Membrane separations are rapidly growing alternatives to traditionally expensive gas separation processes. For natural gas purification, membranes are used to remove carbon dioxide to prevent pipeline corrosion and increase the heating value of the natural gas. The robust chemical and physical properties of polyimide membranes make them ideal for the numerous components and high pressures associated with natural gas production. Typically, the performance of membranes changes over time as a result of physical aging of the polymer. Previous work shows that the thin selective layer of an asymmetric hollow fiber membrane, the morphology of choice for gas separations, ages differently than a thick dense film of the same material. Also, carbon dioxide, which is highly soluble in most polymers, can actively swell and plasticize polymer membranes at higher pressures. In this work, free acid groups present in the model polyimide are covalently crosslinked to stabilize the matrix against plasticization. Physical aging of two different crosslinked derivatives are compared to the free acid polyimide through gas permeation, gas sorption, and refractive index measurements. Thick (~50 m) and thin (~650 nm) films are examined to determine the effects of sample dimension on physical aging. The crosslinking mechanism employs diol substituents to form ester linkages through the free acid group. However, the annealing treatment, above the glass transition temperature, used to "reset" the thermal history of the films is found to form a new crosslinked polymer. Characterization of this new crosslinking mechanism reveals a high-temperature decarboxylation of the free acid creates free-radical phenyl groups which form covalent crosslinks through other portions of the polymer structure. Since ester crosslinks may be vulnerable to hydrolysis in aggressive gas feed streams, this new mechanism of crosslinking may create a more robust membrane for aggressive separations. In addition to the physical aging study, supercritical carbon dioxide conditioning of the two glycol crosslinked polyimides is compared to the free acid polymer. In this case, the free acid polymer is not crosslinked since the esterification crosslinking reaction occurs at much lower temperature than the decarboxylation mechanism. The free acid polymer displays an atypical permeation response under supercritical carbon dioxide conditions which suggests a structural reorganization of the polymer occurs. The crosslinked polymers do not exhibit this type of response. Mixed gas permeation confirms a substantial decrease in the productivity of the free acid polyimide and reveals the enhanced stability of the crosslinked polyimides following the supercritical carbon dioxide conditioning. Finally, examination of structurally similar fluorine-containing polyimides following approximately 18 years of aging allows the study of polymer structure on physical aging. A 6FDA-based polyimide is compared to a BPDA-based polyimide to understand the effects of bulky, CF3 groups on physical aging, and polyimides with diamine isomers reveal the effects of structural symmetry on physical aging.

La microfiltration tangentielle sur membrane en céramique est étudiée dans ce travail comme une méthode de fractionnement de suspensions hétérogènes obtenues après hydrolyse acide d'amidon de maïs cireux pour la récupération en continu de nanocristaux d'amidon. Le but est d'évaluer la possibilité de coupler la microfiltration au procédé d'hydrolyse pour augmenter le rendement de production des nanocristaux d'amidon. Une caractérisation des suspensions (taille et charge) a été réalisée à différents stades de la production afin de comprendre l'évolution de la taille des particules au cours de l'hydrolyse et du post-traitement et de pouvoir choisir la bonne membrane pour un fractionnement efficace. Deux pilotes de filtration ont été conçus pour permettre l'étude du fractionnement des suspensions de nanocristaux d'une part à l'échelle laboratoire (membranes planes) et d'autre part à l'échelle semi-industrielle (membrane tubulaire). L'analyse de la suspension produite par le procédé d'hydrolyse classique a montré qu'elle était constituée majoritairement d'agrégats de nanoparticules et de résidu d'amidon partiellement hydrolysé, la quantité de nanocristaux individualisés ne représentant que 5 % de l'amidon initial. L'opération de microfiltration tangentielle a été optimisée (transmission maximale des SNC et colmatage minimum des membranes) en fonction des conditions opératoires grâce à la réalisation d'un plan d'expériences. Dans les conditions optimisées, il était possible de récupérer dans le perméat, 25 % des particules initialement introduites en gardant des flux de perméat important. Ces particules ont une taille inférieure à 300 nm. Dans ces mêmes conditions, il était possible de séparer des nanocristaux d'amidon directement à partir de la suspension acide après hydrolyse. La modélisation du colmatage à partir des essais de filtration frontale a montré que le colmatage se fait essentiellement par formation d'un gâteau à la surface. Nous avons abordé également dans ce travail la piste de la purification en continu des suspensions acides à travers un procédé de diafiltration sur membranes d'ultrafiltration permettant une industrialisation de la production des SNC. / The current work investigates the use of cross flow microfiltration using ceramic membrane to fractionate the heterogeneous suspension obtained after starch hydrolysis in order to isolate starch nanocrystals. The final aim is to evaluate the possibility of coupling the filtration step to the hydrolysis step in a single production loop in order to enhance the starch nanocrystal production yield. The characterizations of the suspension (particle size and charge) obtained with the classic production process indicates that it was a mixture of starch nanocrystal aggregates and starch residues, individualized starch