[ES] En la presente Tesis Doctoral se investigó la aplicación del proceso de ultrafiltración (UF) y el fenómeno de ensuciamiento de las membranas en la eliminación de sustancias disueltas y coloidales (DCS) de efluentes tratados de la industria papelera (PMTE) para su reutilización en los diferentes procesos de fabricación de papel y cartón reciclado. El objetivo general de esta investigación se dividió en tres partes principales: i) describe cómo encontrar las condiciones óptimas de operación de cuatro parámetros de proceso: presión transmembrana (TMP), velocidad de flujo cruzado (CFV), temperatura y corte de peso molecular (MWCO) para maximizar el flujo promedio de permeado (Jp) y rechazo de la demanda química de oxígeno (COD) y minimizar el descenso del flujo de permeado acumulado (SFD) utilizando el método de Taguchi (Design Robusto) y utility concept aplicado a un proceso de UF a flujo cruzado, para remover DCS de efluentes tratados de la industria papelera, ii) el descenso del flujo de permeado y los mecanismos de ensuciamiento de las membranas de UF ensuciadas con PMTE se examinaron mediante modelos matemáticos semi-empíricos. Los resultados para los diferentes ensayos de UF se expresaron en términos de variación del Jp en función del tiempo para verificar la precisión del ajuste (mayor valor de R2 y menor valor de desviación estándar) de los distintos modelos de Hermia adaptados a flujo tangencial y del modelo de formación de torta en filtración a presión constante ajustados a los datos experimentales, y iii) describe métodos de identificación, caracterización y posibles orígenes de las sustancias contaminantes (foulants) en las membranas de UF. Técnicas como el análisis físico-química, FESEM, SEM-EDS, ATR-FTIR y 3DEEM se llevaron a cabo para comprender qué fracción de los contaminantes son responsables por la formación de incrustaciones en las membranas. Los resultados obtenidos durante la etapa de optimización de parámetros del procesos demostraron que TMP y MWCO tienen la mayor contribución en el Jp y SFD. En el caso de la tasa de rechazo de COD, los resultados mostraron que MWCO tiene la mayor contribución seguida de CFV. Por consiguiente, las condiciones óptimas se encontraron para el segundo nivel de TMP (2.0 bar), el tercer nivel del CFV (1.041 m/s), el segundo nivel de la temperatura (15°C) y el tercer nivel de MWCO (100 kDa). Bajo estas condiciones óptimas de operación Jp, rechazo de COD y SFD alcanzaron respuestas de 81.15 L/m2.h, 43.90% y 6.01 (alrededor de 28.96 % para (FD), respectivamente, valores dentro del rango previsto del intervalo de confianza del 95%. Además, los modelos de Hermia adaptados a UF en flujo tangencial fueron capaces de predecir con gran precisión el descenso del Jp y los mecanismos de ensuciamiento en función del tiempo para todas las membranas seleccionadas (10, 30 y 100 kDa) y bajo diferentes condiciones ensayadas de UF. Por lo tanto, los modelos que presentan un mayor grado de ajuste son el bloqueo completo de poros (coeficiente de determinación R2 >0.97) y bloqueo intermedio (R2 >0.96), seguido por el modelo de formación de torta (R2 >0.94), lo que indica que estés son los principales mecanismos de ensuciamiento de las membranas. Análisis de 3DEEM revelaron que la mayoría de la materia orgánica fluorescentes en las membranas sucias eran proteínas coloidales (componentes similares a proteínas I + II) y proteínas macromoleculares (componentes similares a SMP). Además, polisacáridos (especie celulósica) y sustancias como ácidos grasos y resinosos fueron identificadas en las membranas contaminadas mediante análisis ATR-FTIR. Por fin, análisis SEM-EDS para las membranas ensuciadas con PMTE se detectó concentración de contaminantes inorgánicos (iones metálicos multivalentes) especialmente el Ca2+ que podría acelerar la formación torta en la superficie de la membrana. / [CA] En la present Tesi Doctoral es va investigar l'aplicació del procés d'ultrafiltració (UF) i el fenomen d'embrutiment de les membranes en l'eliminació de substàncies dissoltes i col·loïdals (DCS) d'efluents tractats de la indústria paperera (PMTE) per al seu reutilització en els diferents processos de fabricació de paper i cartó reciclatge. L'objectiu general d'aquesta investigació es va dividir en tres parts principals: