FRLP - I+D+i - CENTROS - CITEMA - TRABAJOS DE INVESTIGACIÓN
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Item Synthesis, characterization and swelling behavior of new pH-sensitive hydrogels derived from copolymers of 2-hydroxyethyl methacrylate and 2-(diisopropylamino) ethylmethacrylate(2012) Faccia, Paula; Amalvy, JavierThe aim of this work was to synthesize and to characterize new pH-sensitive hydrogels that can be used in the controlled release of drugs, useful for dermal treatments or ophthalmology’s therapies. Copolymers containing 2-hydroxyethyl methacrylate (HEMA) with different amounts of 2-(diisopropylamino)ethyl methacrylate (DPA) (10 and 30 wt %) and different amounts of cross- linker agent, ethylene glycol dimethacrylate (EGDMA) (1 and 3 wt %) were prepared by bulk photo-polymerization. The copolymers were fully characterized by using Fourier-transform infrared (FTIR) spectra, differential scanning calorimetry, thermogravimetric anal- ysis, UV–visible spectroscopy, and measuring water content and dynamic swelling degree. The results show that modifications in the amount of DPA and/or crosslinker in the hydrogel produce variations in the thermal properties. When adding of DPA, we observed an increase in the thermal stability and decomposition temperature, as well as a change in the mechanism of decomposition. Also a decrease in the glass transition temperature was observed with regard to the value for pure pHEMA, by the addition of DPA. The water content of the hydrogels depends on the DPA content and it is inversely proportional to both the pH value and the crosslinking degree. Pure poly-HEMA films did not show important changes over the pH range studied in this work. The dynamic swelling curves show the overshooting effect associated with the incorporation of DPA, the pH of the solution, and the crosslinking density. On the other hand, no important variations in the optical properties were observed. The synthesized hydrogels are useful as a drug delivery pH-sensitive matrix.Item Synthesis and swelling behavior of pH-responsive polyurethane poly(2-(diethylamino)ethyl methacrylate) hybrid materials(2013) Pardini, Francisco; Amalvy, JavierPolyurethane (PU)/poly[2-(diethylamino)ethyl methacrylate] hybrids, having a chemical bond between the PU and acrylic moieties and with different compositions, were prepared by the dispersion polymerization of 2-(diethylamino)ethyl methacrylate (DEA) in the presence of preformed PU chains with polymerizable terminal vinyl groups. The PU dispersion was synthesized accord- ing to a prepolymer mixing process by the polyaddition of isophorone diisocyanate, poly(propylene glycol), 2-hydroxyethyl methacry- late, and dimethylol propionic acid (DMPA). Then, it was dispersed in water by the prior neutralization of the carboxylic acid groups of DMPA with triethylamine, chain-extended with ethylenediamine. The effect of the DEA content on the swelling properties (water uptake and dynamic swelling degree) at different pHs and at 37�����C was determined. The samples were also characterized by Fourier transform infrared spectroscopy and modulated differential scanning calorimetry. The experimental results indicate a higher water uptake when the DEA content was increased on the hybrid materials and a significant change in the kinetics of swelling at pH 4 com- pared to those at pH 7. The water content of the hydrogels depended on the DEA content, and it was inversely proportional to the pH value. The pure PU film did not show important changes over the pH range examined in this study. The synthesized hybrids were useful as drug-delivery, pH-sensitive matrices.Item Preparation and evaluation of carbon supported catalysts for ethanol oxidation(Springer, 2013) Bonesi, Alejandro; Asteazaran, Mariano; Moreno, Mario; Bengio, Silvina; Zampieri, Guillermo; Triaca, Walter; Castro Luna, AnaSupported PtSnIr/C, PtSn/C, and IrSn/C catalysts with potential application in a direct alcohol fuel cell were prepared by chemical reduction employing Pechini methodology. The catalyst particles were characterized by high-resolution transmission electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy (XPS). Linear sweep voltammetry (LV), chronoamperometry, and electrochemical impedance spectroscopy (EIS) measurements were performed by using