Browsing by Author "Anunziata , Oscar Alfredo"

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Aniline adsorption and polymerization over gallium modified mesoporous material.
(Univesidsad Tecnológica Nacional., 2018) Martínez , María Laura; Rivoira , Lorena Paola; Beltramone, Andrea Raquel; Anunziata , Oscar Alfredo; Anunziata , Oscar Alfredo; Rivoira , Lorena Paola
In this work we study aniline polymerization over a mesoporous Ga-SBA-3 synthesized in our laboratory. In order to modify the intrinsic acidity of the mesoporous material gallium was incorporated into the structure by post synthesis wet impregnation method using gallium nitrate. Structural and textural characterization of the materials was performed by X-ray diffraction (XRD), ICP and EDX analysis, N2 adsorption-desorption and BET area analysis, FTIR and scanning electron microscopy (SEM). The catalytic material presented a ratio Si/Ga=32. Aniline is a weak organic base and an amphiprotic compound, so it can accept or donate protons. The polyaniline (PANI) exists in diverse ways presenting different chemical and physical properties. The protonated polyaniline feature the conductivity of a semiconductor material, over 100 S/cm. Toward achieve aniline adsorption, the solid gallium silicate was exposed to aniline vapours. The aniline adsorption was studied by infrared spectroscopy and the results obtained were evaluated so as to been able to polymerize it over the mesoporous material generating a unique polyaniline-host composite with new properties. Those polyaniline/hosts composites obtained by a polymerization in-situ technique were characterized by infrared spectroscopy (FTIR) and X-ray diffraction (XRD) analysis. Comparing to previous results FTIR analysis of the polyaniline/Ga SBA-3 composite (PANI/Ga-SBA-3) showed characteristics bands attributed to the quinoidal stretching (N=Q=N) and C-C stretching of the benzene ring. The low angle XRD analysis showed that the mesoporous structure was maintained in spite of the gallium incorporation. The absence of PANI peaks and G2O3 in the wide angle XRD pattern confirms that the polyaniline is adsorbed over the gallium silicate mesoporous surface and the gallium is well dispersed over the support.
Controlled drug release system: cyclophosphamide delivery contained in LP-SBA-15 functionalized with terbutylamine.
(Univesidsad Tecnológica Nacional., 2023) Cussa, jorgelina; Juárez , Juliana María; Gómez Costa, Marcos Bruno; Anunziata , Oscar Alfredo; Anunziata , Oscar Alfredo; Juárez , Juliana María
Controlled drug administration systems can keep the level of drugs in specific locations in the organism with low toxicity and above the optimal level. We suggest the LP-SBA15 material as a auspicious new host for drug delivery systems because of its low toxicity high biocompatibility and in vivo biodegradability. LP-SBA-15 materials were synthesized and functionalized using 0-15-30% of tert-butylamine (TBA) and used as effective drug delivery systems. The anticancer drug Cyclophosphamide (CP) is an alkylating compound which is a phosphoramide derivative and is habitually used in autoimmune diseases. Reactive oxygen species production has been related to the mechanism of CP-induced cell death or tumor cell killing. The activated metabolites of CP are released in both healthy and tumor tissues and destroy the cellular DNA and proteins as well as mitochondrial and lysosomal membranes. CP was loaded into the nanomaterial of the transporters and characterized by XRD, FTIR, TGA, TEM and texture, determining the adsorption capacity and its release. The release of the drug was studied for each material by simulating the physiological conditions and submerging the composite, at 37 °C with constant stirring, in a HCl solution (0.1 M) for the first two hours and in Buffer solution pH = 7 the following hours to simulate the conditions of the organism. Release experiment were conducted to determine the requisite efficacy of treatment. The study was performed by UV-Vis spectrophotometry to evaluate the amount of CP released. The mechanism of drug release from the LP-SBA-15 matrix was evaluated by adjusting the experimental data, being the Ritger-Peppas. The promising results we obtained for the controlled release of the drug in a controlled manner using the new material, reaching a quick initial release rate and maintaining a constant rate at high moments, allow us to keep the concentration of the drug in the therapeutic efficacy range, applying it to a great extent to the treatment of diseases that require a rapid response. Lastly, it was suggested that the LP-SBA-15 nanomaterial functionalized with 15% TBA was the most desirable system due to they had adequate amounts of both drug loading and release.