i) descriu com trobar les condicions òptimes d'operació de quatre paràmetres de procés: pressió transmembrana (TMP), velocitat de flux creuat (CFV), temperatura i tall de pes molecular (MWCO) per a maximitzar el flux mitjà de permeat (Jp) i rebuig de la demanda química d'oxigen (COD) i minimitzar el descens del flux de permeado acumulat (SFD) utilitzant el mètode de Taguchi (Design Robust) i utility concept aplicat a un procés de UF a flux creuat en escala pilot, per a remoure DCS d'efluents tractats de la indústria paperera (PMTE), ii) el descens del flux de permeat i els mecanismes de embrutiment (fouling) de les membranes de UF embrutades amb PMTE es van examinar mitjançant models matemàtics semi-empírics. Els resultats per als diferents assajos de UF es van expressar en termes de variació del flux de permeat (Jp) en funció del temps per a verificar la precisió de l'ajust (major valor de R2 i menor valor de desviació estàndard) dels diferents models de Hermia adaptats a flux tangencial i del model de formació de coca en filtració a pressió constant ajustats a les dades experimentals, i iii) descriu mètodes d'identificació, caracterització i possibles orígens de les substàncies contaminants (foulants) en les membranes de UF. Tècniques com l'anàlisi física-química, FESEM, SEM-EDS, ATR-FTIR i 3DEEM es van dur a terme per a comprendre quina fracció dels contaminants són responsables per la formació d'incrustacions sobre la superfície i adsorció dins dels porus de les membranes. Els resultats obtinguts durant l'etapa d'optimització de paràmetres del processos van demostrar que TMP i MWCO tenen la major contribució en el Jp i SFD. En el cas de la taxa de rebuig de COD, els resultats van mostrar que MWCO té la major contribució seguida de CFV. Per consegüent, les condicions òptimes es van trobar per al segon nivell de TMP (2.0 bar), el tercer nivell del CFV (1.041 m/s), el segon nivell de la temperatura (15°C) i el tercer nivell de MWCO (100 kDa). Sota aquestes condicions òptimes d'operació Jp, rebuig de COD i SFD van aconseguir respostes de 81.15 L/m².h, 43.90% i 6.01 (al voltant de 28.96% per a (FD)), respectivament, valors dins del rang previst de l'interval de confiança del 95%. A més, els models de Hermia adaptats a UF en flux tangencial van ser capaços de predir amb gran precisió el descens del Jp i els mecanismes de embrutiment en funció del temps per a totes les membranes seleccionades (10, 30 i 100 kDa) i baix diferents condicions assajades de UF. Per tant, els models que presenten un major grau d'ajust són el bloqueig complet de porus (coeficient de determinació R2 >0.97) i bloqueig intermedi (R2 >0.96), seguit pel model de formació de coca (R2 >0.94), la qual cosa indica que estigues són els principals mecanismes de embrutiment de les membranes. Anàlisi de 3DEEM van revelar que la majoria de la matèria orgànica fluorescents en les membranes brutes eren proteïnes col·loidals (components similars a proteïnes I + II) i proteïnes macromoleculars (components similars a SMP). A més, polisacàrids (espècie cel·lulòsica) i substàncies com a àcids grassos i resinosos van ser identificades en les membranes contaminades mitjançant anàlisis ATR-FTIR, tals substàncies exerceixen un paper important en el embrutiment de les membranes. Per fi, anàlisi SEM-EDS per a les membranes embrutades amb PMTE es va detectar concentració de contaminants inorgànics (ions metàl·lics multivalents) especialment el Ca2+ que podria accelerar la formació coca en la àrea de la membrana. / [EN] In this PhD Thesis, the application of ultrafiltration process (UF) and membrane fouling phenomenon used to remove dissolved and colloidal substances (DCS) from paper mill treated effluent (PMTE) for reuse in different recycled paper and cardboard manufacturing processes was investigated. The overall goal of this research has been divided into three main parts: i) describes how to find optimal operating conditions of four controlling parameters, such as transmembrane pressure (TMP), cross-flow velocity (CFV), temperature and molecular weight cut-off (MWCO) for maximizing the average permeate flux (Jp) and chemical oxygen demand (COD) rejection, and minimizing the cumulative flux decline (SFD) using Taguchi method and utility concept for a cross-flow UF in pilot scale, used