a glassy carbon working electrode covered with the catalyst in a 1 M ethanol+0.5 M H2SO4 solution at 60 °C. It was demonstrated through XPS that PtSnIr/C and IrSn/C contain both IrO2 and SnO2. LV and chronoamperometry show a better catalytic behavior for ethanol oxidation on PtSnIr/C in the low-potential region and the improvement is attributed to the presence of both Sn and Ir oxides. The EIS accurately established that PtSnIr/C improved ethanol oxidation at lower potentials than PtSn/C.Item Decay resistance and dimensional stability of Araucaria angustifolia using siloxanes synthesized by solegel process(Elsevier, 2013-05-16) Giúdice, Carlos Alberto; Alfieri, Paula; Canosa, GuadalupeSolid wood specimens of Araucaria angustifolia were impregnated with alkoxysilanes hydrolyzed and condensed “in situ” by the solegel process. Alkoxysilanes selected were aminopropyl methyldiethoxysilane and aminopropyl triethoxysilane; it was also used the aminopropyl methyldiethoxysilane/aminopropyl triethoxysilane mixture in 50/50 ratio w/w. The pH was adjusted to alkaline value for controlling kinetic of hydrolysis and condensation reactions. Impregnation process was carried out under controlled operating conditions to achieve different weight gains of the chemical modifier. Unmodified and modified wood specimens were exposed to brown rot (Polyporus meliae) and white rot (Coriolus versicolor) under laboratory conditions. The results indicate that the improved resistance to fungal exposure would be based on the wood chemical modification (the protection of cellulose caused by steric hindrance of hSieOeCellulose preventing the formation of enzymeesubstrate complex). Moreover, the results also would be based on the enhanced dimensional stability of the treated wood; the quoted high dimensional stability, which limits the growth of the spores, is supported in the hydrophobicity generated by both the decreasing of the amount of polar hydroxyl groups and the partial occupation of pores with polysiloxanes.Item Hybrid finishing coatings applied on laminar zinc primers(American Chemical Society, 2013-05-29) Giúdice, Carlos Alberto; Canosa, Guadalupe; Alfieri, PaulaHybrid finishing coatings were formulated with several film-forming materials and reinforcement fibers. In all cases, the same tri-pigmented epoxy-polyamide coating based on laminar zinc was used as primer. The results indicated that wellwetted fibers improved mechanical properties of finishing coating films, such as tensile strength, modulus of elasticity, hardness, adhesion, and impact resistance; on the other hand, elongation decreased according with type and level of reinforcement fibers selected. In addition, finishing coatings with semiconductive fibers displayed in salt spray (fog) apparatus, a high dissolution of metallic zinc of primer since these fibers would act as cathode in galvanic cells. According to IR spectrum analysis, chemical degradation was observed only in coatings with the binder susceptible to basic hydrolysis due to the action of hydroxyl ions formed on semiconductive fibers. Furthermore, nonconductive fibers included in finishing coatings displayed no changes in any film-forming material (even when alkyd resin was used) nor promoted excessive zinc dissolution of primer.Item Pinturas híbridas de terminación sobre fondos anticorrosivos de zinc modificados(Atipat, 2013-10-01) Giúdice, Carlos Alberto; Alfieri, Paula; Canosa, GuadalupeLas pinturas basadas en zinc metálico presentan una mayor eficiencia contra la corrosión en relación con otros recubrimientos. Sin embargo, éstas necesitan generalmente una pintura de terminación ya sea para conferirle al sistema un mejor acabado o bien para otorgarle una protección adecuada contra la acción del medio; en otros casos, la pintura de terminación también se aplica para conferirle dureza superficial (puentes de acero, estructuras metálicas portantes, etc.). En este trabajo se seleccionaron tres sistemas en lo referente al ligante; en todos los casos se empleó el mismo “primer” epoxi-poliamídico basado en zinc laminar mientras que para la capa de terminación se seleccionaron como ligantes una resina acrílica pura, una vinílica y una alquídica. En la formulación de estas pinturas, se emplearon fibras para conferirle elevada resistencia a la rotura y alto módulo