Controlled Release of Haloperidol from a novel SWCNT Nano composite coated with ZnO nanocrystals.
(Univesidsad Tecnológica Nacional., 2023) Anunziata , Oscar Alfredo; Cussa , jorgelina; Martínez , María Laura; Martínez , María Laura; Cussa , jorgelina
Starting from the physicochemical knowledge of the host properties of the na noscale systems would be applied to drug dosage [1,2]. We propose NM synthesis strategies that offer the necessary characteristics for these processes. First, we study the physicochemistry of the anchoring sites of the respective hosts (chemical bonds with reversible or irreversible adsorption) or physisorption (straightforward interactions). Then, whether to design carbon based nanomaterials (CNM), or nano engineered materials, containing the respective active sites (deposited or generated nanospecies), capable of interacting with the aforementioned hosts such as: redox sites, proton acceptor sites, electron donor-acceptor sites, to allow HOMO-LUMO chemical interactions that satisfy the needs of the process to be studied. The nanostructures that allow free diffusions and reversible adsorptions, dosage of molecules with applications in nanokinetics, etc., and determination of critical molecular sizes, calculated using experimental methods, and methods such as density functional theory and semiempirical methods, to avoid steric hindrances between molecules and 100 80 40 60 8 12 16 20 Experimental data Weibull Ritger-Peppas Higuchi Drug Released , % mol/w Time (h) 4 20 nanomaterials whether 2D or 3D, designing NMs with large surface area, physical, ther mal and chemical stability, and pore size, and adequate pore size. Advancing in this sense, this work studies the usage of: Haloperidol Release from ZnO nanocrystal Coated SWCNT, with 30nm of wide and 5 um of long, which by the effect of the interaction between the host and drug molecules and by diffusion through the porosity, leads to a substantial contribution to controlled drug release. The reduction in the dose and frequency of administration, possible improvement in the selectivity of the pharmacological activity, and a prolonged therapeutic effect. CNT prepared by sol gel method (using the same technique describe by us, [3]), but at different pH and long range of pristine mesoporous carbons material calcination, to obtain SWCNTs. The posterior deposition of ZnO, was obtained, employing ZnNO3, activated under N2 flow at 500ºC; offering adequate LUMO of Zn (the hybridized MO) for Haloperidol interactions. Haloperidol competitively blocks postsynaptic dopamine (D2) receptors in the meso limbic system of the brain, thereby eliminat ing dopamine neurotransmission and leading to antidelusionary and antihallucinagenic effects. Specifically, the dose of Haloperidol (potent antipsychotic drug), indicates that its release follows the so called "power law" or Weibull model, based on the results we obtained in our laboratory
Experimental Desing Optimization of the tetralin Hydrogenation over Ir-Pt-SBA-15.
(Univesidsad Tecnológica Nacional, 2016) Vallés , Verónica Alejandra; Ledesma, Brenda Cecilia; Rivoira , Lorena Paola; Cussa , jorgelina; Anunziata , Oscar Alfredo; Beltramone, Andrea Raquel; Anunziata , Oscar Alfredo; Cussa , jorgelina; Rivoira , Lorena Paola; Ledesma, Brenda
Experiment design-response surface methodology (RSM) is used in this work to model and optimize two responses in the hydrogenation of tetralin to decalin using bimetallic Ir–Pt-SBA-15 catalyst. In this study, we analyze the influence of the nature of the catalyst (metal molar fraction and metal loading), the catalyst/substrate ratio and the temperature of the reaction as factors for the design. The responses analyzed were conversion at 3 h and at 5 h of reaction time. The response surfaces were obtained with the Box–Behnken design, finding the best combination between the reaction parameters that allowed optimizing the process. By applying the statistic methodology, the higher levels of the two objective functions were obtained employing the catalyst with 1 wt.% of iridium and 0.7–0.8 wt.% of platinum; the optimal ratio between mass of catalyst and mole of tetralin was 17–19 g/mol and temperature between 200 and 220 ◦C.
Experimental desing optimization of the tetralin hydrogenation over Ir-Pt-SBA-15.