to remove DCS from a paper mill treated effluent (PMTE), ii) flux decline and fouling mechanisms of UF membranes fouled with PMTE were examined by theoretical modelling. The results from UF tests were expressed in terms of permeate flux (Jp) as a function of time to check modified Hermia's models adapted to crossflow filtration and cake formation in constant-pressure filtration, and iii) describes the Identification, characterization and possible origins of UF membrane foulants. Techniques such as chemical analysis, FESEM, SEM-EDS, ATR-FTIR and 3DEEM analysis were applied to understand which fraction of the foulants caused the fouling. This research found that the TMP and MWCO have the greatest contribution to the average permeate flux and SFD. In the case of the COD rejection rate, the results showed that MWCO has the highest contribution followed by CFV. The optimum conditions were found to be the second level of TMP (2.0 bar), the third level of the CFV (1.041 m/s), the second level of the temperature (15°C), and the third level of MWCO (100 kDa). Under these optimum conditions Jp, COD rejection and SFD resistance of 81.15 L/m2/h, 43.90% and 6.01 (around 28.96 % of (FD), respectively, were obtained and they were within of the predicted range at the 95% confidence interval. Furthermore, the results showed that the predictions of the modified Hermia's models adapted to cross-flow UF had good agreements with experimental data, under different conditions tested for PMTE. Therefore, it can be concluded that for all cases the best fit (higher accuracy) to the experimental data corresponds to the complete (coefficient of determination R2 >0.97) and intermediate (R2 >0.96) blocking, followed by the cake layer formation (R2 >0.94). Moreover, measurements of particle size distribution and zeta potential near the isoelectric point, showed a substantial reduction in colloidal compounds. The 3DEEM analysis revealed that the majority of the organic foulants with fluorescence characteristics on the fouled membranes were colloidal proteins (protein-like substances I+II) and macromolecular proteins (SMP-like substances). Further, polysaccharide (cellulosic specie), fatty and resin acid substances were identified on the fouled membrane by the ATR-FTIR analysis and they play an important role in membrane fouling. In addition, the membrane SEM-EDS analysis showed accumulate and adsorbed onto the membrane surfaces of inorganic foulants, such as multivalent metal ions and especially Ca2+ (acts as a binding agent) that could accelerate cake layer formation on the membrane. / Santos Sousa, MR. (2020). Optimization of Operation Parameters in Ultrafiltration by Experiment Design, Mathematical Modelling and Fouling Characterization of the Membranes Used to Remove Dissolved and Colloidal Substances from a Treated Paper Mill Effluent [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/155975 / TESIS

Membrane bioreactors (MBRs) have proven to be an extremely effective wastewater treatment process combining ultrafiltration with biological processes to produce high-quality effluent. However, one of the major drawbacks to this technology is membrane fouling – an inevitable process that reduces permeate production and increases operating costs. The prediction of membrane fouling in MBRs is important because it can provide decision support to wastewater treatment plant (WWTP) operators. Currently, mechanistic models are often used to estimate transmembrane pressure (TMP), which is an indicator of membrane fouling, but their performance is not always satisfactory. In this research, existing mechanistic and data-driven models used for membrane fouling are investigated. Data-driven machine learning techniques consisting of random forest (RF), artificial neural network (ANN), and long-short term memory network (LSTM) are used to build models to predict transmembrane pressure (TMP) at various stages of the MBR production cycle. The models are built with 4 years of high-resolution data from a confidential full-scale municipal WWTP. The model performances are examined using statistical measures such as coefficient of determination (R2), root mean squared error, mean absolute percentage error, and mean squared error. The results show that all models provide reliable