Ce travail de thèse vise l'étude des effets des étapes de récolte et de concentration des cellules, sur la dégradation des fonctionnalités de Lactobacillus delbrueckii subsp. bulgaricus CFL1. Cet objectif s'accompagne de l'identification des mécanismes physiologiques qui expliquent les différences observées. La mise en œuvre de conditions de stress modéré, permettant aux cellules de s'adapter au stress ultérieur de congélation, constitue le troisième volet abordé dans cette thèse. Lors de la première partie du travail, l'effet d'une acidification en fin de fermentation sur la cryotolérance des cellules a été analysé. Un plan d'expériences a permis de définir la condition optimale d'acidification (pH 5,25 pendant 30 min) induisant une adaptation des cellules. Elle conduit à une meilleure résistance à la congélation et au stockage à -20 °C. Deux mécanismes physiologiques à l'origine de cette adaptation ont été identifiés. Le premier est lié à l'augmentation de la concentration de l'acide gras membranaire C18:1. Le deuxième, caractérisé pour l'analyse du protéome cytoplasmique, correspond à une réduction du métabolisme azoté, une augmentation des métabolismes énergétique et nucléotidique, et à une synthèse plus importante de protéines de stress. Dans une deuxième étape, les cellules ont été concentrées selon différentes conditions de centrifugation (vitesse de rotation, durée et température). Celles-ci n'ont pas d'effet sur la résistance de Lb. bulgaricus CFL1 à l'étape de concentration elle-même, mais présentent un effet faible mais significatif sur leur cryotolérance. Les évolutions de la résistance des cellules à la congélation et au stockage étant opposés, l'effet des conditions de centrifugation sur les cellules stockées à long terme est cependant négligeable. La troisième partie de ce travail a permis de quantifier l'impact de la concentration des cellules par microfiltration, sur leur résistance aux différentes étapes du procédé et sur l'état physiologique de Lb. bulgaricus CFL1. Les résultats montrent que les cellules sont moins résistantes à l'étape de microfiltration qu'à la centrifugation. Par contre, la résistance à la congélation augmente significativement (entre 28 % et 88 %) selon les conditions de microfiltration appliquées, par rapport à la centrifugation. La meilleure cryotolérance a été obtenue pour une vitesse tangentielle égale à 2,01 m.s-1 et une pression transmembranaire de 0,15 MPa. Cette meilleure résistance est liée à une augmentation des teneurs en acides gras C16:0, 18:1 et cycC19:0, ainsi qu'à une réduction de la concentration en C14:0. Les résultats des analyses protéomiques montrent aussi que les cellules les plus actives et les plus résistantes voient leur métabolisme énergétique augmenter, alors que leur métabolisme général et azoté est, au contraire, réduit. Finalement, ce travail propose deux voies intéressantes pour l'adaptation de Lb. bulgaricus CFL1, en vue d'améliorer sa cryotolérance. Certaines réponses physiologiques générales induisant ces adaptations cellulaires ont pu être identifiées, aux niveaux membranaire et cytoplasmique.