(Univesidsad Tecnológica Nacional., 2015) Vallés , Verónica Alejandra; Ledesma , Brenda Cecilia; Rivoira , Lorena Paola; Cussa , jorgelina; Anunziata , Oscar Alfredo; Beltramone, Andrea Raquel; Anunziata , Oscar Alfredo; Cussa , jorgelina; Rivoira , Lorena Paola; Ledesma , Brenda Cecilia
Experiment design-response surface methodology (RSM) is used in this work to model and optimize two responses in the hydrogenation of tetralin to decalin using bimetallic Ir–Pt-SBA-15 catalyst. In this study, we analyze the influence of the nature of the catalyst (metal molar fraction and metal loading), the catalyst/substrate ratio and the temperature of the reaction as factors for the design. The responses analyzed were conversion at 3 h and at 5 h of reaction time. The response surfaces were obtained with the Box– Behnken design, finding the best combination between the reaction parameters that allowed optimizing the process. By applying the statistic methodology, the higher levels of the two objective functions were obtained employing the catalyst with 1 wt.% of iridium and 0.7–0.8 wt.% of platinum; the optimal ratio between mass of catalyst and mole of tetralin was 17–19 g/mol and temperature between 200 and 220 ◦C
Experimental Desing Optimization of the tetralin Hydrogenation over Pt-Ir/SBA-15.
(Univesidsad Tecnológica Nacional, 2015) Vallés , Verónica Alejandra; Ledesma , Brenda Cecilia; Rivoira , Lorena Paola; Cussa , jorgelina; Anunziata , Oscar Alfredo; Beltramone, Andrea Raquel; Anunziata , Oscar Alfredo; Cussa , jorgelina; Rivoira , Lorena Paola; Ledesma , Brenda
The oil refining industry has a difficult challenge to meet the increasingly stringent regula tions on environmental issues. Contaminants such as sulfur, nitrogen, fused ring aromatic compounds or metals are the principal to remove to achieve "green" fuels. The hydrotreating (HDT) is one of the processes most used in the refinery to remove these contaminants. To optimize the gas oil hydrotreater, it is crucial to understand the aromatic hydrogenation reac tion chemistry occurring in the gas oil hydrotreater. To find alternative processes, it is neces sary to develop new and more active catalysts to replace the current ones. Bimetallic Pt–Pd catalysts have received considerable attention, because they show high actvity in a variety of catalytic applications [1,2]. From a fundamental point of view, exploring bimetallic catalysts also allows better understanding of mechanisms and variables involved in the catalytic reac tions. The features of the catalysts here studied are going to be correlated with their catalytic performance in the hydrogenation of tetralin. The final goal is to find the optimal proportion of each metal in order to be more active and the best reaction conditions. The statistical expe riments design is the process of planning an experiment to obtain appropriate data that can be analyzed by statistical methods, to produce concrete and valid conclusions [3]. One of the main advantages in the response curve is to visualize the response for all levels of the experi mental factors Experiment design response surface methodology (RSM) is used in this work to model and to optimize the process
Experimental Desing Optimization of the tetralin Hydrogenation over Pt-Ir/SBA-15.
(Univesidsad Tecnológica Nacional., 2015) Vallés , Verónica Alejandra; Ledesma , Brenda Cecilia; Rivoira , Lorena Paola; Cussa , jorgelina; Anunziata , Oscar Alfredo; Beltramone, Andrea Raquel; Anunziata , Oscar Alfredo; Cussa , jorgelina; Rivoira , Lorena Paola; Ledesma , Brenda Cecilia
he oil refining industry has a difficult challenge to meet the increasingly stringent regula tions on environmental issues. Contaminants such as sulfur, nitrogen, fused ring aromatic compounds or metals are the principal to remove to achieve "green" fuels. The hydrotreating (HDT) is one of the processes most used in the refinery to remove these contaminants. To optimize the gas oil hydrotreater, it is crucial to understand the aromatic hydrogenation reac tion chemistry occurring in the gas oil hydrotreater. To find alternative processes, it is neces sary to develop new and more active catalysts to replace the current ones. Bimetallic Pt–Pd catalysts have received considerable attention, because they show high actvity in a variety of catalytic applications [1,2]. From a fundamental point of view, exploring bimetallic catalysts also allows better understanding of mechanisms and variables involved in the catalytic reac tions. The features of the catalysts here studied are going to be correlated with their catalytic performance in the hydrogenation of tetralin. The final goal is to find the optimal proportion of each metal in order to be more active and the best reaction conditions. The statistical expe riments design is the process of planning an experiment to obtain appropriate data that can be analyzed by statistical methods, to produce concrete and valid conclusions [3]. One of the main advantages in the response curve is to visualize the response for all levels of the experi mental factors Experiment design response surface methodology (RSM) is used in this work to model and to optimize the process.