nanocrystals represent only 5 % of the initial starch. The fractionation study was done using two pilot plans, in a dead end configuration at laboratory scale (plate membrane) and in a cross flow configuration at semi-industrial scale (tubular membrane). Design of experiments methodology was used to optimize the fractionation efficiency when filtering a neutral suspension considering the effect of filtration parameter on the transmission yield and membrane fouling. In the optimized condition, it was possible to recover 25 % of starch nanocrystals while keeping the permeate flux at its highest value. Mean diameter of the recovered particle was less than 300 nm. At this condition, it was also possible to recover the starch nanocrystals directly from the acidic mixture obtained at the end of the hydrolysis step. The analysis of fouling mechanism using dead end filtration experiments highlights that membrane fouling occurs because a cake bult up at the membrane surface. This study investigates also the use of ceramic ultrafiltration membrane in a diafiltration process in order to purify the acidic suspension from soluble molecules without modifying particle size distribution which is a promising technique for a large scale production.

O uso de membranas poliméricas vem sendo extensivamente estudado para operações de separação. O estudo de materiais e metodologias para desenvolvimento de tais membranas para redução de custos e melhora em propriedades, faz-se necessário frente a este cenário. No processo de preparação de membranas, materiais orgânicos, tais como polímeros, elastômeros, são empregados com a possibilidade de incorporação de materiais de reforço e para modificar as características de forma a favorecer determinados processos. Estas membranas são chamadas compósitas, obtidas pela dispersão física de um componente na matriz polimérica, sendo que as dimensões da fase dispersa variam da escala micrométrica a nanométrica e a interface entre as fases deve ser bem definida. As fibras naturais tem destaque como materiais de reforço, devido sua natureza renovável e sua vasta fonte de matéria-prima, além de apresentarem boas propriedades mecânicas e baixo custo. A celulose presente na parede celular de plantas pode ser purificada, isolada e incorporada a membranas atuando como agente de reforço. As técnicas de hidrólise são metodologias empregadas para isolar cristais de celulose, que utilizam diferentes ácidos, resultando em diferentes materiais. Neste trabalho foi empregada celulose 1kraft de Eucalyptus ssp seguindo duas metodologias para isolamento de micro (MCC) e nanocristais celulósicos (CNC) utilizando ácido clorídrico e ácido sulfúrico (HCl e H2SO4). A incorporação destes materiais em membranas de polissulfona (PSf) foi avaliada por fluxo de permeado, rejeição de proteínas, ângulo de contato e microscopia eletrônica de varredura e de transmissão. As nanoceluloses apresentaram diâmetro, comprimento definidos e razão de aspecto favorável a incorporação em membranas poliméricas. A solução de nanocelulose obtida pela hidrólise com H2SO4 pode ser considerada mais estável, pois apresentou menos aglomerações. A adição de microcelulose e nanocristais de celulose às membranas de polisulfona (PSf) se mostrou satisfatória para a preparação das membranas poliméricas. Ocorreu aumento na rejeição das proteínas submetidas, da seletividade e da hidrofilia para as membranas reforçadas, principalmente com nanocelulose obtida por hidrólise com HCl. / Submitted by Ana Guimarães Pereira (agpereir@ucs.br) on 2015-03-04T17:08:49Z No. of bitstreams: 1 Dissertacao Diana Favero.pdf: 2660380 bytes, checksum: 03cfad09eac7d1d57e9de212d7afcbc9 (MD5) / Made available in DSpace on 2015-03-04T17:08:49Z (GMT). No. of bitstreams: 1 Dissertacao Diana Favero.pdf: 2660380 bytes, checksum: 03cfad09eac7d1d57e9de212d7afcbc9 (MD5) / Fundação de Amparo à Pesquisa do Estado do Rio Grande do Sul / The use of polymeric membranes has been extensively studied for separation processes. The study of materials and methodologies for development of such membranes for cost reduction and improvement in their properties are necessary to face this scenario. In the preparation of membranes, organic materials such as polymers and elastomers are employed with the possibility of incorporation of reinforcement materials and to modify the characteristics to favor certain processes. These membranes are called composite, they are obtained by dispersing a physical component in the polymer matrix, where the size of the dispersed phase varies from micrometer to nanometer scale and the interface between the phases must be well defined. Natural fibers has highlighted as a reinforcing material due to their renewable nature and vast source of raw materials, in addition having good mechanical properties and low cost. The plant cell wall cellulose can be purified, isolated and incorporated into membranes acting as reinforcing agent. The hydrolysis techniques are employed methodologies for isolating crystals of cellulose, using different acids resulting in different properties. In this work we used Kraft pulp from Eucalyptus ssp following two methods for isolation (acids HCl and H2SO4) of micro (MCC) and nanocrystals (NCC) of cellulose. Incorporating these materials into membranes of polysulfone (PSf) were evaluated for permeate flux, rejection protein, contact angle and scanning and transmission electron microscopy. Nanocelulose presented diameter and length defined and favorable aspect ratio for incorporation into polymeric membranes. The solution obtained after hydrolysis with H2SO4 can be consider more stable as it presented less agglomerations. The addition of microcellulose and cellulose nanocrystals to membranes proved satisfactory for the preparation of polymeric membranes. There was an increase in rejection of the proteins, selectivity and hydrophilicity for the reinforced membranes, especially with nanocelulose obtained by hydrolysis with H2SO4.

