Removal of emerging pollutants in water through adsorption and catalytic processes using pillared clays synthesized from aluminum saline slags

• Autores: Yaneth Cardona Rodríguez
• Directores de la Tesis: Antonio Gil Bravo (dir. tes.), Sophia Korili (dir. tes.)
• Lectura: En la Universidad Pública de Navarra ( España ) en 2022
• Idioma: inglés
• Número de páginas: 474
• Títulos paralelos:
  • Eliminación de contaminantes emergentes en aguas mediante adsorción y procesos catalíticos utilizando arcillas pilares sintetizadas a partir de escorias salinas de aluminio
• Enlaces
  • Tesis en acceso abierto en: Academica-e
• Resumen
  • español

    En este trabajo se extrajo el aluminio de las escorias salinas utilizando tanto la vía alcalina como la ácida. Dichos extractos fueron utilizados como precursores en la síntesis de Arcillas Pilares (PILC) obteniendo estructuras pilareadas a partir del extracto ácido (Al-PILCAE) y del alcalino (Al-PILCBE). Se estudiaron los parámetros en la síntesis de dichos PILC caracterizando los sólidos obtenidos con el fin de optimizar el proceso de síntesis y elegir los sólidos con mejores características. Los sólidos elegidos se estudiaron como adsorbentes y soportes catalíticos para la eliminación de tres contaminantes emergentes del agua: 2,6-diclorofenol (2,6-DCP), triclosán (TCS) y bisfenol A (BPA). Se comparó el comportamiento adsorbente y catalítico tanto con la arcilla cruda utilizada en su síntesis (montmorillonita – Mt) como con un PILC sintetizado por el método convencional utilizando como precursor una sal comercial de aluminio (Al-PILCCM). Las dos primeras secciones de esta tesis se centran en la teoría relacionada con el tema. El Capítulo Primero (I) se refiere a los PILC, su síntesis, los parámetros que intervienen en esta, y su importancia e impacto en las propiedades del sólido obtenido. Este capítulo recogió los estudios relacionados con este campo, tratando de comprender la formación de los policationes que hacen posible la síntesis de PILC. El Capítulo Segundo (II) está relacionado con la contaminación del agua y las técnicas utilizadas para eliminar los contaminantes del medio acuático. Este capítulo se centró en el uso del proceso de adsorción, y el uso de PILC como adsorbentes de contaminantes orgánicos, recogiendo los estudios que los han utilizado con este fin. Los siguientes cuatro capítulos (Capítulo III a Capítulo VI) están relacionados con los resultados y análisis de los resultados de la parte experimental desarrollada en este trabajo. Los dos primeros de ellos (Capítulo III y Capítulo IV) están relacionados con la síntesis de los materiales porosos a base de arcilla y su uso como adsorbentes, y los dos siguientes (Capítulo V y Capítulo VI) con su uso en fotocatálisis. El Capítulo Tres (III) corresponde a la síntesis de PILC a partir de la escoria salina y su evaluación como adsorbentes en modo discontinuo. Se evaluaron los parámetros involucrados en el proceso de síntesis, caracterizando cada vez los sólidos sintetizados para confirmar que el proceso de pilarización fue exitoso. Se escogió el proceso de síntesis que dio como resultado sólidos con mejores características para cada uno de los dos extractos: alcalino (Al-PILCBE) y ácido (Al-PILCAE). Esos PILC se evaluaron como adsorbentes para eliminar 2,6-DCP, BPA y TCS del agua, en modo discontinuo. Las capacidades de adsorción resultantes se compararon con Mt y Al-PILCCM. Además, también se estudió la reutilización del agente intercalante secuencialmente para sintetizar Al-PILC como la reutilización del Al-PILC inicial sintetizado como adsorbente. Es necesario resaltar que esta es la primera vez que se sintetiza un material poroso a partir de escoria salina utilizando ambos extractos, alcalino y ácido. El anexo de este documento está relacionado con esta parte del estudio. Los resultados obtenidos en la optimización de la síntesis de PILC utilizando escorias salinas dieron como resultado, una metodología que sintetizó PILC con características de textura mejoradas en comparación con los preparados a través del método convencional. Esta metodología se evaluó utilizando una sal comercial como precursor y los resultados confirmaron que los sólidos obtenidos con esta tenían mejores propiedades texturales que con la metodología convencional. Por ello, debido a la novedad de la metodología encontrada, la información técnica de la invención fue divulgada en una solicitud de patente (202130047) como se puede apreciar en el apartado anexo. El