HaP/LP-SBA15 Nanocomposite for efficient removal of fluoride from contaminated water.
(Univesidsad Tecnológica Nacional., 2020) López, Claudia; Cussa, jorgelina; Anunziata , Oscar Alfredo; Anunziata , Oscar Alfredo; Cussa, jorgelina
Hydroxyapatite (HaP) composites and highly ordered large pore mesoporous silica, such as LP-SBA 15 (Large Pore-SBA-15), were developed, characterized by XRD, BET, FTIR, and HRTEM, applied to fluoride removal from contaminated water. The proposed procedure to prepare HaP/LP-SBA-15 was successful, which acts as supports to anchor the HaP crystals, in nanometer-scale (<12 nm), with higher fluoride retention from contaminated water. The free OH- groups of HaP nanocrystals, inside the host, permitted fluoride retention with high capacity. The fluoride holding activity was over 3 orders of magnitude higher than pure HaP.
HaP/SBA-3 Nanostructured Composite to Remove Fluoride Effectively from Contaminated Water.
(Univesidsad Tecnológica Nacional., 2021) Cussa , jorgelina; López, Claudia; Anunziata , Oscar Alfredo; Anunziata , Oscar Alfredo; López, Claudia
Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and textural properties, were successfully applied to remove fluoride from contaminated water. The proposed procedure to prepare HaP/SBA-3 was successful, which acts as supports to anchor the HaP crystals, in nanometer-scale (<2nm), with higher fluoride retention from contaminated water. The free OH- groups of HaP nanocrystals, within the host, facilitated the high-performance fluoride trapping. The fluoride retention activity was much higher than that of pure HaP and the composites HaP/SBA-15 and HaP/MCM-41. Keywords: F- retention; Contaminated water; HaP/SBA-3; Nanocomposites
HDN of indole over Ir-modified Ti-SBA-15.
(Univesidsad Tecnológica Nacional., 2015) Ledesma , Brenda Cecilia; Anunziata , Oscar Alfredo; Beltramone, Andrea Raquel
The hydrodenitrogenation of indole has been studied over a series of Ti-modified SBA-15 supports and their respective Ir-catalysts. Ti-SBA-15 was synthesized using sol-gel method and Ti was added during the synthesis using Tetraethyl Orthotitanate. Iridium was added by wetness impregnation. The acidity of Ti-SBA-15 was modified adding F or Al in order to improve the catalytic activity. The catalysts pre pared were extensively characterized by X-ray diffraction (XRD), N2 adsorption isotherms, UV–vis-DRS, Raman spectroscopy, 27 Al-MAS-NMR spectroscopy, XPS, TEM-EDS, Py-FTIR, H2-Chemisorption and TPR. UV–vis-DRS and Raman spectroscopy confirmed that Ti was incorporated in tetrahedral coordination in the framework of the SBA-15. The analysis showed that the mesoporous structure was maintained after F or Al incorporation. 27 Al-MAS-NMR spectroscopy indicated that aluminum was incorporated mainly in Td positions. The results showed that Ti incorporation helps to reduce significantly the size of iridium crystallites and improves its dispersion considerably. Ir/Ti-SBA-15 modified with Al, with Bronsted acid ity, was the most active catalyst for indole HDN, in mild conditions in a Batch reactor. The experimental data for indole hydrodenitrogenation was quantitatively represented by a Langmuir–Hinshelwood type rate equation
Hidrodenitrogenación de Indol utilizandocatalizadores de Ir soportado sobre SBA-15 modificada con Ti.