The two most common commercial copper baths are the acid sulfate copper bath and the alkaline cyanide copper bath. Alkaline copper baths are mostly used to coat parts with complex geometry and to avoid galvanic deposition when depositing a metal on a less noble substrate. Because of the toxicity of cyanide compounds, alternative baths have been developed using different complexing agents. The starting point of the present study is a cyanide-free strike bath developed for copper plating on Zamak substrates developed by the Institute for Technological Research of the State of São Paulo/ Brazil. The replacement of a raw material such as cyanide must be economically advantageous and technically feasible. Therefore, this study intended to propose an alternative to the treatment of liquid wastes from the mentioned bath, aiming at simultaneous water reclamation and chemicals recovery in a closed system. The electrodialysis membrane separation process was studied, using a laboratoryscale system operating with a synthetic solution simulating the rinsing waters from the HEDP-based bath. The feasibility of the technique was evaluated by analyzing operational parameters such as ion extraction, demineralization rate, concentration rate, current efficiency for each anionic specie and average energy consumption. Because HEDP is a chelating agent, the transport of Cu(II)-HEDP chelates through anion-exchange membranes was also evaluated by means of electrochemical methods. Chronopotentiometric and current-voltage curves were constructed for different model solutions containing the same compounds as the original bath. A relation between the presence of chelates in the solutions and the fixed ion exchange group could be established. Lastly, deposition tests were performed using electrolytes containing the recycled inputs and the characteristics of the coatings were analyzed. The results showed that an electrodialysis stack using strongly basic anion-exchange membranes was suitable to produce treated solutions and a concentrate containing the ions from the bath. The concentrate could be added to the copper bath to compensate eventual drag-out losses without affecting the quality of the coatings. Thus, the application of electrodialysis was shown to be a feasible alternative for recovering water and inputs from the evaluated solution, reducing the wastewater generation and saving natural resources. / Os dois banhos de cobre comerciais mais comuns são o banho ácido à base de sulfato e o banho alcalino à base de cianeto. Os banhos alcalinos são usados principalmente para recobrir peças com geometria complexa e para evitar a deposição por deslocamento galvânico quando se deposita um metal em um substrato menos nobre. Por causa da toxicidade dos compostos cianídricos, banhos alternativos vêm sendo desenvolvidos usando diferentes agentes complexantes. O ponto de partida do presente estudo é um banho toque isento de cianeto para deposição de cobre em substratos de Zamak, desenvolvido pelo Instituto de Pesquisas Tecnológicas / Brasil. A substituição de matérias-primas como o cianeto deve ser economicamente vantajosa e tecnicamente viável. Desta forma, este estudo pretendeu propor uma alternativa para o tratamento de resíduos líquidos do banho mencionado, visando à recuperação simultânea da água e das matérias-primas em um sistema fechado. Foi estudado o processo de separação por membranas de eletrodiálise, usando um sistema em escala laboratorial operando com uma solução sintética que simulava as águas de lavagem do banho à base de HEDP. A viabilidade da técnica foi avaliada por meio da análise de parâmetros operacionais, como a extração dos íons, a taxa de dessalinização, o percentual de concentração, a eficiência de corrente calculada para cada espécie iônica e o consumo médio de energia. Devido ao HEDP ser um agente quelante, o transporte de quelatos Cu(II)-HEDP através de membranas aniônicas foi avaliado por meio de métodos eletroquímicos. Curvas cronopotenciométricas e curvas corrente-potencial foram construídas para diferentes soluções sintéticas que continham os mesmos compostos que o banho original. A relação entre a presença de quelatos nas soluções e os grupos fixos de troca iônica pôde ser estabelecida. Por fim, testes de deposição foram realizados usando eletrólitos contendo os compostos reciclados e as características dos depósitos foram analisadas. Os resultados mostraram que o sistema de eletrodiálise usando membranas aniônicas contendo grupos de troca fortemente básicos pôde produzir soluções tratadas e um concentrado contendo os íons do banho. O concentrado pôde ser adicionado ao banho original para compensar eventuais perdas por arraste sem afetar a qualidade dos depósitos. Assim, a aplicação da eletrodiálise se mostrou uma alternativa viável para a recuperação de água e de insumos da solução avaliada, reduzindo a geração de efluentes e economizando recursos naturais.