de elasticidad a la película (grafito, nitruro de silicio, vidrio o cuarzo). Los resultados indican que en las estructuras híbridas con fibras semiconductoras se observó una elevada disolución del zinc ya que las citadas fibras actuarían como cátodos de la celda galvánica; también se constató que en el caso del ligante susceptible a la hidrólisis básica se produjo su degradación y la pérdida de propiedades de la películaItem Siloxanes synthesized in situ by solgel process for fire control in wood of Araucaria angustifolia(Elsevier, 2013-10-10) Giúdice, Carlos Alberto; Alfieri, Paula; Canosa, GuadalupePanels of Araucaria angustifolia were chemically modified with alkoxysilanes, hydrolyzed and condensed “in situ” by the sol–gel process. Alkoxysilanes selected were aminopropyl methyldiethoxysilane (A), aminopropyl triethoxysilane (B) and a mixture of both (C). Ethanol was used as solvent in 4/1 ethanol/ alkoxide molar ratio. The pH was adjusted to alkaline value for controlling the kinetic of hydrolysis– condensation reactions. Impregnation process was carried out at 45–50 1C in an autoclave, controlling the operating conditions for achieving different weight gains. Laboratory tests were carried out in Two-Foot Tunnel (flame spread index, panel consumption and smoke density) and in TGA detector (mass loss). The performance in laboratory tests can be explicated according the reactivity of the alkoxides. The results support the conclusion that the best fireproof efficiency was observed in woods treated with the alkoxide B, followed by those modified with the mixture C and the alkoxide A, in this order; the results also indicates that as weight gain increased the performance of impregnants against fireItem Dimensional stability, fire performance and decay resistance in wood impregnated with alkylalkoxysilanes(2013-11-20) Canosa, Guadalupe; Alfieri, Paula; Giúdice, Carlos AlbertoThe wood, very heterogeneous and complex material, changes its volume by water absorption or desorption causing swelling or shrinkage and also it can be degraded both by action of microorganisms and fire; the above-mentioned is a great inconvenient for most commercial uses. In this research, wood specimens of Pinus radiata were previously pretreated in a Soxhlet extractor for 2 hours with a solution of sodium hydroxide (activation of the cellulose) and then impregnated with alkylalkoxysilanes hydrolyzed and condensed "in situ" by the sol-gel process. Silanes selected were triethoxysilane, methyltriethoxysilane, n-propyltriethoxysilane, n-buthyltriethoxysilane and n-octhyltriethoxysilane. Impregnation process was carried out under controlled operating conditions to achieve similar weight gains of the chemical modifier. The pH was adjusted to alkaline value for controlling kinetic of hydrolysis and condensation reactions. Results indicated that dimensional stability increased with the increase of the length of the hydrocarbon chain of the alkoxydes, which would be based essentially on their enhanced hydrophobicity but without discarding the partial occupation of the pores by polymerized siloxanes and the interaction of alkoxides with cell wall components. In addition, wood specimens impregnated with mentioned alkylalkoxysilanes also showed an excellent fire performance and decay resistance.Item Preparation and characterization of graphite anodes for lithium ion batteries(The Electrochemical Society, 2014) Humana, Rita; Ortiz, Mariela; Thomas, Jorge; Real, Silvia; Sedlarikova, Marie; Vondrak, Jiri; Visintin, ArnaldoThe lithium-ion batteries are energy storage systems of high performance and low cost. They are employed in multiple portable devices and these require the use of increasingly smaller and lighter batteries with high energy and power density, fast charging and long service life. Moreover, these systems are promising for use in electric or hybrid vehicles. However, the lithium-ion battery still requires to improve the electrode materials properties, such as cost, energy density, cycle life, safety, and environmental compatibility. These batteries use carbon as anode material, usually synthetic graphite, because of its high coulombic efficiency and acceptable specific capacity for the formation of intercalation compounds (LiC6). In this paper the methodology used to prepare and