Polymer flocculants, traditionally used with primary coagulant to enhance flocculation and sedimentation, are used in the coagulation-/microfiltration process as well assuming they can improve membrane performance similarly. However, there are several uncertainties concerning the use of polymer flocculants in the coagulation-microfiltration process. First, polymer flocculants may not have measurable effect on turbidity removal, because microfiltration membranes can remove significantly smaller particles than those removed by the conventional treatment process. Second, the effect of using polymer flocculants on NOM removal has been controversial. Although a number of studies reported improved NOM removal when polymers were used, others reported no or negative impact of polymers on NOM removal. Third, polymer flocculants are high molecular weight organic compounds. When carried over to membrane residual polymers can potentially foul the membranes. Finally, the use of polymer flocculants will change floc properties (i.e. size, fractal dimension, and stickiness) and subsequently bring uncertain effect on cake layer resistance. Therefore, the role of polymer flocculants in coagulation-microfiltration system needs to be carefully assessed for system optimization. In the reported research, three types of polymer flocculants with different charge and molecular weights were tested for comprehensively evaluating the impact of polymer flocculants on the performance of coagulation-microfiltration of surface water. Operation conditions such as inline filtration, direct filtration, and filtration with sedimentation were included. Two membrane reactors were designed to study the mechanism through which polymer flocculants affect the performance of coagulation-microfiltration systems. The result demonstrated that the use of polymer flocculants provides little to no benefit to turbidity and NOM removal in most cases, but pDADMACs can enhance NOM removal if applied properly; All polymer flocculants significantly increased membrane fouling except for pDADMACs when sedimentation proceeds MF; Polymer flocculants increase deposition/attachment of floc particles on the membrane surface through both adsorption of residual polymer on the membrane surface and polymer molecules on the floc particle surface; Even though polymers form larger and more fractal floc particles, they did not have notable impact on cake layer structure.

Over the past few decades there has been great interest in exploring alternatives to conventional separation methods due to their high cost and energy requirements. Membranes offer a potentially attractive alternative as they potentially address both of these points. The overarching theme of this dissertation is to design nanocomposite membranes for processes where existing separation schemes are inadequate. This dissertation focuses on three challenges: 1) designing organic-inorganic hybrid membranes for reverse-selective removal of alkanes from light gases, 2) defect-free inorganic nanocomposite membranes that have uniform pores, and 3) nanocomposite membranes for minimizing protein fouling in microfiltration applications. Reverse-selective gas separations that preferentially permeate larger/heavier molecular species based on their greater solubility have attracted considerable recent attention due to both economic and environmental concerns. In this study, dendrimer-ceramic hybrid membranes showed exceptionally high propane/nitrogen selectivities. This result was ascribed to the presence of stable residual solvent that affects the solubility of hydrocarbon species. Mesoporous silica-ceramic nanocomposite membranes have been fabricated to provide defectless mesoporous membranes. As mesoporous silica is iteratively synthesized in the ceramic macropores, the coating method and the surfactant removal step significantly affected permeance and selectivity. It was also shown that support layers can cause a lower selectivity than Knudsen limit. Membrane fouling which results from deposition and nonspecific adsorption of proteins on the membrane surface is irreversible in nature, and results in a significant decrease in the membrane performance. To address this problem, two approaches were explored: 1) control of the surface chemistry tethering alumina membranes with organic components and 2) development of a novel photocatalytic membrane that exhibits hydrophilicity and can be easily regenerated. Both approaches can offer a viable route to the synthesis of attractive membranes, in that 1) the density of protein-resistant organic groups such as PEG is controllable by changing scaffolds or synthesis conditions and 2) the photocatalytic nanocomposite membranes can open the way for a new regeneration method that is environmentally benign.

While considerable progress has been made towards understanding the effect that membrane-based layer-by-layer (LbL) immobilizations have on the activity and stability of enzymatic catalysis, detailed work is required in order to fundamentally quantify and optimize the functionalization and operating conditions that define these properties. This work aims to probe deeper into the nature of transport mechanisms by use of pressure-induced, flow-driven enzymatic catalysis of LbL-functionalized hydrophilized poly(vinyldiene) (PVDF)-poly(acrylic acid) (PAA)-poly(allylamine hydrochloride) (PAH)-glucose oxidase (GOx) membranes. These membranes were coupled in a sealed series following cellulose acetate (CA) membranes for the elimination of product accumulation within the feed-side solution during operation. At pH = 6 and T = 21oC, the enzymatic catalysis of LbL-immobilized GOx from Aspergillus niger performed remarkably well in comparison to the homogeneous-phase catalysis within an analogous aqueous solution. On average, the enzymatic turnover was 0.0123 and 0.0076 mmol/(mg-GOx)(min) for the homogeneous-phase catalysis and the LbL-immobilized catalysis, respectively. Multiple consecutive permeations resulted in replicable observed kinetic results with R2 > 0.95. Permeations taking place over the course of a three week trial period resulted in a retention of >90% normalized activity when membranes were removed when not in use and stored at -20oC, whereas the homogenous-phase kinetics dropped below 90% normalized activity in under one day.