(Univesidsad Tecnológica Nacional., 2016) Ledesma , Brenda Cecilia; Vallés , Verónica Alejandra; Anunziata , Oscar Alfredo; Beltramone , Andrea Raquel; Anunziata , Oscar Alfredo; Vallés , Verónica Alejandra
La hidrodenitrogenación de indol se estudió utilizando una serie de catalizadores de Ir soportado sobre SBA 15 modificada con Ti. El mesoporoso modificado Ti-SBA-15 se sintetizó usando el método sol-gel. El iridio fue incorporado mediante la técnica de impregnación húmeda incipiente. Con el fin de mejorar la actividad catalítica se modificó la acidez del material mesoporoso añadiendo F o Al. Los catalizadores fueron caracterizados por difracción de rayos X (XRD), isotermas de adsorción de N2, UV-Vis-DRS, espectroscopía Raman, espectroscopía 27Al-MAS-RMN, XPS, TEM, Py-FTIR y TPR. Los análisis confirman que el Ti fue incorporado en coordinación tetraédrica dentro de la SBA-15 y que la estructura mesoporosa se mantuvo después de la incorporación de F o Al. La espectroscopía27Al-MAS-RMN indica que el aluminio se incorporó principalmente en posicion tetraédrica. Los resultados mostraron que la incorporación del Ti ayuda a reducir significativamente el tamaño de los clusters de Iridio y mejora considerablemente su dispersión. El catalizador Ir-Ti-SBA-15, modificado con Al, fue el catalizador más activo para la hidrodenitrogenación de indol, en condiciones suaves en un reactor discontinuo. Los datos experimentales para la hidrodenitrogenación de indol fueron cuantitativamente representados por una ecuación de velocidad del tipo Langmuir-Hinshelwood. Palabras claves: hidrodenitrogenación, titanio, mesoporoso, clusters de Iridio, cinética
Hidrogenación de tetralin sobre Ir-Pt-SBA-15. Parte 1: Síntesis, caracterizacíon y actividad catalítica.
(Univesidsad Tecnológica Nacional, 2015) Vallés , Verónica Alejandra; Ledesma, Brenda Cecilia; Rivoira , Lorena Paola; Cussa , jorgelina; Anunziata , Oscar Alfredo; Beltramone , Andrea Raquel; Anunziata , Oscar Alfredo; Cussa , jorgelina; Rivoira , Lorena Paola
Se estudia aquí la hidrogenación de tetralin a decalin utilizando un catalizador bimetálico Ir-Pt SBA-15. En esta Parte se describe la síntesis de los catalizadores, la preparación de la matriz de SBA 15 y el método de co-impregnacion mediante el cual se incorporaron los metales en diferentes proporciones y carga total metalica. Los catalizadores fueron caracterizados por XRD, TEM, análisis fisicoquimicos, XPS, SEM y EDX. En la Parte 2 de este trabajo se analizará la influencia de la naturaleza del catalizador, la relación catalizador sustrato y la temperatura de reacción como factores de un Diseño de Experimentos para optimizar el proceso.
Hidrogenación de tetralin sobre Ir-Pt-SBA-15. Parte 2: Optimización por Diseño de Experimentos.
(Univesidsad Tecnológica Nacional, 2015) Vallés , Verónica Alejandra; Ledesma, Brenda Cecilia; Rivoira , Lorena Paola; Cussa , jorgelina; Anunziata , Oscar Alfredo; Beltramone , Andrea Raquel; Anunziata , Oscar Alfredo; Cussa , jorgelina; Rivoira , Lorena Paola; Ledesma, Brenda
La Metodología Diseño de Experimentos - Superficie de Respuesta – se utiliza en este trabajo para modelar y optimizar 2 respuestas en la reacción de hidrogenación de tetralin a decalin usando un catalizador bimetálico Ir-Pt-SBA-15. En este estudio se analizó la influencia de la naturaleza del catalizador, la relación catalizador/sustrato y la temperatura de reacción como factores del diseño. Las respuestas analizadas fueron conversión a 3 y 5 horas Las Superficies de Respuesta fueron obtenidas mediante un diseño Box-Behnken a fin de encontrar la mejor combinación de los distintos parámetros para optimizar el proceso. La metodología estadística aplicada indica que las conversiones más altas de ambas respuestas, a 3 y 5 horas, se obtienen trabajando en el siguiente rango: Catalizador: 1% Ir y 0.7-0.9 %(p/p) Pt; Relación: 17-19 g cat/ mol TL y Temperatura: 200-220°C.
Hidrogenación de tetralin utilizando un catalizador bifuncional de iridio/platino-SBA-15.