O uso de membranas poliméricas vem sendo extensivamente estudado para operações de separação. O estudo de materiais e metodologias para desenvolvimento de tais membranas para redução de custos e melhora em propriedades, faz-se necessário frente a este cenário. No processo de preparação de membranas, materiais orgânicos, tais como polímeros, elastômeros, são empregados com a possibilidade de incorporação de materiais de reforço e para modificar as características de forma a favorecer determinados processos. Estas membranas são chamadas compósitas, obtidas pela dispersão física de um componente na matriz polimérica, sendo que as dimensões da fase dispersa variam da escala micrométrica a nanométrica e a interface entre as fases deve ser bem definida. As fibras naturais tem destaque como materiais de reforço, devido sua natureza renovável e sua vasta fonte de matéria-prima, além de apresentarem boas propriedades mecânicas e baixo custo. A celulose presente na parede celular de plantas pode ser purificada, isolada e incorporada a membranas atuando como agente de reforço. As técnicas de hidrólise são metodologias empregadas para isolar cristais de celulose, que utilizam diferentes ácidos, resultando em diferentes materiais. Neste trabalho foi empregada celulose 1kraft de Eucalyptus ssp seguindo duas metodologias para isolamento de micro (MCC) e nanocristais celulósicos (CNC) utilizando ácido clorídrico e ácido sulfúrico (HCl e H2SO4). A incorporação destes materiais em membranas de polissulfona (PSf) foi avaliada por fluxo de permeado, rejeição de proteínas, ângulo de contato e microscopia eletrônica de varredura e de transmissão. As nanoceluloses apresentaram diâmetro, comprimento definidos e razão de aspecto favorável a incorporação em membranas poliméricas. A solução de nanocelulose obtida pela hidrólise com H2SO4 pode ser considerada mais estável, pois apresentou menos aglomerações. A adição de microcelulose e nanocristais de celulose às membranas de polisulfona (PSf) se mostrou satisfatória para a preparação das membranas poliméricas. Ocorreu aumento na rejeição das proteínas submetidas, da seletividade e da hidrofilia para as membranas reforçadas, principalmente com nanocelulose obtida por hidrólise com HCl. / Fundação de Amparo à Pesquisa do Estado do Rio Grande do Sul / The use of polymeric membranes has been extensively studied for separation processes. The study of materials and methodologies for development of such membranes for cost reduction and improvement in their properties are necessary to face this scenario. In the preparation of membranes, organic materials such as polymers and elastomers are employed with the possibility of incorporation of reinforcement materials and to modify the characteristics to favor certain processes. These membranes are called composite, they are obtained by dispersing a physical component in the polymer matrix, where the size of the dispersed phase varies from micrometer to nanometer scale and the interface between the phases must be well defined. Natural fibers has highlighted as a reinforcing material due to their renewable nature and vast source of raw materials, in addition having good mechanical properties and low cost. The plant cell wall cellulose can be purified, isolated and incorporated into membranes acting as reinforcing agent. The hydrolysis techniques are employed methodologies for isolating crystals of cellulose, using different acids resulting in different properties. In this work we used Kraft pulp from Eucalyptus ssp following two methods for isolation (acids HCl and H2SO4) of micro (MCC) and nanocrystals (NCC) of cellulose. Incorporating these materials into membranes of polysulfone (PSf) were evaluated for permeate flux, rejection protein, contact angle and scanning and transmission electron microscopy. Nanocelulose presented diameter and length defined and favorable aspect ratio for incorporation into polymeric membranes. The solution obtained after hydrolysis with H2SO4 can be consider more stable as it presented less agglomerations. The addition of microcellulose and cellulose nanocrystals to membranes proved satisfactory for the preparation of polymeric membranes. There was an increase in rejection of the proteins, selectivity and hydrophilicity for the reinforced membranes, especially with nanocelulose obtained by hydrolysis with H2SO4.