The work described by this thesis is a comparison of pore opening geometry for true surface microfilters. True surface microfilters can be thought of as very fine sieves, with pore sizes less than 10 microns. All other types of so-called microfiltration membranes do not rely on sieving, but obtain their pore retention rating by particle collection mechanisms similar to depth filters. Particle deposition within such microfilters results in permeate flow rate dechne, for a fixed pressure filtration, or pressure drop rise, for a fixed rate filtration. The true surface microfilter pore geometnes considered were circular and slotted, and microfilters with filtering dimension of less than 10 microns were used. The slotted pore microfilters are not commercially available and had to be made in the laboratory as part of this study. The technique used was to plate nickel onto an existing substrate, thereby reducing the pore dimension until It was within the microfiltration range. The plating was by electroless nickel solution and not by galvanic means. Significant development of the electroless platmg technique led ultimately to the successful manufacture of process scale slotted surface microfilters.

Microalgas são microrganismos fotossintéticos, capazes de sintetizar uma ampla gama de produtos dependendo de sua rota metabólica. A produção de microalgas envolve as etapas de cultivo, recuperação da biomassa e obtenção dos produtos intracelulares, sendo a etapa de recuperação de biomassa um gargalo da produção. No presente estudo foi avaliado a concentração e purificação de biomassa de duas espécies de microalgas, Chlorella sp. e Dunaliella tertiolecta, através da microfiltração tangencial, nos seguintes modos de operação: reciclo total, batelada e batelada combinada com diafiltração. Também foi avaliada a disponibilidade de reuso do permeado como meio de cultivo para as microalgas. No modo de reciclo total foram testadas quatro pressões transmembranas (PTM) para Chlorella sp. e cinco pressões transmembranas para D. tertiolecta em duas velocidades tangenciais para determinação das melhores condições operacionais para as etapas posteriores de concentração e purificação, considerando o efeito dessas condições de operação sobre a integridade celular. A velocidade selecionada foi 0,6 m s-1 para o processamento das duas suspensões de microalgas e a PTM de 0,5 bar para Chlorella sp. e de 0,15 bar para D. tertiolecta. As análises de microscopia ótica, microscopia eletrônica de transmissão e na câmara Neubauer não demostraram um efeito significativo do sistema de MF sobre a estrutura celular de Chlorella sp., entretanto, para D. tertiolecta, as análises mostraram a necessidade de operar o sistema em PTM de 0,15 bar. Foi observado um baixo percentual médio de fouling, sendo de 16 % para Chlorella sp. e 6 % para D. tertiolecta para as duas velocidades tangenciais testadas. A resistência da membrana foi elevada quando comparada com a resistência devido ao fouling de ambas as suspensões de microalgas. Em modo batelada, observou-se em todos os experimentos, a completa retenção das células de microalgas pela membrana de microfiltração. O fator de concentração volumétrico médio foi de 2,6 para a suspensão de Chlorella sp. e 2,5 para a de D. tertiolecta. Na operação do sistema em modo diafiltração foi possível reduzir o teor salino em 42 % para o concentrado da Chlorella sp. e 38 % para o concentrado de D. tertiolecta. O modelo de Hermia modificado por Field foi utilizado em software EMSO para a determinação dos mecanismos de fouling, e concluiu-se que a formação de torta foi o mecanismo de fouling dominante em filtração de Chlorella sp.. Para D. tertiolecta, todos os mecanismos se ajustaram bem aos dados experimentais, indicando que os mesmos ocorreram simultaneamente. Foram propostos dois tipos de meio de cultura para o reuso da corrente de permeado: o permeado simples e o permeado enriquecido com a adição de micronutrientes. Foi possível verificar a utilização do permeado como meio de cultivo, principalmente para o cultivo de D. tertiolecta; o permeado com adição de micronutrientes apresentou