capítulo cuarto (IV) corresponde al estudio de los tres Al-PILC (Al-PILCAE, Al-PILCBE y Al-PILCCM) como adsorbentes en sistemas de columna de lecho fijo para la remoción de TCS. Además de las curvas de avance, la adsorción de adsorción de TCS en este sistema fue optimizada para su uso en Extracción en Fase Sólida (SPE) por Metodología de Superficie de Respuesta usando un Diseño Box-Behnken (RSM-BBD). Los estudios de columna de lecho fijo se suelen realizar para considerar la posible aplicación de los adsorbentes en los procesos de potabilización de agua, sin embargo, dichos estudios se pueden realizar a pequeña escala para proponer nuevos materiales que mejoren las metodologías y técnicas rutinarias utilizadas en el laboratorio, incluyendo la metodologías de preparación de muestras como SPE. Este estudio, por primera vez, utilizó herramientas quimiométricas para optimizar la adsorción de TCS en columna de lecho fijo por Al-PILC para usarlo en SPE. Esta es otra forma de apoyar la investigación relacionada con la contaminación del agua con EP. Las bajas concentraciones de EP en las fuentes de agua pueden ser inferiores al Límite de Detección (LOD) y al Límite de Cuantificación (LOQ) de las técnicas analíticas necesarias para evaluarlas. Hace necesario un paso de preconcentración previo a su determinación y cuantificación. Por ello, es relevante el estudio y propuesta de nuevos sorbentes que puedan ser utilizados en técnicas de preparación como SPE para la determinación y cuantificación de EP en agua. El capítulo cinco (V) corresponde al uso y comparación de Mt y los tres Al-PILC como soportes catalíticos para la eliminación de 2,6-DCP, TCS y BPA del agua a través de la degradación fotocatalítica usando irradiación de luz VIS y UV. Los catalizadores/TiO2 se sintetizaron mediante impregnación húmeda mediante agitación seguida de calcinación. Se estudiaron diferentes cargas de titanio, y la caracterización de los sólidos se realizó mediante varias técnicas. Finalmente, los fotoproductos presentes en las soluciones al final del proceso fueron evaluados por cromatografía líquida de alta resolución-espectrometría de masas (HPLC-MS). Además, dado que este capítulo es el primero relacionado con la catálisis, complementa la información teórica mostrada en el capítulo dos, enumerando aquellos estudios que han utilizado arcillas y PILC en procesos de fotodegradación catalítica. La novedad de este trabajo radica en el uso de Al-PILC sintetizado a partir de escorias salinas de aluminio como soportes catalíticos y la evaluación de la irradiación con luz visible para este proceso. Finalmente, el Capítulo Seis (VI) corresponde al uso y comparación de Mt y los tres Al-PILC como soportes catalíticos para la remoción de 2,6-DCP, TCS, y BPA del agua mediante procesos similares a Fenton y Photo-Fenton. Se evaluaron catalizadores de Fe(III)/TiO2/ con diferentes cargas de titanio y hierro en soluciones monocomponentes y en una mezcla equimolar. Todos los catalizadores se caracterizaron mediante varias técnicas y los subproductos de cada contaminante se identificaron durante las reacciones mediante HPLC-MS. Se sugirió una ruta de degradación para cada contaminante basada en los subproductos identificados durante las reacciones. La originalidad de este trabajo está relacionada con el hecho de analizar el proceso tanto en sistemas monocomponentes como mixtos, utilizando Al-PILC sintetizado a partir de escorias salinas de aluminio como soportes catalíticos. Todos los catalizadores se caracterizaron mediante varias técnicas y los subproductos de cada contaminante se identificaron durante las reacciones mediante HPLC-MS. Se sugirió una ruta de degradación para cada contaminante basada en los subproductos identificados durante las reacciones. La originalidad de este trabajo está relacionada con el hecho de analizar el proceso tanto en sistemas monocomponentes como mixtos, utilizando Al-PILC sintetizado a partir de escorias salinas de aluminio como soportes catalíticos. Todos los catalizadores se caracterizaron mediante varias técnicas y los subproductos de cada contaminante se identificaron durante las reacciones mediante HPLC-MS. Se sugirió una ruta de degradación para cada contaminante basada en los subproductos identificados durante las reacciones. La originalidad de este trabajo está relacionada con el hecho de analizar el proceso tanto en sistemas monocomponentes como mixtos, utilizando Al-PILC sintetizado a partir de escorias salinas de aluminio como soportes catalíticos.