Orientador: Maria Regina Wolf Maciel / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Quimica / Made available in DSpace on 2018-08-05T04:48:34Z (GMT). No. of bitstreams: 1 TorresAlvarez_MarioEusebio_D.pdf: 10381978 bytes, checksum: 6d92d3ef3288c11e5d00589fa7bff9e7 (MD5) Previous issue date: 2005 / Resumo: Neste trabalho de tese, foi realizado um estudo do potencial do processo de pervaporação como um processo de separação de misturas azeotrópicas. Foram realizados o estudo, a avaliação e a comparação de dois modelos matemáticos selecionados da literatura par o processo de pervaporação, que têm como base o mecanismo solução-difusão. Forma desenvolvidos dois programas computacionais, o PERKAT e o PERBRUN, que pemitiram avaliar, segundo estes modelos, qualquer tipo de mistura binária, aqui exemplificados pelos sistemas etanol/água e acetato de metila/água. Foi proposto um modelo matemático a partir do mecanismo solução-difusão procurando minimizar a necessidade de dados experimentais e assim, possibilitar a avaliação rápida em estágios iniciais de projetos de processos. Foi , ainda, elaborado um algoritmo de calculo para o processo de pervaporação. Afim de obter um modelo mais robusto, minimizando a necessidade de dados experimentais, foram realizados e estudo da predição do coeficiente de difusão na membrana, a determinação do parâmetro de interação binário solvente/polímero, a validação do método de predição com dados experimentais e uma análise de sensibilidade paramétrica. Com isso, foi desenvolvido o simulador ¿PERVAP¿ a partir do modelo matemático proposto neste trabalho. A intenção foi possibilitar ao engenheiro de processos tomadas de decisão rápidas a respeito da possibilidade de usar o processo de pervaporação para a separação de uma mistura binária qualquer ...Observação: O resumo, na íntegra, poderá ser visualizado no texto completo da tese digital / Abstract: In this work, a study of the potential of pervaporation process for the separation of azeotropic mixtures was carries out. Two mathematical models were chosen from the literature for pervaporation process based on solution diffusion mechanism and a study, an evaluation and a comparison between these models were made. Two computational programs were developed, PERKAT and PERBRUN, which allow the evaluation, according to these models, of any type of binary mixture, here exemplified by the system ethanol/water and methyl acetate/water. A mathematical model was proposed based on the solution-diffusion mechanism with the aim of minimizing the necessity of experimental data and, thus, to make possible the fast evaluation in early stages of process design.Furthermore, it was elaborated a calculation algorithm for the pervaporation process. In order to get a more robust model, minimizing the necessity of experimental data, the study of the prediction of the diffusion coefficient in the membrane, the determination of the binary interaction parameter of solvent/polymer, the validation of the prediction method with experimental data and a parametric sensitivity analysis were carried out. With this, the "PERVAP" simulator was developed from the mathematical model proposed in this work. The intention was to make possible for engineers to take rapid decisions regarding the possibility for using the pervaporation process for separating any binary mixture ...Note: The complete abstract is available with the full electronic digital thesis or dissertations / Doutorado / Desenvolvimento de Processos Químicos / Doutor em Engenharia Química

Submitted in fulfilment of the requirements for the Degree of Master of Engineering, Durban University of Technology, 2017. / In this research, the woven fibre microfiltration (WFMF) fabric which is produced locally in South Africa is used as a membrane material. It is cheaper in price in comparison with the current commercial membrane materials that are in use. The WFMF is also more robust when compared with the commercial membrane materials thus is able to withstand harsh working conditions. From previous studies on the WFMF, it has been shown that it can be used as a membrane material without any compromise to permeate quality. This research seeks to optimize the working conditions of this membrane material (WFMF) with an aim of achieving lower running costs and better anti fouling strategies in comparison to the commercial MBRs. The objectives and aims of this research was to come up with a MBR system whose running cost is lower than that for the commercial systems, which can be adapted for use in any environment, especially in the hardship regions where its robustness would be an added advantage. The performance of the WFMF submerged MBR was also optimised including antifouling operating regimes. This study was done in a pilot plant that