maior capacidade de crescimento que o meio padrão para esta microalga. No cultivo da Chlorella sp., a concentração de biomassa alcançada utilizando o permeado simples e enriquecido foi inferior a concentração de biomassa em meio de cultivo padrão. Os resultados obtidos neste trabalho comprovaram que o processo de microfiltração apresenta-se como uma alternativa promissora na etapa de concentração e purificação de suspensões de microalgas; além disso, a corrente de permeado gerada pode ser utilizada como meio de cultivo, garantindo, desta forma, um menor consumo de água e nutrientes, melhorando a viabilidade econômica do processo. / Microalgae are photosynthetic organisms with simple structures and capable to synthesize a wide range of products depending on their metabolic route. The production of microalgae comprises the steps of cultivation, biomass recovery and extraction of intracellular products, being the stage of biomass recovery a production bottleneck. In the present study was evaluated the concentration and purification of biomass of two species of microalgae, Chlorella sp. and Dunaliella tertiolecta, by crossflow microfiltration, in the following modes of operation: total recycling, batch and batch combined with diafiltration. It was also assessed the availability of the reuse the permeate as medium for microalgae cultivation. In total recycling mode were tested four different transmembrane pressures (TMP) for Chlorella sp. and five transmembrane pressures for D. tertiolecta in two crossflow velocities to determine the proper operating conditions for the stages of concentration and purification, considering the effect of operating conditions on the cellular integrity. The selected crossflow velocity was 0.6 m s-1 for processing the two suspensions of microalgae and TMP of 0.5 bar for Chlorella sp. and 0.15 bar for D. tertiolecta. The analyses of optical microscopy, transmission electron microscopy and the Neubauer chamber demonstrated no significant effect of the operating conditions of the MF system on the cellular structure of Chlorella sp., however, for D. tertiolecta, the analysis showed the need to operate the system at lower TMP of 0.15 bar. The average percentage of fouling observed was 16 % for Chlorella sp. and 6 %. for D. tertiolecta for both crossflow velocities tested. The resistance of the membrane was elevated when compared with the resistance due to fouling for both suspensions of microalgae. In batch mode, it was observed, for all the experiments, complete retention of microalgal cells by microfiltration membrane. The average volumetric concentration factor was 2.6 for the suspension of Chlorella sp. and 2.5 for D. tertiolecta. In the operation of the system in diafiltration mode was possible to reduce the the salt content in 42 % for the Chlorella sp. and 38 % for D. tertiolecta. The model of Hermia model was used in software EMSO for the determination of fouling mechanisms, and it is concluded that the cake formation was the dominant fouling in the filtration of Chlorella sp.. For D. tertiolecta, all the mechanisms adjusted well to the experimental data, demonstrating that all mechanisms occurred simultaneously. Were proposed two different culture mediums for the reuse of the permeate stream: the plain permeate and the permeate enriched with micronutrients. It was possible to verify the ability of the permeate as cultivation medium, mainly for the D. tertiolecta; in this case, the permeate enriched with micronutrients presented greater capacity for growth when compared with the standard medium. On the other hand, for the cultivation of Chlorella sp., the biomass concentration achieved using both, the plain permeate and the enriched one was less than that achieved using the standard medium. The results obtained in this work proved that the microfiltration process is a promising alternative for the concentration and purification of suspensions of microalgae. In addition, the permeate stream generated could be used as a growth medium, ensuring thereby a less consumption of water and nutrients, improving the economic viability of the process.