(Univesidsad Tecnológica Nacional, 2014) Vallés , Verónica Alejandra; Ledesma, Brenda Cecilia; Rivoira, Lorena Paola; Cussa , jorgelina; Martínez , María Laura; Anunziata , Oscar Alfredo; Beltramone, Andrea Raquel; Anunziata , Oscar Alfredo; Martínez , María; Cussa , jorgelina; Ledesma, Brenda
Los catalizadores bimetálicos de Pt–Pd han recibido considerable atención debido a que demuestran tener una alta actividad en una amplia variedad de aplicaciones catalíticas (1). Con alta actividad, selectividad y estabilidad, comparada con catalizadores monometálicos de Pt y Pd. Por ejemplo, catalizadores bimetálicos Pt-Pd muestran tener mayor resistencia frente a envenenamientos en comparación con catalizadores de Pt (2-4). Las características estudiadas del catalizador serán correlacionadas con su performance catalítica en la hidrogenación del tetralin. El objetivo final es encontrar la proporción óptima de cada uno de los metales de forma de lograr la mayor actividad en dicho proceso.
Hydrodenitrogenation of over Ir supporteD Ti-SBA-15 modified with F AND AI.
(Univesidsad Tecnológica Nacional., 2015) Ledesma , Brenda Cecilia; Vallés , Verónica Alejandra; Rivoira , Lorena Paola; Balangero, Gerardo Simón; Anunziata , Oscar Alfredo; Beltramone, Andrea Raquel; Anunziata , Oscar Alfredo; Rivoira , Lorena Paola; Vallés , Verónica Alejandra
The hydrodenitrogenation of Indole has been studied over a series of Ti-modified SBA 15 supports and their respective Ir-catalysts. Ti-SBA-15 was synthesized using sol-gel method and Ti was added during the synthesis using TEOT as Ti source. Ti was incorporated into the framework replacing the Si atoms in the mesoporous structure. Ir/Ti-SBA-15 with and without F and/or Al were prepared to improve the catalytic activity. F and Al have been incorporated by wetness impregnation method. The effect of the incorporation of F and Al in the mesoporous structure was tested in the hydrodenitrogenation reaction of indole. The catalysts were extensively characterized by X-ray diffraction (XRD), N2 adsorption isotherms, TEM, FTIR and UV-vis-DRS and Raman spectroscopy. The low angle X-ray analysis showed for all the materials intensive reflection, characteristic of SBA-15 structure. The mesoporous structure was maintained after F and Al incorporation. The results showed that Ti incorporation reduces significantly the cluster size and improves considerably the Ir cluster dispersion. The catalytic activity of Ir/Ti-SBA-15 modified with F and Al, with higher acidity, avoided the irreversible adsorption of indole. The catalytic activity was studied in a 4563 Parr reactor, at 250°C, 15 atm of pressure of hydrogen and 360 rpm. The catalysts synthesized had good activity measured in hydrodenitrogenation of indole at mild conditions. The preliminary results show these materials as promising catalysts for HDN reactions.
Hydrogenation of tetralin in presence of nitrogen using a noble-bimetallic couple over a Ti-modified SBA-15.
(Univesidsad Tecnológica Nacional., 2017) Vallés , Verónica Alejandra; Ledesma , Brenda Cecilia; Rivoira , Lorena Paola; Cussa , jorgelina; Anunziata , Oscar Alfredo; Beltramone, Andrea Raquel; Cussa , jorgelina; Rivoira , Lorena Paola; Ledesma , Brenda Cecilia
The increased attention paid to catalytic hydrogenation in the oil refining industry is due in part to legislation regarding the maximum contents of sulfur, aromatic compounds, and alkenes in traffic fuels. Aromatics in diesel increase the particle emissions in exhaust gases and they have the further effect of lowering the fuel quality. Many factors such as the catalysts, process parameters, feedstock source and quality, reactivities of sulfur compounds, inhibition effects of H2S, nitrogen compounds and aromatics present in the feed, etc. can have significant influences on the degree of hydrogenation of diesel feeds1,2. Recently, studies have been reviewed and the investigations have also been extended to noble metals3 . In our previous investigations with bimetallic catalysts4 , we had very good results preparing the catalysts by co impregnation of the relevant metals on the SBA-15 mesoporous matrix. These studies showed high activity, selectivity and stability as well also greater resistance to poisons compared to monometallic catalysts. In this contribution titanium is incorporated in tetrahedral position replacing silicon in the mesoporous framework. We expect that Ti incorporation improve the dispersion of the bimetallic clusters. In the present work three compounds tetralin, indole and quinoline were used as models for the compounds in diesel. The model compounds were hydrogenated both separately and as mixtures in order to study the inhibition effect.