characterize the reversible and irreversible capacity and, cyclic stability of graphite materials as anodes in lithium-ion batteries of commercial carbon and Sungite carbon, is presented. The results obtained using electrochemical techniques, are discussed.Item Surface, thermal, and mechanical properties of composites and nanocomposites of polyurethane PTFE nanoparticles(2014) Anbinder, Pablo; Peruzzo, Pablo; de Siervo, A.; Amalvy, JavierFilms from blends of polyurethane and nano-polytetrafluoroethylene aqueous dispersions (PU/nanoPTFE) were prepared, and the effect of the addition of different amounts of PTFE nanoparticles (50 nm) was studied. The changes in the superficial properties of the films were studied by means of XPS, ATR/FTIR, and contact angle measurements. SEM and TEM results are also included. The contact angle values confirm the surface hydrophobicity of com- posite films. Even though nanoparticles are present in the bulk, higher concentrations of particles appear at the surface in samples with lower nanoPTFE content (up to 10 wt%), as revealed by XPS. Higher amounts of nanoPTFE particles cause aggregation. The mechanical and thermal properties of composites are also discussed.Item Síntesis de nano catalizadores para celdas de combustible de metanol directo(Revista Tecnología y Ciencia UTN, 2014) Asteazaran, Mariano; Bonesi, Alejandro; Triaca, Walter; Castro Luna, AnaLas celdas de combustible de metano/ directo, DMFCs, permiten una conversión completa de la energía de la reacción química (CH)3OH(ac)+3/2 O2(g)=7CO2(g)+2H2O(l) en energía eléctrica. El platino es el catalizador más utilizado en las DMFCs. Para poder generar cantidades aceptables de corriente no se puede prescindir del uso de este metal como catalizador. Como la catálisis se manifiesta a nivel superficial, si se sintetizan nano partículas catalíticas soportadas sobre negro de carbón se obtendrá una gran área de reacción. El empleo de la nano tecnología y la combinación de Pt con otros metales aumenta la actividad electro catalítica y reduce el costo de las celdas de combustible. Se sintetizan y se determinan las actividades electro catalíticas de nano partículas en base platino como material de electrodo para el cátodo donde se lleva a cabo la reacción de reducción de oxígeno en la DMFC.Item Effect of antioxidant active films on the oxidation of soybean oil monitored by Fourier transform infrared spectroscopy(2014) Anbinder, Pablo; Peruzzo, Pablo; Martino, Miriam; Amalvy, JavierAn active film prepared from waterborne polyurethane incorporated with different concentrations of butylated hydroxytoluene (BHT) and a-tocopherol was developed, and the films’ antioxidant character- istics were studied using soybean oil as food model. The release behavior of additives from such films was studied using isooctane as a simulant fatty food. Antioxidant activity of the films into soybean oil at three experimental conditions was monitored by FTIR spectroscopy. Induction time and the kinetics of the oxi- dation process were followed using different bands of the FT-IR spectra. Films incorporated with 2 wt.% of BHT or a-tocopherol showed enough antioxidant activity to preclude oil oxidation during 60 days at 60 °C in the dark. The results showed that this type of active films could be used for food preservation as part of a packaging containing oils or oily related products.Item Adherence in a pavement rehabilitated with a polymeric grid used as interlayer(Elsevier, 2014-01-02) Delbono, Héctor Luis; Giúdice, Carlos AlbertoA polymeric grid was placed between layers of a pavement with the aim of preventing the reflection of cracks from the base material to the upper layer. Results explain why the usual faults that occur in rehabilitated pavements: (i) chemical modifications of geosynthetic polypropylene determined by FTIR lead to changes in its melting point; (ii) the discontinuity or continuity of the interface observed by SEM depends on the application temperature of the asphalt mix and (iii) the adherence obtained in laboratory tests correlates perfectly with the quoted chemical modifications of geosynthetic polypropylene and the structure of interface in multilayer pavements.Item Preparation and characterization of positive electrode of NiMH batteries with cobalt additives(Elsevier, 