O lixiviado de aterro sanitário é um efluente complexo de alta carga orgânica, composto basicamente de substâncias recalcitrantes, amônia e poluentes tóxicos. Quando descartado de forma inadequada nos corpos receptores, desempenha um papel significativo dentre os principais fatores causadores de danos ao meio ambiente. A tecnologia de separação por membranas consiste em uma alternativa atrativa no tratamento do lixiviado, pois é capaz de remover contaminantes que não são removidos por processos de tratamento convencionais. O presente estudo tem por objetivo a avaliação, em escala de bancada, do tratamento do lixiviado por processos de separação por membranas e o monitoramento de fatores de fouling e resistências nas membranas. O sistema de membrana fibra-oca de microfiltração de poli(éter-imida) foi testado a fim de promover o polimento final do tratamento do lixiviado. O resultado obtido de remoção de matéria orgânica, expressado em DQO, variou entre 14 e 43%, no entanto, esse sistema não foi eficiente na remoção de cor. Para a remoção de cor foram realizados ensaios em sistemas de osmose inversa e de eletrodiálise, no entanto, apenas o sistema de osmose inversa apresentou resultados positivos. Foi verificado que as características do lixiviado têm influencia na formação de fouling, reduzindo o fluxo de permeado e contribuindo para o aumento das resistências. O percentual médio de fouling observado foi de 53% e a resistência da membrana contribuiu com mais de 50% da resistência total do sistema. Os resultados comprovam que a implementação do sistema de membranas de microfiltração e osmose inversa, como polimento final no tratamento de lixiviado, seriam de grande valia, tanto para atender aos padrões mínimos de lançamento de efluentes previsto na legislação brasileira como para a preservação dos recursos hídricos. / Landfill leachate is a complex wastewater of high organic matter, composed basically of recalcitrant substances, ammonia and toxic pollutants. When leachate is improperly disposed in the receiving waters, it has a significant role among the main factors causing damage to the environment. The membrane separation technology is an attractive alternative in the treatment of the leachate, because it is able to remove contaminants that are not removed by conventional treatment processes. The present study aims to evaluate, using a bench scale system, leachate treatability by membrane separation processes and to monitor fouling factors and membrane resistance. The microfiltration system of hollow fiber membrane poly(ether-imide) was tested in order to promote leachate treatment. The result of organic matter removal, expressed in COD, varied between 14 and 43%, however, this system was not efficient to color removal. Tests were performed for color removal in a reverse osmosis and electrodialysis systems, however, only the reverse osmosis system showed positive results. It was found that the characteristics of leachate have influence in the fouling formation, permeate flux reducing and contributes to the resistance increase. The average percentage of fouling observed was 53% and the membrane resistance contributed more than 50% of the total resistance of the system. The results show that microfiltration and reverse osmosis systems implementation to treat the leachate would be of great importance, both to meet the minimum standards for effluent discharge as provided for in Brazilian law to the preservation of water resources.