Hydrogenation of tetralin in presence of nitrogen using a noble-bimetallic couple over a Ti-modified SBA-15.
(Univesidsad Tecnológica Nacional., 2016) Vallés , Verónica Alejandra; Ledesma , Brenda Cecilia; Pecchi, Gina; Anunziata , Oscar Alfredo; Beltramone , Andrea Raquel; Anunziata , Oscar Alfredo; Ledesma , Brenda Cecilia
Monometallic Pt- and bimetallic Pt-Ir-modified Ti-SBA-15 were used in the hydrogenation of tetralin to decalin in the presence of 150 ppm of N as quinoline and indole at 250 ◦C and 15 atm of pressure of hydrogen, using a Parr reactor. The catalyst was synthesized using sol-gel method and Ti was added during the synthesis using Tetraethyl Orthotitanate. Pt/Ir was added by wetness impregnation. The catalysts prepared were extensively characterized by X-ray diffraction (XRD), N2 adsorption isotherms, UV–vis DRS, Raman spectroscopy, XPS, TEM-EDS and TPR. UV–vis-DRS and Raman spectroscopy confirmed that Ti was incorporated in tetrahedral coordination in the framework of the SBA-15. The analysis showed that the mesoporous structure was maintained after metal incorporation and Ti incorporation helps to reduce significantly the size of the metals clusters and improves its dispersion considerably. Pt-Ir/Ti-SBA 15 was the most active catalyst. The experimental data were quantitatively represented by a modified Langmuir-Hinshelwood type rate equation. The preliminary results show these materials as a promising catalyst for HDT reactions.
Ir-Pt/SBA-15 applied in the optimization of tetralin hydrogenation.
(Univesidsad Tecnológica Nacional, 2015) Vallés , Verónica Alejandra; Ledesma , Brenda Cecilia; Rivoira, Lorena Paola; Cussa , jorgelina; Anunziata , Oscar Alfredo; Beltramone, Andrea Raquel; Cussa , jorgelina; Ledesma , Brenda
Bimetallic catalysts have received considerable attention for hydrotreating (HDT) because they show high activity. The features of the catalysts here studied are going to be correlated with their catalytic performance in the hydrogenation of tetralin at mild conditions. The final goal is to find the optimal proportion of each metal in order to be more active and the best reaction conditions (temperature and amount of catalyst). The statistical experiments design is the process of planning an experiment to obtain appropriate data that can be analyzed by statistical methods, to produce concrete and valid conclusions. One of the main advantages in the response curve is to visualize the response for all levels of the experimental factors Experiment design response surface methodology (RSM) is used in this work to model and to optimize the process. Platinum and Iridium nanoparticles were incorporated into SBA-15 support by the wet co-impregnation method. Ir content was set as 1wt. % and Pt was varied from 0 to 1wt. %. The catalysts were characterized by XRD, BET, XPS, TEM, ICP and TPR. XRD profiles are characteristic of the two-dimensional p6mm hexagonal mesostructure with d100 spacing of 10.16 nm; where the d100 spacing upon Ir and Pt incorporation were quite similar to pristine SBA-15. The TEM images and XPS demonstrate that the metal particles were mainly present inside the porous and XPS and TPR corroborated the reduced state of the metals. The catalytic activity was measured in a 4563Parr reactor at 15 atm of hydrogen and 360 rpm. Feed consisted in 50 mL of tetralin in Dodecane, the amount of tetralin is set according to the ratio of catalyst mass/mass reagent corresponding to each reaction. The application of this methodology allows a better understanding of the influence of the different factors: content of metal on catalyst (A), relationship: mass of catalyst/reagent mass (B) and reaction temperature (C), on two responses: conversion at 3 h and at 5 h of reaction time. These factors were carefully selected taking account the influence of the parameters in the reaction. The design was analyzed by Statgraphics and Statistica Soft. We found that, the variable Catalyst has the best influence over the Conversion at the 95.0% confidence level, according to the Pareto.
Ir-Pt/SBA-15 applied in the optimization of tetralin hydrogenation.