  • English

    In this work, the aluminum was extracted from the saline slags using both ways the alkaline and the acidic one. Those extracts were used as precursors in the synthesis of Pillared Clays (PILC) obtaining pillared structures from the acidic extract (Al-PILCAE) and from the alkaline one (Al-PILCBE). The parameters in the synthesis of those PILC were studied characterizing the solids obtained with the purpose to optimize the synthesis process and choose the solids with the better characteristics. The solids chosen were studied as adsorbents and catalytic supports for the removal of three emerging pollutants from water: 2,6-dichlorophenol (2,6-DCP), triclosan (TCS), and bisphenol A (BPA). The adsorptive and catalytic behavior was compared with both the raw clay used in their synthesis (montmorillonite – Mt) and with a PILC synthesized by the conventional method using an aluminum commercial salt as the precursor (Al-PILCCM). The first two sections of this thesis focus on the theory related to the subject. First Chapter (I) refers to PILC, their synthesis, the parameters involved in this, and their importance and impact on the properties of the solid obtained. This chapter collected the studies related to this field, trying to understand the formation of the polycations that make possible the synthesis of PILC. The Second Chapter (II) is related to water pollution and the techniques used to eliminate pollutants from the aquatic environment. This chapter focused on the use of the adsorption process, and the use of PILC as adsorbents for organic pollutants, collecting the studies which have used them for this purpose. The next four chapters (Chapter III to Chapter VI) are related to the results and analysis of the results of the experimental part developed in this work. The first two of them (Chapter III and Chapter IV) are related to the synthesis of the porous clay-based materials and their use as adsorbents, and the next two (Chapter V and Chapter VI) to their use in photocatalysis. Chapter Three (III) corresponds to the synthesis of PILC from the saline slag and their evaluation as adsorbents in batch mode. The parameters involved in the synthesis process were evaluated, characterizing every time the synthesized solids to confirm that the pillaring process was successful. The synthesis process which resulted in solids with better characteristics was chosen for every one of both extracts: alkaline (Al-PILCBE) and acidic (Al-PILCAE). Those PILC were evaluated as adsorbents to remove 2,6-DCP, BPA, and TCS from water, in batch mode. The resulting adsorption capacities were compared with Mt and Al-PILCCM. Additionally, the reuse of the intercalating agent sequentially to synthesize Al-PILC as the reuse of the initial Al-PILC synthesized as adsorbent also was studied. It is necessary to highlight that this is the first time that a porous material is synthesized from saline slag using both extracts, alkaline, and acid. The annex in this document is related to this part of the study. The results obtained in the optimization of the synthesis of PILC using saline slag gave, as a result, a methodology that synthesized PILC with improved textural characteristics compared with those prepared through the conventional method. This methodology was evaluated using a commercial salt as the precursor and the results confirmed that the solids obtained using this had improved textural properties than using the conventional methodology. For this reason, due to the novelty of the methodology found, the technical information about the invention was disclosed in a patent application (202130047) as can be seen in the annex section. Chapter Four (IV) corresponds to the study of the three Al-PILC (Al-PILCAE, Al-PILCBE, and Al-PILCCM) as adsorbents in fixed bed column systems for the removal of TCS. In addition to the breakthrough curves, the adsorption of TCS adsorption in this system was optimized for its use in Solid Phase Extraction (SPE) by Response Surface Methodology using a Box–Behnken Design (RSM-BBD). Fixed-bed column studies are usually carried out to consider the possible application of the adsorbents in water purification processes, however, those studies can be made on a small scale to propose new materials to improve methodologies and routinary techniques used in the laboratory, including the sample preparation methodologies such as SPE. This study, for the first time, used chemometric tools to optimize the adsorption of TCS in fixed bed column by Al-PILC to use it in SPE. This is another way to support the research