A utilização de subprodutos provenientes da indústria de alimentos tem como objetivo agregar valor aos mesmos propiciando o desenvolvimento de novas propostas para o uso de tecnologias ainda não consolidadas pela indústria. No caso do beneficiamento de arroz polido, além da extração das proteínas dos grãos quebrados, uma nova proposta seria a extração do amido presente nestes grãos. Neste contexto, os objetivos deste trabalho são testar um método alternativo para a separação do amido do restante dos componentes do grão de arroz, o método Al-Hakkak, utilizar a microfiltração para a etapa de concentração/purificação do amido obtido e, ainda, determinar e comparar a composição e as propriedades da farinha e do amido obtido em cada etapa do processo. Foi verificado que as características da solução de amido obtida pós extração têm influência na formação do fouling, reduzindo o fluxo de permeado e contribuindo para o aumento das resistências. O percentual médio de fouling observado foi de 38%; deve-se à resistência por polarização por concentração cerca de 75% da resistência total do sistema. Já o declínio do fluxo de permeado é controlado pelo mecanismo de formação de torta. O método Al-Hakkak de extração de amido foi capaz de reduzir os teores de proteínas, lipídeos e fibra alimentar em aproximadamente 52%, 94% e 82%, respectivamente. O teor de amido diminuiu com a extração, mas aumentou durante o processo de concentração pelo PSM, resultando em percentuais que variaram de 91,59 a 93,67%. Através das imagens obtidas por MEV foi possível visualizar que não houve alteração da estrutura dos grânulos de amido, além disto, se confirmou o formato poliédrico e o tamanho dos grânulos de 3 a 6 μm. O tamanho dos grânulos também foi confirmado pela análise granulométrica. O poder de inchamento (PI) e a solubilidade (IS) dos grânulos das amostras aumentaram com o acréscimo da temperatura. As temperaturas de gelatinização (Tg) apresentaram valores variando de 71,3 a 74,4°C. / The use of by-products from the food industry aims to add value to the same stimulating the development of new proposals for using technologies not yet consolidated the industry. For the improvement of polished rice, besides the extraction of proteins from broken grains a new proposal would be the extraction of the starch present in these grains. In this context, the objectives of this study are to test an alternative method for the separation of starch from the rest of the components of the rice grain, the Al-Hakkak method using microfiltration to stage concentration/purification of starch obtained, and also determine and compare the composition and properties of flour and starch obtained at each step of the process. It was found that the characteristics of the starch solution obtained after extraction influence the formation of fouling, reducing the permeate flux and contributing to the growing resistance. The average percentage of fouling observed was 38% and is due to the concentration polarization resistance by about 75 % of the total resistance of the system. Since the decline of permeate flux is controlled by mecanism of cake block. The Al-Hakkak method for starch extraction was able to reduce the levels of proteins, lipids and dietary fiber, in approximately 52%, 94% and 82%, respectively. The amount of starch decreased after the Al-Hakkak process but increased during the concentration process by PMS, resulting in a percentage ranging from 91.59 to 93.67%. Through the images obtained by SEM was possible to see that there was no change in the structure of starch granules, moreover, confirmed the polyhedral shape and size of granules 3-6 μm. The size of the granules was also confirmed by particle size analysis. The swelling power (PI) and solubility (S) of the granules of the samples increased with increasing temperature. The gelatinization temperatures (Tg) had values ranging from 71.3 to 74.4°C.

Microalgas são microrganismos fotossintéticos, capazes de sintetizar uma ampla gama de produtos dependendo de sua rota metabólica. A produção de microalgas envolve as etapas de cultivo, recuperação da biomassa e obtenção dos produtos intracelulares, sendo a etapa de recuperação de biomassa um gargalo da produção. No presente estudo foi avaliado a concentração e purificação de biomassa de duas espécies de microalgas, Chlorella sp. e Dunaliella tertiolecta, através da microfiltração tangencial, nos seguintes modos de operação: reciclo total, batelada e batelada combinada com diafiltração. Também foi avaliada a disponibilidade de reuso do permeado como meio de cultivo para as microalgas. No modo de reciclo total foram testadas quatro pressões transmembranas (PTM) para Chlorella sp. e cinco pressões transmembranas para D. tertiolecta em duas velocidades tangenciais para determinação das melhores condições operacionais para as etapas posteriores de concentração e purificação, considerando o efeito dessas condições de operação sobre a integridade celular. A velocidade selecionada foi 0,6 m s-1 para o processamento das duas suspensões de microalgas e a PTM de 0,5 bar para Chlorella sp. e de 0,15 bar para D. tertiolecta. As análises de microscopia ótica, microscopia eletrônica de transmissão e na câmara Neubauer não demostraram um efeito significativo do sistema de MF sobre a estrutura celular de Chlorella sp., entretanto, para D. tertiolecta, as análises mostraram a necessidade de operar o sistema em PTM de 0,15 bar. Foi observado um baixo percentual