membranes have been investigated for 2650 h, up to 600 °C and in fluidized bed conditions. Results show the importance and the contribution of the sealing of the membranes at temperatures up to 500 °C. At higher temperatures the membranes surface deformation results in pinhole formation and a consequent decrease in selectivity. Stable operation of the membranes in a fluidized bed is observed up to 450 °C, however, at higher temperatures the scouring action of the particles under fluidization causes significant deformation of the palladium surface resulting in a decreased selectivity.Item Morphology and N2 Permeance of Sputtered Pd-Ag Ultra-Thin Film Membranes(2016-02-10) Fernandez, Ekain; Sanchez-Garcia, Jose Angel; Viviente, J.L.; van Sint Annaland, Martin; Gallucci, Fausto; Pacheco Tanaka, David A.; Tecnalia Research & Innovation; TECNOLOGÍAS DE HIDRÓGENO; TECNOLOGÍA DE MEMBRANAS E INTENSIFICACIÓN DE PROCESOSThe influence of the temperature during the growth of Pd-Ag films by PVD magnetron sputtering onto polished silicon wafers was studied in order to avoid the effect of the support roughness on the layer growth. The surfaces of the Pd-Ag membrane films were analyzed by atomic force microscopy (AFM), and the results indicate an increase of the grain size from 120 to 250–270 nm and film surface roughness from 4–5 to 10–12 nm when increasing the temperature from around 360–510 K. After selecting the conditions for obtaining the smallest grain size onto silicon wafer, thin Pd-Ag (0.5–2-µm thick) films were deposited onto different types of porous supports to study the influence of the porous support, layer thickness and target power on the selective layer microstructure and membrane properties. The Pd-Ag layers deposited onto ZrO2 3-nm top layer supports (smallest pore size among all tested) present high N2 permeance in the order of 10−6 mol•m−2•s−1•Pa−1 at room temperature.Item Pd-Based Membranes for High Temperature Applications: Current Status(Austin Publishing Group, 2016-03-29) Gallucci, Fausto; Fernandez, Ekain; Medrano, Jose Antonio; Pacheco Tanaka, David A.; van Sint Annaland, MartinNot availableItem Preparation and characterization of metallic supported thin Pd–Ag membranes for hydrogen separation(2016-12-01) Fernandez, Ekain; Medrano, Jose Antonio; Melendez, Jon; Parco, Maria; Viviente, Jose Luis; van Sint Annaland, Martin; Gallucci, Fausto; Pacheco Tanaka, D. A.; TECNOLOGÍAS DE HIDRÓGENO; Tecnalia Research & Innovation; EXTREMAT; TECNOLOGÍA DE MEMBRANAS E INTENSIFICACIÓN DE PROCESOSThis paper reports the preparation and characterization of thin-film (4–5 μm thick) Pd–Ag metallic supported membranes for high temperature applications. Various thin film membranes have been prepared by depositing a ceramic interdiffusion barrier layer prior to the simultaneous Pd–Ag electroless plating deposition. Two deposition techniques for ceramic layers (made of zirconia and alumina) have been evaluated: Atmospheric Plasma Spraying and dip coating of a powder suspension. Initially, the prepared ceramic layers have been characterized for nitrogen permeation at room temperature and surface roughness for the selection of the appropriate type of ceramic layer. The most promising membranes have been tested at 400–600 °C for single gas permeation (H2 and N2), and have shown extremely high H2/N2 permselectivities (>200,000).