predictions while the RF models have the best predictive accuracy when compared to the ANN and LSTM models. The corresponding R2 values for RF when predicting before, during, and after back pulse TMP are 0.996, 0.927, and 0.996, respectively. Model uncertainty (including hyperparameter and algorithm uncertainty) is quantified to determine the impact of hyperparameter tuning and the variance of extreme predictions caused by algorithm choice. The ANN models are most impacted by hyperparameter tuning and have the highest variability when predicting extreme values within each model’s respective hyperparameter range. The proposed models can be useful tools in providing decision support to WWTP operators employing fouling mitigation strategies, which can potentially lead to better operation of WWTPs and reduced costs. / Thesis / Master of Applied Science (MASc)

Les procédés d'osmose inverse (OI) permettent la production d'eau recyclée de très haute qualité grâce à l'élimination de contaminants organiques et inorganiques et de micro-organismes. Le suivi du bon fonctionnement de ce procédé est nécessaire pour valider la rétention des virus pathogènes afin de protéger la santé des usagers. La présence de minéraux et matières organiques dans les effluents rend inévitable le colmatage des membranes lors de leur fonctionnement et diminue ainsi leur performance. Afin d'éviter et d'éliminer ces colmatages, les stations de traitements des eaux utilisent des produits chimiques. Ces derniers vont modifier les performances globales des membranes en polyamide comme par exemple la diminution de la perméabilité à l'eau, et plus particulièrement les performances de rétention des virus, or l'ensemble de ces perturbations n'est que très peu compris et donc peu maitrisé. L'abattement des virus par l'OI sur des membranes intègres ou modifiées (ex : colmatage) ont donc été déterminés en mesurant la rétention d'un virus modèle de type phage MS2 et de substituts comme les sels (mesurés par conductivité), la rhodamine-WT (R-WT) ou les sulfates. La conductivité est, en effet, la technique de contrôle standard dans les stations de traitement des eaux (échelle industrielle).Le premier objectif de ce travail est d'évaluer l'utilisation d'un autre paramètre, les matières organiques dissoutes (DOM) comme nouveau substitut de virus et de déterminer l'impact du dysfonctionnement des procédés d'OI sur l'abattement des DOM et des sels à l'échelle industrielle. Les DOM peuvent en effet également être utilisées comme indicateur de qualité des eaux en fonction de leurs compositions et de leurs concentrations. L'abattement des DOM est donc testé comme nouvelle technique de surveillance afin de distinguer les fuites des changements de performance des membranes. Il est conclu que les DOM peuvent être utilisées comme nouvelle technique de contrôle. De plus, une variation de l'abattement des DOM peut aider à identifier des fuites de manière plus robuste que par l'abattement des sels. Le deuxième objectif est de déterminer l'effet des défauts membranaires sur les abattements d'un virus modèle (phage MS2) et de quatre substituts (R-WT, DOM, sulfate et sels) à l'échelle de systèmes de laboratoire. Deux systèmes à flux longitudinal est utilisés : une membrane plane et un module à spirale. Dans un premier temps, l'effet du colmatage sur les abattements de ces différents virus et substituts est étudié. Le colmatage organique, créé en utilisant un mélange de matières organiques, a pour effet d'augmenter de plus de 0,1 log les abattements de la R-WT, des sels et des DOM. Cette augmentation générale peut être due au blocage des cavités de la membrane et/ou par la sorption des substituts sur les matières organiques.Le colmatage inorganique, créé en utilisant un mélange de sels, n'a pas d'effet sur le rejet des substituts sauf pour les sels qui montre un comportement différent entre les deux systèmes. Dans le système à membrane plane, la couche inorganique permet d'augmenter le passage des sels à travers la membrane. Par opposition, il n'y a pas d'effet sur leur abattement avec le module à spirale. Cette variation entre les deux systèmes peut être causée par la différence de configuration (module à spirale contre membrane plane). Dans un deuxième temps, l'effet du chlore (modes passif et