2014-02-18) Ortiz, Mariela; Real, Silvia; Castro, Élida BeatrizThe present paper shows the preparation and characterization of alkaline batteries cathodes formed by nickel hydroxide with the addition of cobalt. This additive was incorporated by two methods: on the electrode surface, using the electroless technique and by direct incorporation of cobalt powder in the active material. The electrochemical behavior of both nickel hydroxide electrodes was investigated and compared. The results indicate that active materials containing cobalt additive by the electroless technique exhibit an improvement on the electrochemical performance.Item Effect of cobalt electroless deposition on nickel hydroxide electrodes(Elsevier, 2014-02-21) Ortiz, Mariela; Castro, Élida Beatriz; Real, SilviaThe effects of cobalt additive on the positive electrode surface of nickel alkaline batteries are investigated. Electrode surface modifications by electroless cobalt deposits were made at different immersion times. The performance of nickel hydroxide electrodes was studied by optical techniques, such as scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX) and electrochemical methods as cyclic voltammetry, charge discharge curves and electrochemical impedance spectroscopy (EIS). According to these results, electroless cobalt deposits obtained with 5 min of immersion time in the electroless-bath exhibit a better electrode performance.Item High solids, one coat paints based on aliphatic epoxi resin siloxanes for steel protection(Elsevier, 2014-05-01) Canosa, Guadalupe; Alfieri, Paula; Giúdice, Carlos AlbertoThis research involved the design of high-solids, one-coat paints for the protection of metal structures with low maintenance requirements. The main paint components were: (i) an aliphatic epoxy resin cured with an aminosilane and chemically modified with alkoxysilanes as film-forming material, and (ii) rutile titanium dioxide as opaque pigment, a polysilicate strontium and zinc as corrosion inhibitor and, a synthetic calcium silicate and barites as extenders. Some paints displayed excellent performance in salt spray apparatus (degree of rusting) and in 100% relative humidity cabinet(degree of blistering). Results indicate that as the aliphatic epoxy resin/alkoxide ratio increased, the degree of rusting improved while the degree of blistering worsened, in total agreement with film permeability. In addition, binders based on dimethyldiethoxysilane, methyltriethoxysilane and tetraethoxysilane, in that order, displayed an improved corrosion performance and a decreased blistering resistance. The reactivity of alkoxides and the chemical interaction with the metal substrate supports the obtained results. Initial gloss and gloss and color retention improved as the alkoxide level increased; no significative differences were registered when the alkoxide type variable was considered. In summary, the use of alkoxides as modifiers of an aliphatic epoxy resin allowed the formulation of hybrid paints with high anticorrosive and weathering resistance performance. The more suitable hybrid organic–inoganic paint must be selected according to the requirements of each structure in serviceItem Pinturas basadas en resina epoxi alifática curada con alcoxisilanos para la protección de sustratos metálicos(Atipat, 2014-05-01) Canosa, GuadalupeLa presente investigación involucró el diseño de pinturas de altos sólidos, de aplicación en una sola capa, destinadas a la protección de construcciones metálicas con necesidades de mínimo mantenimiento y alta durabilidad; la composición se basó en una resina epoxi alifática curada con un aminosilano y modificada químicamente con alcoxisilanos como material co-formador de película y en dioxide de titanio rutilo como pigmento oipaco, un polisilicato de estroncio y zinc como pigmento inhibidor y, silicato de calcio sintético y barita como extendedores. Los resultados indican que las pinturas diseñadas presentaron una excelente resistencia a la corrosión metálica en cámara de niebla salina y a la formación de ampollas en cabina de humedad relativa 100%, incluso sustancialmente superiores a aquéllas formuladas con los convencionales diglicidil éter del bisfenol A; esta mejorada performance de las pinturas orgánica-inorgánicas se debería a la formación de uniones covalentes con el