médio de fouling, sendo de 16 % para Chlorella sp. e 6 % para D. tertiolecta para as duas velocidades tangenciais testadas. A resistência da membrana foi elevada quando comparada com a resistência devido ao fouling de ambas as suspensões de microalgas. Em modo batelada, observou-se em todos os experimentos, a completa retenção das células de microalgas pela membrana de microfiltração. O fator de concentração volumétrico médio foi de 2,6 para a suspensão de Chlorella sp. e 2,5 para a de D. tertiolecta. Na operação do sistema em modo diafiltração foi possível reduzir o teor salino em 42 % para o concentrado da Chlorella sp. e 38 % para o concentrado de D. tertiolecta. O modelo de Hermia modificado por Field foi utilizado em software EMSO para a determinação dos mecanismos de fouling, e concluiu-se que a formação de torta foi o mecanismo de fouling dominante em filtração de Chlorella sp.. Para D. tertiolecta, todos os mecanismos se ajustaram bem aos dados experimentais, indicando que os mesmos ocorreram simultaneamente. Foram propostos dois tipos de meio de cultura para o reuso da corrente de permeado: o permeado simples e o permeado enriquecido com a adição de micronutrientes. Foi possível verificar a utilização do permeado como meio de cultivo, principalmente para o cultivo de D. tertiolecta; o permeado com adição de micronutrientes apresentou maior capacidade de crescimento que o meio padrão para esta microalga. No cultivo da Chlorella sp., a concentração de biomassa alcançada utilizando o permeado simples e enriquecido foi inferior a concentração de biomassa em meio de cultivo padrão. Os resultados obtidos neste trabalho comprovaram que o processo de microfiltração apresenta-se como uma alternativa promissora na etapa de concentração e purificação de suspensões de microalgas; além disso, a corrente de permeado gerada pode ser utilizada como meio de cultivo, garantindo, desta forma, um menor consumo de água e nutrientes, melhorando a viabilidade econômica do processo. / Microalgae are photosynthetic organisms with simple structures and capable to synthesize a wide range of products depending on their metabolic route. The production of microalgae comprises the steps of cultivation, biomass recovery and extraction of intracellular products, being the stage of biomass recovery a production bottleneck. In the present study was evaluated the concentration and purification of biomass of two species of microalgae, Chlorella sp. and Dunaliella tertiolecta, by crossflow microfiltration, in the following modes of operation: total recycling, batch and batch combined with diafiltration. It was also assessed the availability of the reuse the permeate as medium for microalgae cultivation. In total recycling mode were tested four different transmembrane pressures (TMP) for Chlorella sp. and five transmembrane pressures for D. tertiolecta in two crossflow velocities to determine the proper operating conditions for the stages of concentration and purification, considering the effect of operating conditions on the cellular integrity. The selected crossflow velocity was 0.6 m s-1 for processing the two suspensions of microalgae and TMP of 0.5 bar for Chlorella sp. and 0.15 bar for D. tertiolecta. The analyses of optical microscopy, transmission electron microscopy and the Neubauer chamber demonstrated no significant effect of the operating conditions of the MF system on the cellular structure of Chlorella sp., however, for D. tertiolecta, the analysis showed the need to operate the system at lower TMP of 0.15 bar. The average percentage of fouling observed was 16 % for Chlorella sp. and 6 %. for D. tertiolecta for both crossflow velocities tested. The resistance of the membrane was elevated when compared with the resistance due to fouling for both suspensions of microalgae. In batch mode, it was observed, for all the experiments, complete retention of microalgal cells by microfiltration membrane. The average volumetric concentration factor was 2.6 for the suspension of Chlorella sp. and 2.5 for D. tertiolecta. In the operation of the system in diafiltration mode was possible to reduce the the salt content in 42 % for the Chlorella sp. and 38 % for D. tertiolecta. The model of Hermia model was used in software EMSO for the determination of fouling mechanisms, and it is concluded that the cake formation was the dominant fouling in the filtration of Chlorella sp.. For D. tertiolecta, all the mechanisms adjusted well to the experimental data, demonstrating that all mechanisms occurred simultaneously. Were proposed two different culture mediums for the reuse of the permeate stream: the plain permeate and the permeate enriched with micronutrients. It was possible to verify the ability of the permeate as cultivation medium, mainly for the D. tertiolecta; in this case, the permeate enriched with micronutrients presented greater capacity for growth when compared with the standard medium. On the other hand, for the cultivation of Chlorella sp., the biomass concentration achieved using both, the plain permeate and the enriched one was less than that achieved using the standard medium. The results obtained in this work proved that the microfiltration process is a promising alternative for the concentration and purification of suspensions of microalgae. In addition, the permeate stream generated could be used as a growth medium, ensuring thereby a less consumption of water and nutrients, improving the economic viability of the process.