actif) sur la rétention de ces cinq composés est mesuré. Après un contact de 9000 ppm.h de NaOCl à pH 7, la surface membranaire change chimiquement. La formation de liaison Cl dans la couche en polyamide et la rupture des liaisons NH provoquent l'augmentation de la perméabilité à l'eau et diminuent l'abattement de l'ensemble des substituts. Malgré une forte diminution de 1,2 log de l'abattement en sel, l'abattement minimum du phage MS2 reste de 3 log. / One of the major applications of reverse osmosis (RO) process is the production of high quality recycled water by providing a barrier to remove organic and inorganic contaminants as well as pathogens including viruses. In order to protect public health, validation and monitoring of the RO process integrity are necessary to ensure its correct operation. During operation a certain degree of fouling is inevitable and can reduce RO membrane performance. Thus, chemicals are often used in water treatment plants to prevent or remove the membrane fouling. However, these chemicals can modify the integrity of the polyamide layer on RO membrane overtime. Up-to-date, the impact of membrane's physical change on its virus removal efficiency cause by the chemical use during operation is still not well understood.A minimum virus removal efficiency of intact and impaired (e.g. by fouling) RO membranes can be ascertained by measuring the rejection of MS2 phage and virus surrogates such as salt as measured by conductivity, rhodamine-WT (R-WT) or sulphate. However, conductivity measurement is the only full-scale standard monitoring technique. The removal of dissolved organic matter (DOM), which has been used as an indicator of water quality, can possibly be used for this purpose.The first objective of this work was to assess the suitability of DOM as a virus surrogate and to determine the impact of process failure on salt and DOM rejection in full-scale plants. A change of the conductivity does not necessarily mean that the membrane integrity has been breached. Thus, DOM monitoring has been tested and combined with the conductivity monitoring in order to distinguish between leaks and changes in membrane performances. It was concluded that DOM could be used as new monitoring technique. Moreover, a variation of DOM rejection can help identifying leaks better than just conductivity profiling alone.The second objective was to determine the effect of membrane impairments on the rejection of one model virus (MS2 phage) and four virus surrogates (R-WT, DOM, sulphate and salt) using lab-scale RO set-ups. To this aim, two different cross-flow set-ups were used: a flat-sheet and a single 2.5” spiral-wound module.Firstly, the effects of organic fouling and scaling on the rejection of model virus and virus surrogates were studied separately. Organic fouling was created using a mix of organic foulants. The result of this study showed an increase of the rejection by more than 0.1 log for R-WT, salt and DOM. The general increase of the surrogates' rejection might be due to the blocking of cavities of the polyamide membrane and/or to the sorption of surrogates to the fouling layer, which was observed by different autopsy techniques.Scaling was created using a mix of inorganic salts in order to reconstitute the composition of a RO feed water and avoiding the presence of organic foulants. Scaling was found to have no impact on the rejection of all tested virus surrogates except for salt. Salt rejection showed a change of behaviour between different set-ups: with the 2.5” module set-up the inorganic layer led to a stabilisation of the salt rejection, whereas the salt rejection increased with the flat-sheet set-up. This could be explained by the variations of the systems configuration (i.e. spiral module versus flat-sheet, feed spacer height, etc.).Secondly, the long-term impact of membrane ageing by exposure to chlorine, either active under filtration or passive by soaking, on the rejection of the model virus and four surrogates was studied. After a contact time of 9000 ppm∙h NaOCl at pH 7, the membrane surface chemistry changed. The introduction of chlorine in the membrane chemistry and the breakage of amide bonds caused an increase of the water permeability and a decrease of the model virus and virus surrogates rejection.

