Facultad Regional Córdoba
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Item Direct synthesis of ordered mesoporous carbon applied in hydrogen storage(Springer Science+Business Media, 2018) Juárez, Juliana María; Gómez Costa , Marcos Bruno; Anunziata, Oscar AlfredoIn this work, we present a direct, novel and low cost method for the preparation of an ordered mesoporous carbon (OMC). OMC was successfully synthesized by the carbonization of the silica/triblock copolymer/sucrose composite in the presence of sulfuric acid. The resulting material was characterized by XRD, N2 sorption analysis and TEM techniques. The novel synthesis technique improved significantly the H2 storage properties (3.78 wt%) compared with that of CMK-3 synthesized using the nanocasting strategy (2.2 wt%) at 77 K and 10 bar.Item Nanoclusters of iron oxice included in CMK-3mesoporous carbon use as hydrogen storage material(Materials Research Society, 2019) Juárez, Juliana María; Venosta, Lisandro F.; Gómez Costa , Marcos Bruno; Anunziata, Oscar AlfredoIn this work we studied the influence of the incorporation of iron oxide nanoparticles inside the channels of the nanostructured mesoporous carbon CMK-3. This research includes synthesis of the mesoporous silicate and synthesis of CMK-3 by nanocasting strategy, incorporation of the iron oxide nanoclusters by wetness impregnation, characterization of these nanomaterials by XRD, N2 adsorption, XPS, and TEM, and study of the improvement in hydrogen adsorption. This material is promising in hydrogen adsorption and storage application for energy harvesting. According to XRD studies, the incorporation of oxide nanoclusters does not compromise the overall structure of the mesoporous carbon CMK-3. In the wide angle region it has been found typical reflections of iron oxide corresponding to the magnetite phase (Fe2+Fe3+ 2 O4). The modified sample Fe-CMK-3 reveal a reduced specific surface area and smaller pore diameter compared to pristine CMK-3 which involves the formation of magnetite nanoparticles within the mesoporous channels of CMK-3. TEM images of Fe-CMK-3 presents metallic oxide nanoparticles well dispersed. The incorporation of iron oxide nanoparticles improved significantly the H2 storage behavior (4.45% wt at 77K and 10 bar) compared to its respective support (CMK-3). Magnetite nanoclusters increased the capacity of hydrogen adsorption in pristine materials. Supposing that weakly orbital interactions occur between H2 and the metal nanocluster, physisorption is the main interaction, all cases have the potential to uptake H2 weakly as physisorption process and the last interaction achieves sufficiently strong energies to store more hydrogen to reach the level adsorption in Fe-CMK-3. In addition, no hydrogen chemisorption was detected. The materials synthesized are promising in hydrogen uptake by weak link forces (physisorption).Item Sustainable utilization of orange peels waste for preparation of activated carbon: Synthesis, Characterization and Hydrogen storage application(2022) Juárez, Juliana María; Ledesma, Brenda Cecilia; Beltramone, Andrea Raquel; Gómez Costa, Marcos Bruno; Anunziata, Oscar AlfredoThe recovery and reuse of orange peel waste (OP) is a sustainable strategy in a circular economy. In this research, OP was used as the raw material for the preparation of a novel carbonaceous nanomaterial to be used in the adsorption of hydrogen as an alternative in the use of green hydrogen. Activated carbons were synthesized from orange peel using different synthesis conditions. The activation of the carbon was carried out by means of a chemical process with phosphoric acid as activating agent, varying the the activating agent/precursor ratio, and the contact time between them. The activating agent used is a solution of phosphoric acid (50 wt %) in different weight ratios of acid/precursor of 3:1 or 6:1, with resting time of 24 hours. The best support was obtained using a carbonization time of 1 h, a carbonization temperature of 470oC, 6:1 precursor/acid ratio and 24 hours of resting time. According XRD analysis all samples present amorphous structure of activated carbons with BET surface areas of 1000 to 1400 m2 /g. With the activated carbons obtained with the best structure and texture, the adsorption of hydrogen and the effects on their meso / microporosity were studied. Said material significantly improved H2 storage behaviour compared to CMK-3 type nanostructured carbon (3.1% by weight at -196,15 oC and 10 bar). The synthesized material shows promise in absorbing hydrogen by weak binding forces (physisorption)Item Nanostructured mesoporous materials modified with nickel for alternative energy and environmental applications(2017) Carraro, Paola; Benzaquén, Tamara; Oliva, Marcos Iván; Eimer, Griselda AlejandraNickel modified mesoporous silicas with MCM-41 structure were prepared by direct hydrothermal synthesis with Si/Ni molar ratio = 20 and 60 in the synthesis gel and increased days of synthesis from 0 to 7 days. Various characterization techniques including XRD, N2 adsorption at 77 K, TEM, SEM, ICP-OES, UV-Vis DRS, TPR, FT-IR and adsorption of pyridine coupled to FT-IR spectroscopy were conducted in order to study the textural, structural and chemical properties of the materials. The effect of Ni loading on the textural, structural, adsorbing and catalytic properties of the materials was investigated. The samples presented well-ordered hexagonal structure; however, the structural ordering appears to be slightly decreased when increasing the hydrothermal treatment days. A hydrothermal treatment time of 3 days appears optimum to obtain a good ordering and Ni species incorporation into the structure. Longer hydrothermal treatment times decreased the degree of ordering structural, giving account for the restructuration and reorganization of the network. Thus, combined characterization results indicate that the synthesis time has an important influence on the textural, structural and chemical properties of the nickel modified mesoporous silica. Hydrogen adsorption capacity of Ni-containing mesoporous materials modified with nickel was measured at 77 K up to 10 bar. The results demonstrated that the sample with a molar ratio Si/Ni = 60 and without hydrothermal treatment presented the highest hydrogen adsorption, probably due to their SBET and the presence of highly dispersed nickel species on the support . Besides, the mesostructured nickel-containing catalysts have been successfully proved in Atrazine degradation by the heterogeneous photo-Fenton process in aqueous solutions. As a result of this, the sample with nickel loading of 1.6 wt. % (Ni(60)0) allowed to reach values of the pollutant degradation about of 60.3 %. In conclusion, the nickel incorporation into the mesoporous framework presents the option of developing materials versatile and efficient for to be employed in energy and environmental applications.Item Studies of hydrogen adsorption on ni-modified mcm-41 mesoporous materials.(2016) Carraro, Paola; García Blanco, Andrés; Soria, Federico; Lener, Germán; Sapag, Karim; Oliva, Marcos Iván; Eimer, Griselda AlejandraMCM-41 mesoporous materials were prepared modified with different Ni contents, as promising materials for hydrogen storage. The final materials were reduced for studying the metallic nickel effect. The Ni/MCM-41 samples were characterized for different experimental techniques such as TPR, XRD and N2 adsorption-desorption. The hydrogen storage capacity of the materials was evaluated at 77 K and room temperature, and at low and high-pressure conditions respectively. In this study, we focused on the role of dispersed nickel as a way of promoting the interaction with hydrogen as an alternative to improve hydrogen storage materials. The results obtained show that the amount of hydrogen stored was highly enhanced by the dispersion of small amounts of Ni nanoparticles both at 77 and 298 K, indicating that these materials could be used for hydrogen storage in cryogenic and room temperature conditions.