related to water pollution with EP. The low concentrations of EP in water sources can be lower than the Limit of Detection (LOD) and Limit of Quantitation (LOQ) of the analytical techniques necessary to evaluate those. It makes necessary a pre-concentration step prior to their determination and quantification. For this reason, the study and proposal of new sorbents that can be used in preparation techniques such as SPE for the determination and quantification of EP in water are relevant. Chapter Five (V) corresponds to the use and comparison of Mt and the three Al-PILC as catalytic supports for the removal of 2,6-DCP, TCS, and BPA from water through photocatalytic degradation using both VIS and UV light irradiation. TiO2/catalysts were synthesized by wet impregnation through stirring followed by calcination. Different loads of titanium were studied, and the characterization of the solids was carried out by several techniques. Finally, the photoproducts present in the solutions at the end of the process were evaluated by High-Performance Liquid Chromatography-Mass Spectrometry (HPLC-MS). Additionally, since this chapter is the first related to catalysis, it complements the theoretical information shown in chapter two, listing those studies which have used clays and PILC in catalytic photodegradation processes. The novelty of this work lies in the use of Al-PILC synthesized from aluminum saline slags as catalytic supports and the evaluation of visible light irradiation for this process. Finally, Chapter Six (VI) corresponds to the use and comparison of Mt and the three Al-PILC as catalytic supports for the removal of 2,6-DCP, TCS, and BPA from water by Fenton and Photo-Fenton like processes. Fe(III)/TiO2/ catalysts with different titanium and iron loads were evaluated in single-component solutions and in an equimolar mixture. All catalysts were characterized by several techniques and the by-products for every pollutant were identified during the reactions by HPLC-MS. A degradation pathway was suggested for every pollutant based on the by-products identified during the reactions. The originality of this work is related to the fact of analyzing the process in both single and mixture components systems, using Al-PILC synthesized from aluminum saline slags as catalytic supports.In this work, the aluminum was extracted from the saline slags using both ways the alkaline and the acidic one. Those extracts were used as precursors in the synthesis of Pillared Clays (PILC) obtaining pillared structures from the acidic extract (Al-PILCAE) and from the alkaline one (Al-PILCBE). The parameters in the synthesis of those PILC were studied characterizing the solids obtained with the purpose to optimize the synthesis process and choose the solids with the better characteristics. The solids chosen were studied as adsorbents and catalytic supports for the removal of three emerging pollutants from water: 2,6-dichlorophenol (2,6-DCP), triclosan (TCS), and bisphenol A (BPA). The adsorptive and catalytic behavior was compared with both the raw clay used in their synthesis (montmorillonite – Mt) and with a PILC synthesized by the conventional method using an aluminum commercial salt as the precursor (Al-PILCCM). The first two sections of this thesis focus on the theory related to the subject. First Chapter (I) refers to PILC, their synthesis, the parameters involved in this, and their importance and impact on the properties of the solid obtained. This chapter collected the studies related to this field, trying to understand the formation of the polycations that make possible the synthesis of PILC. The Second Chapter (II) is related to water pollution and the techniques used to eliminate pollutants from the aquatic environment. This chapter focused on the use of the adsorption process, and the use of PILC as adsorbents for organic pollutants, collecting the studies which have used them for this purpose. The next four chapters (Chapter III to Chapter VI) are related to the results and analysis of the results of the experimental part developed in this work. The first two of them (Chapter III and Chapter IV) are related to the synthesis of the porous clay-based materials and their use as adsorbents, and the next two (Chapter V and Chapter VI) to their use in photocatalysis. Chapter Three (III) corresponds to the synthesis of PILC from the saline slag and their evaluation as adsorbents in batch mode. The parameters involved in the synthesis process were evaluated, characterizing every time the synthesized solids to confirm that the pillaring