was set up at Veolia wastewater treatment plant, Durban Metro Southern Works. The feed water for the pilot plant was pumped from the return activated sludge mixing chamber by means of a submersible pump. The MLSS concentration of the feed water was about 12 g/l. The various investigations that were conducted in the course of this research included the effect of spacing between membrane modules, relaxation steps and frequencies, evaluation of aeration rates and evaluation of coarse vs. fine bubbles which were all aimed at optimizing the performance of the immersed WFMF MBR. The permeate was checked for turbidity and COD levels to ensure that they were within the accepted water standards. From the experiments it is shown that the critical flux increased with an increase in aeration rate which is in concurrence with the literature and a starting flux of 30 LMH was chosen for the running of the pilot plant for the various experimental runs to be carried out. For the pipe diffuser height effect experimental run, the best results were achieved at a height of 5 cm below the membrane modules and the use of a pipe diffuser gave better results than the use of a disc diffuser. For the membrane module spacing effect the best results were obtained at the smallest possible width i.e. 3.5 mm. The best relaxation step sequence was found to be 9 mins on and 1 min off. COD, turbidity and DO was continuously determined during the course of the experimentation. Further studies should be done on use of the disc diffuser with increased surface area of aeration holes and also hole sizes of smaller diameters to check on its effectiveness as a means of reducing fouling on the membrane surface. / M

The thesis handles the problem of biogas purification by membrane separation method, and its application on existing biogas plants. Assessing of impacts of this implementation is carried out from technical and economical point of view.

No description available.

[ES] El agua se convirtió en uno de los recursos más escasos de la Tierra. Por eso es necesario desarrollar nuevas tecnologías para el tratamiento adecuado de las aguas residuales urbanas (UWW), permitiendo su reutilización. Múltiples tecnologías han demostrado ser efectivas cuando se aplican individualmente, pero a menudo no se aplican ni se integran en el tratamiento convencional de UWW, lo que resulta en la pérdida de posibles efectos sinérgicos. Por estas razones, la investigación sobre la combinación e integración de estas tecnologías es de suma importancia. Cuando se aplican de esta manera, también se conocen como Tecnologías Integradas Avanzadas. Hecho un trabajo de investigación sobre el rendimiento de una planta piloto de nanofiltración (NF) a escala piloto para UWW, seguido de la aplicación de métodos de tratamiento (químico). Los Procesos de Oxidación Avanzada (AOP), como el proceso (solar) foto-Fenton (SPF), aprovechan el ciclo catalítico del hierro (Fe2+ y Fe3+), la luz UV-vis, junto con un agente oxidante, como el peróxido de hidrógeno (H2O2), produciendo radicales hidroxilo altamente reactivos. Este proceso de foto-Fenton (solar) se aplica a un pH 3, para evitar la precipitación del hierro, o a un pH más alto mediante agentes quelantes, como el ácido etilendiamino-N, N'-disuccínico (EDDS). Los microcontaminantes (MC) usados fueron cafeína, imidacloprid, tiacloprid, carbamazepina y diclofenaco. La preconcentración es un paso esencial antes de aplicar AOP como tratamiento terciario de los efluentes de las plantas de tratamiento de aguas residuales urbanas (EDAR), ya que reduce significativamente el volumen a tratar y, por lo tanto, los costos económicos. El tratamiento de la corriente de concentrado de la NF mediante el proceso de SPF demostró ser efectivo para la eliminación de los MC mencionados anteriormente cuando se utilizó H2O2 como agente de oxidación. Por lo tanto, a una mayor degradación de los MC se adhiere una toxicidad directamente proporcionalmente menor. Las investigaciones incluyen la valorización de los efluentes EDAR mediante la recuperación de amonio, con la eliminación combinada de MC mediante NF y diferentes AOPs, con el fin de producir corrientes de permeado para la fertilización e irrigación directa de cultivos, también conocida como 'fertirrigación'. Esto incluye el proceso de SPF, pero también se combina con procesos de electrooxidación (EO). El SPF fue más efectivo al tratar las corrientes de concentrado de NF a pH circunneutro, con una concentración de MC inferior a 1 mg/L. Las corrientes de concentrado de NF altamente salinas son ideales para ser tratadas mediante procesos de EO, por sus alta conductividad, con un consumo eléctrico significativamente menor con la asistencia solar. La eficiencia de retención de MC por NF y la toxicidad después de los tratamientos