(Univesidsad Tecnológica Nacional., 2015) Vallés , Verónica Alejandra; Ledesma , Brenda Cecilia; Rivoira , Lorena Paola; Cussa , jorgelina; Anunziata , Oscar Alfredo; Beltramone , Andrea Raquel; Anunziata , Oscar Alfredo; Anunziata; Cussa , jorgelina; Rivoira , Lorena Paola; Ledesma , Brenda Cecilia
Bimetallic catalysts have received considerable attention for hydrotreating (HDT) because they show high activity. The features of the catalysts here studied are going to be correlated with their catalytic performance in the hydrogenation of tetralin at mild conditions. The final goal is to find the optimal proportion of each metal in order to be more active and the best reaction conditions (temperature and amount of catalyst). The statistical experiments design is the process of planning an experiment to obtain appropriate data that can be analyzed by statistical methods, to produce concrete and valid conclusions. One of the main advantages in the response curve is to visualize the response for all levels of the experimental factors Experiment design response surface methodology (RSM) is used in this work to model and to optimize the process. Platinum and Iridium nanoparticles were incorporated into SBA-15 support by the wet co-impregnation method. Ir content was set as 1wt. % and Pt was varied from 0 to 1wt. %. The catalysts were characterized by XRD, BET, XPS, TEM, ICP and TPR. XRD profiles are characteristic of the two-dimensional p6mm hexagonal mesostructure with d100 spacing of 10.16 nm; where the d100 spacing upon Ir and Pt incorporation were quite similar to pristine SBA-15. The TEM images and XPS demonstrate that the metal particles were mainly present inside the porous and XPS and TPR corroborated the reduced state of the metals. The catalytic activity was measured in a 4563Parr reactor at 15 atm of hydrogen and 360 rpm. Feed consisted in 50 mL of tetralin in Dodecane, the amount of tetralin is set according to the ratio of catalyst mass/mass reagent corresponding to each reaction. The application of this methodology allows a better understanding of the influence of the different factors: content of metal on catalyst (A), relationship: mass of catalyst/reagent mass (B) and reaction temperature (C), on two responses: conversion at 3 h and at 5 h of reaction time. These factors were carefully selected taking account the influence of the parameters in the reaction. The design was analyzed by Statgraphics and Statistica Soft. We found that, the variable Catalyst has the best influence over the Conversion at the 95.0% confidence level, according to the Pareto.
Ketorolac-tromethamine contained in SBA-15 host as a drug release system,
(Univesidsad Tecnológica Nacional, 2017) Cussa , jorgelina; Prados, Antonella; Juárez , Juliana María; Gómez Costa , Marcos Bruno; Anunziata , Oscar Alfredo; Anunziata , Oscar Alfredo; Juárez , Juliana María
Drug delivery is an emerging field mainly focused on targeting drugs. The goal of this targeted delivery is to transport an amount of drugs to desirable sites (such as tumors and diseased tissues) while minimizing unwanted side effects of the drugs on other tissues[1]. Controlled drug delivery systems can achieve precise spatial and temporal delivery of therapeutic agents to the target site[2]. The ordered mesoporous silica SBA-15 has been applied in studies of ketorolac tromethamine adsorption and release. The SBA-15 materials with hexagonal and regular structure were obtained using a triblock copolymer Pluronic P123 as a template and TEOS as a silica source[3]. Ketorolac tromethamine was adsorbed into SBA-15 silica nanochannels using ethanol as solvent. The physicochemical and textural properties of SBA-15 and ketorolac tromethamine/SBA-15 were characterized by X-ray diffraction, thermogravimetric analysis, transmission electron microscopy, Fourier transform infrared spectroscopy and BET surface studies. Drug release was evaluated by soaking the loaded silica mesoporous material into a solution of HCl (0.1N) at initial time (0 - 2 h) and buffer pH 7 at high times at 37 ºC under continuous stirring. Oral commercial Keto tablets (Dolten®) and Keto solution (Keto power) were study for the contrast. Release studies were performed in order to evaluate the required therapeutic efficacy. In this work, we have shown a promising drug storage material for the effective encapsulation and controlled release of KETO, achieving the required therapeutic efficacy. SBA-15/KETO shows characteristic bands of both, drug materials and the inorganic framework. This indicates that KETO was adsorbed into SBA-15 channel surface without affecting the chemical structure or composition of KETO. The study also demonstrates the storage capacity and release properties of SBA-15 containing KETO. The release of KETO contained in SBA-15 can offer significant improve in controlled drug release and enhance a good analgesia effect.

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