Nitrogen is the major component of biosphere. Paradoxically, nitrogen pollution is the concern globally. Ammonia pollution is due to its unceasing rejection into nature such as groundwater, current water and the atmosphere. This phenomenon constitutes a threat for the humanity, land and aquatic flora, and consequently disturbs the balance of natural ecosystem. Recently, that situation has lead to develop various techniques and/or technologies for ammonia removal from municipal and industrial wastewaters. Particularly in the environmental biotechnology area, two main objectives were recently aimed in many research activities: the development of new configurations of competitive bioreactors and the monitoring of partial nitrification process, which are the fundamental basis of this thesis project. In this study, the partial ammonium oxidation process, also called nitrite route, was studied in a 60 litre jet-loop submerged membrane bioreactor pilot plant. The research was organized around six chapters. An exhaustive literature review of the state-of- art of the biological nitrification process and the membrane technologies was performed. The materials and measurement methods were presented. The colorimetric method, the chromatography analysis, the biomass estimation by the suspended solids (SS), the aggregates size measurement, the gas holdup, the gas-liquid mass transfer, the bubbles gas diameter determination, the medium rheology aspects, etc., and the complete equipment of the bioreactor were studied in detail. The plant automation functioning was also studied. Membrane module (Mitsubishi Sterapore-L) characterization was carried out and three characteristic parameters were estimated: the membrane intrinsic resistance Rm, the membrane permeability Lp and the membrane porosity εm. Estimations revealed good agreement between experimental results and theoretical methods based on the Darcys law and the Carman-Kozeny law applicable in microfiltration system. Hydrodynamics and aeration aspects were studied. The mixing in the jet-loop system was characterized by the mixing time (tmix) and the circulation time (tc), respectively. The results showed that the characteristic times (tmix and tc) decrease with an increase in input gas flowrate and the circulated liquid flowrate. A model correlation involving the air and the combined liquid effects was proposed to describe the circulation time evolution. The classical non-steady state clean water test was used to determine the gas-liquid mass transfer coefficient (kLa). It was found to be influenced by the combined action of air and recirculated-liquid flowrates and a correlation has been proposed to describe their influence. The interpretation of kLa results and the system mixing data showed that the developed reactor corresponds to a near perfect mixing tank. This criterion was satisfactorily verified by literature data. The gas holdup (εg) was directly measured by the volume expansion method. In the absence of liquid circulation, εg ranged between 1 and 4% for the investigated range of gas liquid superficial velocities. It was found to increase linearly with the air superficial velocity, which corresponds to the bubbly flow regime. However, in the presence of liquid flowrate, εg slightly increased (from 1 to 6%) with increase in the superficial liquid velocity. A model has been proposed to correlate εg and the air and the recirculated-liquid velocities. The average diameter of the bubbles gas (dB) in the system was also estimated by the Leibson theoretical model based on the Reynolds number at the orifice of the gas distributor. Finally, biological aspects were studied. Respirometry measurements were conducted to characterize the process medium. The mass transfer, the gas holdup and the medium viscosity were determined. The obtained data allowed estimating the α factor and the β factor, respectively. The interaction of the growth of microorganisms into the process and the membrane performance was also investigated and a correlation model was proposed to describe membrane fouling with time. The optimal conditions for ammonium partial oxidation were determined using process monitoring and simulation. Dissolved oxygen (DO), temperature (T) and hydraulic retention time (HRT) were selected to achieve a high nitrite accumulation in the system. The results obtained showed that the selected parameters should be fixed at DO ≈ 2 mgO2.l-1, HRT ≈ 6 7 h and T = 30°C, respectively. The partial nitrification was simulated by the use of the TwoPopNitrification model included into the BioWin 2.2 software. For these simulations, a sequencing ammonia oxidation assumption was adopted: the nitrozation followed by the nitration step, respectively. The corresponding kinetics and stoichiometric constants were estimated by combining literature data and experimental nitrification results. For these estimates, the ammonium oxidation was monitored on several process samples taken at different times. The estimates were also delivered by monitoring the ammonium oxidation on the process operated in the batch mode. The plotting of simulations and experimental results revealed good agreement. In order to investigate the process performance in terms of biological stability, a long time period (≈ 600 days) was simulated. The results showed that a high stable nitrite accumulation (> 95%) could be achieved when the above optimal conditions are imposed to the system. However, after a long time, the accumulated nitrite is converted into nitrate and then the system is disrupted. For the simulated experimental conditions, the process disruption period was located between 180 and 350 days. At this period, a corresponding theoretical purge flowrate was found to range between 0.15 10-3 m3.d-1 and 3.0 10-3 m3.d-1. Simulations also showed that increasing the purge flowrate decreases the sludge retention time and then favours nitrite accumulation into the process. That is an interesting strategy to increase the performance of the biological partial nitrification process.