process was successful. The synthesis process which resulted in solids with better characteristics was chosen for every one of both extracts: alkaline (Al-PILCBE) and acidic (Al-PILCAE). Those PILC were evaluated as adsorbents to remove 2,6-DCP, BPA, and TCS from water, in batch mode. The resulting adsorption capacities were compared with Mt and Al-PILCCM. Additionally, the reuse of the intercalating agent sequentially to synthesize Al-PILC as the reuse of the initial Al-PILC synthesized as adsorbent also was studied. It is necessary to highlight that this is the first time that a porous material is synthesized from saline slag using both extracts, alkaline, and acid. The annex in this document is related to this part of the study. The results obtained in the optimization of the synthesis of PILC using saline slag gave, as a result, a methodology that synthesized PILC with improved textural characteristics compared with those prepared through the conventional method. This methodology was evaluated using a commercial salt as the precursor and the results confirmed that the solids obtained using this had improved textural properties than using the conventional methodology. For this reason, due to the novelty of the methodology found, the technical information about the invention was disclosed in a patent application (202130047) as can be seen in the annex section. Chapter Four (IV) corresponds to the study of the three Al-PILC (Al-PILCAE, Al-PILCBE, and Al-PILCCM) as adsorbents in fixed bed column systems for the removal of TCS. In addition to the breakthrough curves, the adsorption of TCS adsorption in this system was optimized for its use in Solid Phase Extraction (SPE) by Response Surface Methodology using a Box–Behnken Design (RSM-BBD). Fixed-bed column studies are usually carried out to consider the possible application of the adsorbents in water purification processes, however, those studies can be made on a small scale to propose new materials to improve methodologies and routinary techniques used in the laboratory, including the sample preparation methodologies such as SPE. This study, for the first time, used chemometric tools to optimize the adsorption of TCS in fixed bed column by Al-PILC to use it in SPE. This is another way to support the research related to water pollution with EP. The low concentrations of EP in water sources can be lower than the Limit of Detection (LOD) and Limit of Quantitation (LOQ) of the analytical techniques necessary to evaluate those. It makes necessary a pre-concentration step prior to their determination and quantification. For this reason, the study and proposal of new sorbents that can be used in preparation techniques such as SPE for the determination and quantification of EP in water are relevant. Chapter Five (V) corresponds to the use and comparison of Mt and the three Al-PILC as catalytic supports for the removal of 2,6-DCP, TCS, and BPA from water through photocatalytic degradation using both VIS and UV light irradiation. TiO2/catalysts were synthesized by wet impregnation through stirring followed by calcination. Different loads of titanium were studied, and the characterization of the solids was carried out by several techniques. Finally, the photoproducts present in the solutions at the end of the process were evaluated by High-Performance Liquid Chromatography-Mass Spectrometry (HPLC-MS). Additionally, since this chapter is the first related to catalysis, it complements the theoretical information shown in chapter two, listing those studies which have used clays and PILC in catalytic photodegradation processes. The novelty of this work lies in the use of Al-PILC synthesized from aluminum saline slags as catalytic supports and the evaluation of visible light irradiation for this process. Finally, Chapter Six (VI) corresponds to the use and comparison of Mt and the three Al-PILC as catalytic supports for the removal of 2,6-DCP, TCS, and BPA from water by Fenton and Photo-Fenton like processes. Fe(III)/TiO2/ catalysts with different titanium and iron loads were evaluated in single-component solutions and in an equimolar mixture. All catalysts were characterized by several techniques and the by-products for every pollutant were identified during the reactions by HPLC-MS. A degradation pathway was suggested for every pollutant based on the by-products identified during the reactions. The originality of this work is related to the fact of analyzing the process in both single and mixture components systems, using Al-PILC synthesized from aluminum saline slags as catalytic