con AOP también se evaluaron mediante la determinación de la fitotoxicidad del permeado. Los resultados mostraron que los permeados utilizados para los cultivos (Sorghum saccharatum, Sinapis alba, Lepidium sativum) redujeron la germinación de las semillas. Contrariamente, se observó que la irrigación con los permeados producidos generalmente promovió el desarrollo de las raíces, mientras que el desarrollo de los brotes prosperó solo cuando se usaron permeados que tenían factores de concentración inferiores al factor de concentración 2. Los estudios mostraron que los permeados deberían diluirse primero en un mínimo del 50%, para ser adecuados para la irrigación directa. El trabajo también incluyó la evaluación de una membrana de ultrafiltración (UF) cerámica foto catalítica TiO2-ZrO2 previamente desarrollada. La disminución del flujo puede revertirse cuando se irradia la membrana UF cerámica con luz en un simulador solar. La retención microbiológica de la membrana UF fue determinada utilizando una cepa bacteriana Gram negativa, Pseudomonas aeruginosa y fue capaz de retener consistentemente hasta un orden de magnitud de 1 x 104 UFC/ml. / [CA] L'aigua es va convertir en un dels productes bàsics més escassos de la Terra. Per tant, cal desenvolupar noves tecnologies, com el tractament adequat de les aigües residuals urbanes (UWW) per a la seva reutilització. Múltiples tecnologies avançades es demostren efectives quan s'apliquen únicament. Aquestes tecnologies sovint no s'apliquen ni s'integren en el tractament UWW convencional. Com a resultat, es perd possibles efectes sinèrgics. Per aquests motius, la investigació sobre la combinació i integració d'aquestes noves tecnologies és de la màxima importància. Quan s'apliquen així, aquestes tecnologies combinades també es coneixen i s'indiquen com a Tecnologies Integrades Avançades. Es va realitzar un treball de recerca sobre el rendiment d'una planta de nanofiltració (NF) a escala pilot per a la preconcentració d'UWW, seguida de l'aplicació de mètodes de tractament (químics), per tal de tractar els corrents de concentrat i permeat produïts. Els processos d'oxidació avançats (AOP), com el procés foto-Fenton (solar) (SPF), fan servir el cicle catalític del ferro (Fe2+ i Fe3+), la llum UV-vis, juntament amb un agent oxidant, com el peròxid d'hidrogen (H2O2), produint radicals hidroxil altament reactius i no selectius. Aquest procés SPF s'aplica a pH3, per tal d'evitar la precipitació del ferro, o a pH circumneutral aplicant agents quelants com l'àcid etilendiamina-N, N¿-disuccinic (EDDS). La preconcentració és un pas essencial abans d'aplicar els AOP com a tractament terciari d'efluents d'EDAR, ja que redueix significativament el volum a tractar i, per tant, els costos globals. El tractament del corrent de concentrat del NF mitjançant el procés SPF va demostrar ser eficaç per a l'eliminació de diferents microcontaminants (MC) quan s'utilitzava H2O2 com a agent d'oxidació. Per al qual una degradació de MC més alta s'adhereix a una toxicitat menor directament proporcional. Els seleccionats (MC) van ser cafeïna, imidacloprid, tiacloprid, carbamazepina i diclofenac. Els treballs de recerca posteriors van tractar la valorització dels efluents d'EDAR mitjançant la recuperació d'amoni, amb l'eliminació combinada de MC per NF i diferents AOP avançats, per tal de produir corrents permeats per a la fertilització directa dels cultius i el reg, també anomenats "fertirrigació". Inclou SPF, però també combinat amb processos d'electrooxidació (EO). El SPF va ser més eficaç quan es tractaven corrents de concentrat de NF a pH circumneutral, a una concentració de MC inferior a 1 mg/L, per obtenir una degradació ràpida de MC. Els corrents concentrats de concentrat NF altament salins són ideals per ser tractats mitjançant processos EO, alhora que posseeixen una alta conductivitat, i un menor consum elèctric significatiu per assistència solar. També es va avaluar l'eficiència de retenció de MC per NF i la toxicitat després dels tractaments amb AOP determinant la fitotoxicitat del permeat. Els resultats van mostrar que els permeats podrien reduir la germinació de llavors si s'utilitzaven per a cultius (Sorghum saccharatum, Sinapis alba, Lepidium sativum). Al contrari d'això, es va demostrar que el reg amb els permeats produïts afavoria generalment el desenvolupament de les arrels, mentre que el desenvolupament dels brots només va prosperar quan s'utilitzaven permeats que tenien factors de concentració inferiors a 2. Els estudis de toxicitat van mostrar que els corrents de permeat s'havien de diluir primer amb un mínim del 50% aigua dolça. El treball de recerca realitzat també va incloure l'avaluació d'una membrana d'ultrafiltració ceràmica (UF) fotocatalítica TiO2-ZrO2 desenvolupada prèviament. La disminució del