sustrato del tipo ≡Si-O-Metal. Finalmente, las pinturas híbridas diseñadas presentaron también una elevada retención de color y brillo. Por lo tanto, las estructuras expuestas en ambientes no muy agresivos no requerirían una capa de pintura de terminación (el nivel creciente de polisiloxano en el ligante conduce a un incremento de la resistencia a la intemperie) como en el caso de las epoxi convencionales.Item Estudio de diferentes condiciones de síntesis para la obtención de zeolita NaA a partir de cenizas volantes(Investigación Joven, 2015) Monzón, Jorge; Pereyra, Andrea; Basaldella, ElenaEn este trabajo se propuso zeolitizar una ceniza volante industrial a través de un proceso hidrotermal. Para ello, se probó mejorar su reactividad sometiéndola a un pretratamiento de calcinación en presencia de compuestos fundentes como Na2CO3, NaOH y ClNa. Fue también pretratada por molienda. Una vez activada, se preparó una mezcla de reacción agregándole cantidades especificadas de Na2O y Al2O3. Luego de la reacción en condiciones de temperatura controlada, se analizó la conversión en fases zeolíticas obtenidas a diferentes tiempos de reacción. La reactividad de diversas mezclas se evaluó en términos de su conversión en zeolita NaA a través de DRX, SEM y EDX. Se observó que la aplicación de un pretratamiento adecuado de calcinación y fusión alcalina, condujo a un aumento de la reactividad de las cenizas.Item Searching for suitable catalysts for a passive direct methanol fuel cell cathode(Elsevier, 2015) Asteazaran, Mariano; Cespedes, German; Moreno, Mario; Bengio, Silvina; Castro Luna, AnaTrimetallic PtMRu/C cathode catalysts with M ¼ Co or Fe obtained by an impregnation procedure using ethylene glycol and NaBH4 as reducing agent, with suitable activity for the oxygen reduction reaction (ORR) and improved tolerance to methanol, have been physically characterized by HRTEM, EDS and XPS. The examined nanoparticles have a small particle size and are well spread on the carbon support. Pt is mainly found as Pt(0) and Co, Fe and Ru are mostly oxidized. To study their durability and performance for ORR and methanol tolerance over time, the catalysts were subjected to an electrochemical accelerated stress test (AST), consisting in cycling the potential 2000 times. Polarization curves for ORR with and without methanol were recorded. After the AST the trimetallic PtMRu/C catalysts are able to keep their performance for ORR in the presence of methanol.Item Research on methanol tolerant catalysts for the oxygen reduction reaction(Springer, 2015) Asteazaran, Mariano; Cespedes, German; Bengio, Silvina; Moreno, Mario; Triaca, Walter; Castro Luna, AnaDirect methanol fuel cells (DMFCs) generate electricity in a clean and efficient way, so they are a valuable alternative to traditional environmentally harmful technologies. Portable power sources are one of the applications of passive DMFCs. One of the requirements in these devices is the use of high alcohol concentration. Methanol permeation across the polymer electrolyte membrane (methanol crossover) causes a loss of fuel cell efficiency as the oxygen reduction reaction (ORR) and the methanol oxidation reaction (MOR) occur simultaneously at the cathode. To develop methanol-tolerant catalysts with suitable activity, different PtM/C and PtMRu/C combinations with M = Co or Fe were prepared by a modified impregnation method. The synthesized catalysts were studied to determine the role of the components in enhancing the ORR and simultaneously discouraging the MOR. The materials were characterized by TEM, XPS and EDS. Well-distributed particles for all the catalysts were shown by TEM. XPS spectra revealed that the method produces a great amount of metallic Pt. The electrochemical characterization was carried out by linear sweep voltammetry and cyclic voltammetry, in a three-electrode electrochemical cell with a glassy carbon rotating disk electrode covered with a thin catalytic layer and a Nafion film as the working electrode. Binary and ternary catalysts have a good activity for the ORR. However, the enhanced activity of binary catalysts is lost when the ORR is studied in the presence of methanol. Ternary catalysts containing Ru showed higher methanol-tolerance, regardless of the composition.
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