supports.In this work, the aluminum was extracted from the saline slags using both ways the alkaline and the acidic one. Those extracts were used as precursors in the synthesis of Pillared Clays (PILC) obtaining pillared structures from the acidic extract (Al-PILCAE) and from the alkaline one (Al-PILCBE). The parameters in the synthesis of those PILC were studied characterizing the solids obtained with the purpose to optimize the synthesis process and choose the solids with the better characteristics. The solids chosen were studied as adsorbents and catalytic supports for the removal of three emerging pollutants from water: 2,6-dichlorophenol (2,6-DCP), triclosan (TCS), and bisphenol A (BPA). The adsorptive and catalytic behavior was compared with both the raw clay used in their synthesis (montmorillonite – Mt) and with a PILC synthesized by the conventional method using an aluminum commercial salt as the precursor (Al-PILCCM). The first two sections of this thesis focus on the theory related to the subject. First Chapter (I) refers to PILC, their synthesis, the parameters involved in this, and their importance and impact on the properties of the solid obtained. This chapter collected the studies related to this field, trying to understand the formation of the polycations that make possible the synthesis of PILC. The Second Chapter (II) is related to water pollution and the techniques used to eliminate pollutants from the aquatic environment. This chapter focused on the use of the adsorption process, and the use of PILC as adsorbents for organic pollutants, collecting the studies which have used them for this purpose. The next four chapters (Chapter III to Chapter VI) are related to the results and analysis of the results of the experimental part developed in this work. The first two of them (Chapter III and Chapter IV) are related to the synthesis of the porous clay-based materials and their use as adsorbents, and the next two (Chapter V and Chapter VI) to their use in photocatalysis. Chapter Three (III) corresponds to the synthesis of PILC from the saline slag and their evaluation as adsorbents in batch mode. The parameters involved in the synthesis process were evaluated, characterizing every time the synthesized solids to confirm that the pillaring process was successful. The synthesis process which resulted in solids with better characteristics was chosen for every one of both extracts: alkaline (Al-PILCBE) and acidic (Al-PILCAE). Those PILC were evaluated as adsorbents to remove 2,6-DCP, BPA, and TCS from water, in batch mode. The resulting adsorption capacities were compared with Mt and Al-PILCCM. Additionally, the reuse of the intercalating agent sequentially to synthesize Al-PILC as the reuse of the initial Al-PILC synthesized as adsorbent also was studied. It is necessary to highlight that this is the first time that a porous material is synthesized from saline slag using both extracts, alkaline, and acid. The annex in this document is related to this part of the study. The results obtained in the optimization of the synthesis of PILC using saline slag gave, as a result, a methodology that synthesized PILC with improved textural characteristics compared with those prepared through the conventional method. This methodology was evaluated using a commercial salt as the precursor and the results confirmed that the solids obtained using this had improved textural properties than using the conventional methodology. For this reason, due to the novelty of the methodology found, the technical information about the invention was disclosed in a patent application (202130047) as can be seen in the annex section. Chapter Four (IV) corresponds to the study of the three Al-PILC (Al-PILCAE, Al-PILCBE, and Al-PILCCM) as adsorbents in fixed bed column systems for the removal of TCS. In addition to the breakthrough curves, the adsorption of TCS adsorption in this system was optimized for its use in Solid Phase Extraction (SPE) by Response Surface Methodology using a Box–Behnken Design (RSM-BBD). Fixed-bed column studies are usually carried out to consider the possible application of the adsorbents in water purification processes, however, those studies can be made on a small scale to propose new materials to improve methodologies and routinary techniques used in the laboratory, including the sample preparation methodologies such as SPE. This study, for the first time, used chemometric tools to optimize the adsorption of TCS in fixed bed column by Al-PILC to use it in SPE. This is another way to support the research related