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The most significant environmental problems related to the food industry is water consumption and pollution, energy consumption and waste production. Most of the water that does not become a part of the products ultimately leaves plants in the form of wastewater, which is often very specific and requires adequate handling / treatment / disposal. For the purpose of this thesis, brewery industry was chosen, because of its very long tradition in the Czech history and culture. Anaerobic technologies are applied for still wider range of industrial wastewater treating. In general anaerobic membrane bioreactors (AnMBRs) can very effectively treat wastewater of different concentration and composition and produce treated water (outlet, permeate) of excellent quality, that can be further utilised. At the same time, it can promote energy self-sufficiency through biogas production usable in WWTPs / plants. Main disadvantages include unavoidable membrane fouling and generally higher CAPEX / OPEX. Within the framework of Ph.D. studies and related research activities, immersed membrane modules for anaerobic applications were selected and lab-scale tested (designed and assembled laboratory unit), an AnMBR pilot plant was designed, built and subsequently tested under real conditions - at Černá Hora Brewery WWTP (waste waters from the brewery and associated facilities). The pilot AnMBR and the technology itself has been verified over more than a year (5/2015 – 11/2016) of trial operation - the initial and recommended operational parameters have been set up, minor construction adjustments / modifications and measurement & regulation optimizations have been made, the recommended membrane cleaning and regeneration procedure has been verified. Last, but not least, conclusions and recommendations of the trial operation were summarised - some key findings and recommendations for further operation, use and modifications of the existing AnMBR pilot plant are presented.

Membrane filtration processes are widely utilized across different industrial sectors for biological and environmental separations. Examples of the former are sterile filtration and protein fractionation via microfiltration (MF) and ultrafiltration (UF) while drinking water treatment, tertiary treatment of wastewater, water reuse and desalination via MF, UF, nanofiltration (NF) and reverse-osmosis (RO) are examples of the latter. A common misconception is that the performance of membrane separation is solely dependent on the membrane pore size, whereas a multitude of parameters including solution conditions, solute concentration, presence of specific ions, hydrodynamic conditions, membrane structure and surface properties can significantly influence the separation performance and the membrane’s fouling propensity. The conventional approach for studying filtration performance is to use a single lab- or pilot-scale module and perform numerous experiments in a sequential manner which is both time-consuming and requires large amounts of material. Alternatively, high-throughput (HT) techniques, defined as the miniaturized version of conventional unit operations which allow for multiple experiments to be run in parallel and require a small amount of sample, can be employed. There is a growing interest in the use of HT techniques to speed up the testing and optimization of membrane-based separations. In this work, different HT screening approaches are developed and utilized for the evaluation and optimization of filtration performance using flat-sheet and hollow-fiber (HF) membranes used in biological and environmental separations. The effects of various process factors were evaluated on the separation of different biomolecules by combining a HT filtration method using flat-sheet UF membranes and design-of-experiments methods. Additionally, a novel HT platform was introduced for multi-modal (constant transmembrane pressure vs. constant flux) testing of flat-sheet membranes used in bio-separations. Furthermore, the first-ever HT modules for parallel testing of HF membranes were developed for rapid fouling tests as well as extended filtration evaluation experiments. The usefulness of the modules was demonstrated by evaluating the filtration performance of different foulants under various operating conditions as well as running surface modification experiments. The techniques described herein can be employed for rapid determination of the optimal combination of conditions that result in the best filtration performance for different membrane separation applications and thus eliminate the need to perform numerous conventional lab-scale tests. Overall, more than 250 filtration tests and 350 hydraulic permeability measurements were performed and analyzed using the HT platforms developed in this thesis. / Thesis / Doctor of Philosophy (PhD) / Membrane filtration is widely used as a key separation process in different industries. For example, microfiltration (MF) and ultrafiltration (UF) are used for sterilization and purification of bio-products. Furthermore, MF, UF and reverse-osmosis (RO) are used for drinking water and wastewater treatment. A common misconception is that membrane filtration is a process solely based on the pore size of the membrane whereas numerous factors can significantly affect the performance. Conventionally, a large number of lab- or full-scale experiments are performed to find the optimum operating conditions for each filtration process. High-throughput (HT) techniques are powerful methods to accelerate the pace of process optimization—they allow for multiple experiments to be run in parallel and require smaller amounts of sample. This thesis focuses on the development of different HT techniques that require a minimal amount of sample for parallel testing and optimization of membrane filtration processes with applications in environmental and biological separations. The introduced techniques can reduce the amount of sample used in each test between 10-50 times and accelerate process development and optimization by running parallel tests.