flux es pot revertir quan la membrana fotocatalítica UF va ser irradiada per llum en un simulador solar. La retenció microbiològica de la membrana UF es va determinar mitjançant el desplegament d'una soca bacteriana gramnegativa, Pseudomonas aeruginosa, ser capaç de retenir constantment fins a un ordre de magnitud d'1 x 104 CFU/ml. / [EN] Water turned to be one of Earths scarcest commodities. Therefore, novel technologies need to be developed, as appropriate treatment of produced urban wastewaters (UWWs) for its reuse as irrigation waters or aquifer recharge. Multiple advanced technologies are proven effective when applied solely. These technologies are often not applied or integrated into conventional UWW treatment. Resulting in missing out on potential synergetic effects. For these reasons that research into the combining and integration of these novel technologies is of the utmost importance. When thus applied, these combined technologies are also known and indicated as Advanced Integrated Technologies. Research work was conducted on the performance of a pilot scale nanofiltration (NF) plant for UWW pre-concentration, followed by the application of (chemical) treatment methods, in order to treat the produced concentrate and permeate streams. Advanced Oxidation Processes (AOPs), such as the (solar) photo-Fenton process make use of the catalytic cycle of iron (Fe2+ and Fe3+), UV-vis light, along with an oxidizing agent, such as hydrogen peroxide (H2O2), producing highly reactive and non-selective hydroxyl radicals (¿OH). This (solar) photo-Fenton process is applied at acidic pH3, in order to prevent iron precipitation, or at circumneutral pH by applying chelating agents such as Ethylenediamine-N, N¿-disuccinic acid (EDDS). Preconcentration is an essential step before applying AOPs as tertiary treatment of UWWTP effluents, as it significantly lowers the to be treated volume, and therefore the overall costs. Treating the concentrate stream from the NF by the solar photo-Fenton process showed to be effective for the removal of different microcontaminants (MCs) when H2O2 was used as an oxidation agent. Opposite to that, the application of persulfate and its derived radicals showed lower degradation of the selected MC. For which a higher MC degradation is adhered to a directly proportional lower toxicity. Selected (MCs) were caffeine, imidacloprid, thiacloprid, carbamazepine, and diclofenac. Further research work covered UWWTP effluent valorization by the recovery of ammonium, with combined MC elimination by NF and different advanced AOPs, in order to produce permeate streams for direct crop fertilization and irrigation, also called 'fertigation'. Including solar photo-Fenton, but also combined with electrooxidation (EO) processes. Solar photo-Fenton was most effective when treating NF concentrate streams at circumneutral pH, at MC concentration lower than 1 mg/L, to obtain rapid MC degradation. High saline and concentrated NF concentrate streams are ideal to be treated by EO processes, while possessing high conductivity. Obtaining significant lower electric consumption by solar assistance. MC retention efficiency by NF and toxicity after AOP treatments was also assessed by determining the permeate phytotoxicity. Results showed that permeates could lower seed germination if they would be used for crops (Sorghum saccharatum, Sinapis alba and Lepidium sativum). Contrary to that, it was showed that irrigation with the produced permeates generally promoted root development, while shoot development only thrived when using permeates which had concentration factors lower than 2. Toxicity studies showed that permeate streams should first be diluted with a minimum of 50% fresh water, in order to be suitable for direct crop irrigation in agriculture. Conducted research work also included the assessment of a priorly developed (collaboration with an PhD within MSCA AQUAlity) photocatalytic TiO2-ZrO2 ceramic ultrafiltration (UF) membrane. Flux decline can be reversed when the photocatalytic UF membrane was irradiated by light in a solar simulator. Microbiological retention of the UF membrane was determined by deploying a Gram-negative bacterial strain, Pseudomonas aeruginosa (P. Aeruginosa). It was able to consistently retain till an order of magnitude of 1x10^4 CFU/ml. / This PhD Thesis has received funding from the European Union’s Horizon 2020 research and innovation program, the AQUAlity project, under the Marie SkłodowskaCurie grant agreement No 765860. Performing research work at CIEMAT – Plataforma Solar de Almería. / Deemter, RD. (2024). Application of Advanced Integrated Technologies (Membrane and Photo-Oxidation Processes) for the Removal of CECs contained in Urban Wastewater [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/203099