to water pollution with EP. The low concentrations of EP in water sources can be lower than the Limit of Detection (LOD) and Limit of Quantitation (LOQ) of the analytical techniques necessary to evaluate those. It makes necessary a pre-concentration step prior to their determination and quantification. For this reason, the study and proposal of new sorbents that can be used in preparation techniques such as SPE for the determination and quantification of EP in water are relevant. Chapter Five (V) corresponds to the use and comparison of Mt and the three Al-PILC as catalytic supports for the removal of 2,6-DCP, TCS, and BPA from water through photocatalytic degradation using both VIS and UV light irradiation. TiO2/catalysts were synthesized by wet impregnation through stirring followed by calcination. Different loads of titanium were studied, and the characterization of the solids was carried out by several techniques. Finally, the photoproducts present in the solutions at the end of the process were evaluated by High-Performance Liquid Chromatography-Mass Spectrometry (HPLC-MS). Additionally, since this chapter is the first related to catalysis, it complements the theoretical information shown in chapter two, listing those studies which have used clays and PILC in catalytic photodegradation processes. The novelty of this work lies in the use of Al-PILC synthesized from aluminum saline slags as catalytic supports and the evaluation of visible light irradiation for this process. Finally, Chapter Six (VI) corresponds to the use and comparison of Mt and the three Al-PILC as catalytic supports for the removal of 2,6-DCP, TCS, and BPA from water by Fenton and Photo-Fenton like processes. Fe(III)/TiO2/ catalysts with different titanium and iron loads were evaluated in single-component solutions and in an equimolar mixture. All catalysts were characterized by several techniques and the by-products for every pollutant were identified during the reactions by HPLC-MS. A degradation pathway was suggested for every pollutant based on the by-products identified during the reactions. The originality of this work is related to the fact of analyzing the process in both single and mixture components systems, using Al-PILC synthesized from aluminum saline slags as catalytic supports.In this work, the aluminum was extracted from the saline slags using both ways the alkaline and the acidic one. Those extracts were used as precursors in the synthesis of Pillared Clays (PILC) obtaining pillared structures from the acidic extract (Al-PILCAE) and from the alkaline one (Al-PILCBE). The parameters in the synthesis of those PILC were studied characterizing the solids obtained with the purpose to optimize the synthesis process and choose the solids with the better characteristics. The solids chosen were studied as adsorbents and catalytic supports for the removal of three emerging pollutants from water: 2,6-dichlorophenol (2,6-DCP), triclosan (TCS), and bisphenol A (BPA). The adsorptive and catalytic behavior was compared with both the raw clay used in their synthesis (montmorillonite – Mt) and with a PILC synthesized by the conventional method using an aluminum commercial salt as the precursor (Al-PILCCM). The first two sections of this thesis focus on the theory related to the subject. First Chapter (I) refers to PILC, their synthesis, the parameters involved in this, and their importance and impact on the properties of the solid obtained. This chapter collected the studies related to this field, trying to understand the formation of the polycations that make possible the synthesis of PILC. The Second Chapter (II) is related to water pollution and the techniques used to eliminate pollutants from the aquatic environment. This chapter focused on the use of the adsorption process, and the use of PILC as adsorbents for organic pollutants, collecting the studies which have used them for this purpose. The next four chapters (Chapter III to Chapter VI) are related to the results and analysis of the results of the experimental part developed in this work. The first two of them (Chapter III and Chapter IV) are related to the synthesis of the porous clay-based materials and their use as adsorbents, and the next two (Chapter V and Chapter VI) to their use in photocatalysis. Chapter Three (III) corresponds to the synthesis of PILC from the saline slag and their evaluation as adsorbents in batch mode. The parameters involved in the synthesis process were evaluated, characterizing every time the synthesized solids to confirm that the pillaring process was