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dc.contributor.advisorOlaya Florez, Jhon Jairo
dc.contributor.advisorRodil, Sandra
dc.creatorSuarez Garcia, Oscar Javier
dc.date.accessioned2020-05-13T23:02:31Z
dc.date.available2020-05-13T23:02:31Z
dc.date.created2017-04-12
dc.identifier.urihttps://repositorio.unal.edu.co/handle/unal/77516
dc.descriptionEn esta investigación se sintetizaron copolímeros sulfonados de estireno - divinilbeceno y terpolímeros de estireno – divinilbenceno – vinilbencen sulfonato de sodio, los cuales fueron caracterizados y empleados como matriz polimérica para la producción de nanocompositos con partículas de bismuto y estaño. La síntesis de nanopartículas se realizó en fase líquida mediante la reducción con borohidruro de sodio de las sales de cloruro de bismuto o estaño, empleando como solvente dimetilformamida. La estabilización de las nanopartículas en fase líquida se logró mediante un mecanismo combinado estérico y electrostático al emplear soluciones de polímero y del tensoactivo no iónico polioxietilen 23 lauril éter (brij 35). Dos de los terpolímeros sulfonados que presentaron la mayor solubilidad en dimetilformamida, así como la resina comercial nafion que es un copolímero fluorado y sulfonado fueron seleccionados como matriz polimérica. Las variables de control del tamaño de partícula durante la síntesis fueron: concentración de brij 35 de 0.1 a 0.3 %, concentración de metal en solución de 3 a 5 mM y la relación atómica Bi/Sn de 0 a 100 %. Se estudiaron la estabilidad de las suspensiones y la cinética de crecimiento de nanopartículas mediante la técnica de dispersión de luz dinámica (DLS). Las suspensiones de nanopartículas producidas con una composición de 0.2 % de brij 35 y 4 mM de metal, presentaron tamaños de partícula del orden de 100 nm y una buena estabilidad, por esta razón fueron seleccionadas para preparar las películas de nanocomposito para su posterior caracterizaron estructural y electroquímica. Los materiales obtenidos se caracterizaron mediante las siguientes técnicas: difracción de rayos X (DRX), microscopía electrónica de barrido y de transmisión (SEM y TEM), espectroscopias infrarroja (IR), de fotoelectrones de rayos X (XPS) y de energía dispersiva (EDX), estos análisis permitieron verificar la existencia de un material nanoestructurado. Por último se evaluó la aplicación funcional de los nanocompositos mediante voltametría de onda cuadrada (SWV) usando el material como recubrimiento en electrodos de grafito para cuantificar metales pesados (Pb, Cd y Zn) en soluciones buffer pH 5.6 así como en aguas residuales procedentes de procesos industriales de zincado. A partir de los resultados experimentales y de la simulación numérica del comportamiento esperado de estos materiales, se compararon las propiedades electroquímicas con respecto a las de los electrodos de película de bismuto que ya han sido empelados como sensores en técnicas electro analíticas y se relacionaron con la estructura del nanocomposito obtenido, apuntando siempre hacia la posible aplicación de este material como electrodo en ambientes químicos complejos como lo son los vertimientos industriales con contenidos de metales pesados. Los nanocompositos producidos presentaron un buen rendimiento en su aplicación para cuantificar metales pesados en aguas residuales, sin embargo se hace necesario mejorar el método de fabricación de los electrodos para lograr mayor uniformidad de los recubrimientos y de esta manera mejorar la precisión y disminuir la variación del error experimental.
dc.description.abstractIn this research, sulfonated styrene - divinylbenzene copolymers and sodium styrene - divinylbenzene - vinylbenzene sulfonate terpolymers were synthesized, which were characterized and used as polymer matrix for the production of nanocomposites with bismuth and tin particles. The synthesis of nanoparticles was carried out in the liquid phase by reduction with sodium borohydride of the bismuth chloride or tin salts, using dimethylformamide as the solvent. The stabilization of the nanoparticles in the liquid phase was achieved by a combined steric and electrostatic mechanism when using solutions of polymer and the nonionic surfactant polyoxyethylene 23 lauryl ether (brij 35). Two of the sulfonated terpolymers which exhibited the highest solubility in dimethylformamide, as well as the commercial nafion resin which is a fluorinated and sulfonated copolymer were selected as polymeric matrix. The particle size control variables during the synthesis were: brij concentration of 0.1 to 0.3%, concentration of metal in solution of 3 to 5 mM and the atomic ratio Bi / Sn of 0 to 100%. Suspension stability and nanoparticle growth kinetics were studied using the dynamic light scattering (DLS) technique. Suspensions of nanoparticles produced with a composition of 0.2% Brij 35 and 4 mM of metal had particle sizes of the order of 100 nm and good stability, for this reason they were selected to prepare the nanocomposite films for structural and electrochemical characterization. The obtained materials were characterized by the following techniques: X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM and TEM), infrared (IR) spectroscopy, X-ray photoelectron (XPS) and dispersive energy (EDX), these analyzes allowed to verify the existence of a nanostructured material. Finally the functional application of the nanocomposites by square wave voltammetry (SWV) using the material as a coating on graphite electrodes was used to quantify heavy metals (Pb, Cd and Zn) in buffer solutions pH 5.6 as well as in waste water from industrial zinc coating processes. From the experimental results and the numerical simulation of the expected behavior of these materials, the electrochemical properties were compared with those of the bismuth film electrodes which have already been electrochemical sensors and were related to the structure of the obtained nanocomposite, always aiming at the possible application of this material as electrode in complex chemical environments such as industrial waste waters with heavy metal content. The nanocomposites produced presented a good performance in their application to quantify heavy metals in wastewater, however, it is necessary to improve the method of manufacture of the electrodes to achieve greater uniformity of the coatings and in this way improve the accuracy and decrease the variation of the experimental error.
dc.format.extent216
dc.format.mimetypeapplication/pdf
dc.language.isospa
dc.rights.urihttp://creativecommons.org/licenses/by-nc-nd/2.5/co/
dc.subjectNanocompositos
dc.subjectPolímeros sulfonados
dc.subjectNafion
dc.subjectBismuto
dc.subjectEstaño
dc.subjectElectroquímica
dc.subject.ddc620 - Ingeniería y operaciones afines
dc.titleObtención y caracterización electroquímica y estructural de nanocompositos de copolimeros sulfonados/bismuto – estaño
dc.typeOther
dc.rights.spaAcceso abierto
dc.contributor.institutionUniversidad Nacional de Colombia - Sede Bogotá
dc.subject.keywordNanocomposites
dc.subject.keywordSulfonated polymers
dc.subject.keywordNafion
dc.subject.keywordBismuth
dc.subject.keywordTin
dc.subject.keywordElectrochemistry
dc.type.spaOtro
dc.type.hasversionAccepted Version
dc.contributor.gruplacGRUPO DE INVESTIGACIÓN AFIS (ANÁLISIS DE FALLAS, INTEGRIDAD Y SUPERFICIES)
dc.description.projectBisnano
dc.description.additionalDoctor en Ingeniería Ciencia y Tecnología de Materiales
dc.coverage.modalityDoctorado
dc.rights.accessRightsOpen Access
dc.rights.ccAtribución-NoComercial-SinDerivadas 2.5 Colombia
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