successful. The synthesis process which resulted in solids with better characteristics was chosen for every one of both extracts: alkaline (Al-PILCBE) and acidic (Al-PILCAE). Those PILC were evaluated as adsorbents to remove 2,6-DCP, BPA, and TCS from water, in batch mode. The resulting adsorption capacities were compared with Mt and Al-PILCCM. Additionally, the reuse of the intercalating agent sequentially to synthesize Al-PILC as the reuse of the initial Al-PILC synthesized as adsorbent also was studied. It is necessary to highlight that this is the first time that a porous material is synthesized from saline slag using both extracts, alkaline, and acid. The annex in this document is related to this part of the study. The results obtained in the optimization of the synthesis of PILC using saline slag gave, as a result, a methodology that synthesized PILC with improved textural characteristics compared with those prepared through the conventional method. This methodology was evaluated using a commercial salt as the precursor and the results confirmed that the solids obtained using this had improved textural properties than using the conventional methodology. For this reason, due to the novelty of the methodology found, the technical information about the invention was disclosed in a patent application (202130047) as can be seen in the annex section. Chapter Four (IV) corresponds to the study of the three Al-PILC (Al-PILCAE, Al-PILCBE, and Al-PILCCM) as adsorbents in fixed bed column systems for the removal of TCS. In addition to the breakthrough curves, the adsorption of TCS adsorption in this system was optimized for its use in Solid Phase Extraction (SPE) by Response Surface Methodology using a Box–Behnken Design (RSM-BBD). Fixed-bed column studies are usually carried out to consider the possible application of the adsorbents in water purification processes, however, those studies can be made on a small scale to propose new materials to improve methodologies and routinary techniques used in the laboratory, including the sample preparation methodologies such as SPE. This study, for the first time, used chemometric tools to optimize the adsorption of TCS in fixed bed column by Al-PILC to use it in SPE. This is another way to support the research related to water pollution with EP. The low concentrations of EP in water sources can be lower than the Limit of Detection (LOD) and Limit of Quantitation (LOQ) of the analytical techniques necessary to evaluate those. It makes necessary a pre-concentration step prior to their determination and quantification. For this reason, the study and proposal of new sorbents that can be used in preparation techniques such as SPE for the determination and quantification of EP in water are relevant. Chapter Five (V) corresponds to the use and comparison of Mt and the three Al-PILC as catalytic supports for the removal of 2,6-DCP, TCS, and BPA from water through photocatalytic degradation using both VIS and UV light irradiation. TiO2/catalysts were synthesized by wet impregnation through stirring followed by calcination. Different loads of titanium were studied, and the characterization of the solids was carried out by several techniques. Finally, the photoproducts present in the solutions at the end of the process were evaluated by High-Performance Liquid Chromatography-Mass Spectrometry (HPLC-MS). Additionally, since this chapter is the first related to catalysis, it complements the theoretical information shown in chapter two, listing those studies which have used clays and PILC in catalytic photodegradation processes. The novelty of this work lies in the use of Al-PILC synthesized from aluminum saline slags as catalytic supports and the evaluation of visible light irradiation for this process. Finally, Chapter Six (VI) corresponds to the use and comparison of Mt and the three Al-PILC as catalytic supports for the removal of 2,6-DCP, TCS, and BPA from water by Fenton and Photo-Fenton like processes. Fe(III)/TiO2/ catalysts with different titanium and iron loads were evaluated in single-component solutions and in an equimolar mixture. All catalysts were characterized by several techniques and the by-products for every pollutant were identified during the reactions by HPLC-MS. A degradation pathway was suggested for every pollutant based on the by-products identified during the reactions. The originality of this work is related to the fact of analyzing the process in both single and mixture components systems, using Al-PILC synthesized from aluminum saline slags as catalytic supports.v