Submitted by Maria Medeiros (maria.dilva1@ufcg.edu.br) on 2018-10-04T12:26:19Z No. of bitstreams: 1 FERNANDO ALMEIDA DA SILVA - TESE (PPGEP) 2009.pdf: 5875918 bytes, checksum: 93c5b10ae310f33943ce3b71854ef0bf (MD5) / Made available in DSpace on 2018-10-04T12:26:19Z (GMT). No. of bitstreams: 1 FERNANDO ALMEIDA DA SILVA - TESE (PPGEP) 2009.pdf: 5875918 bytes, checksum: 93c5b10ae310f33943ce3b71854ef0bf (MD5) Previous issue date: 2009-11 / Atualmente os processos de separação por membranas estão em pleno desenvolvimento. As membranas de cerâmica encontram larga aplicação, principalmente em processos cujas temperaturas de trabalho são superiores à 250 ºC, como também, na separação de soluções em que o pH seja extremamente ácido, ou até mesmo quando houver presença de solventes orgânicos no sistema. Este trabalho consiste na preparação de membranas tubulares, obtidas a partir de duas composições contendo argila, caulim e óxido de alumínio, conformadas pelo processo de extrusão, utilizando diferentes temperaturas na etapa de sinterização para uso em microfiltração. Foi feita caracterização nas massas cerâmicas antes da sinterização, através dos ensaios de análise granulométrica, análise termogravimétrica, análise química e difração de raios X. As análises químicas mostraram altos teores de SiO2 e de Al2O3 e os ensaios de difração de raios X mostraram a presença de caulinita, quartzo e óxido de alumínio em ambas as composições. Foram feitos ensaios de difração de raios X nas massas após as sinterizações e os resultados mostraram a presença de mulita, óxido de alumínio e quartzo em todas as sinterizações efetuadas. Com relação ao tamanho e a distribuição destes poros nas membranas, os resultados das micrografias e de porosimetria por intrusão de mercúrio mostraram a presença de poros em todas as temperaturas de sinterização, com dimensões na faixa de microfiltração. Os ensaios de fluxo com escoamento tangencial utilizando água dessalinizada mostraram na composição 1 que as membranas sinterizadas a 1300 ºC obtiveram maior valor. Quanto a composição 2, o maior fluxo foi obtido pela membrana sinterizada a 1150 ºC. Os valores médios dos fluxos utilizando tanto a água dessalinizada quanto a água do açude Epitácio Pessoa, encontrados nas membranas sinterizadas nas temperaturas de 1150, 1200, 1250 e 1300 ºC da composição 1 foram bem maiores que os observados nas membranas da composição 2. Com relação à aplicação das membranas no tratamento da água do açude Epitácio Pessoa, verificou-se que a turbidez da água foi reduzida de 7,1 UTN para valores próximos de zero para todas as membranas estudadas. / Membrane separation processes has experienced a great development recently. Ceramic membranes are applied in several processes, mainly in application in which temperatures are above 250 oC, as well in separation of solutions with extremely acid pH and even in systems with organic solvents. The aim of this work is to prepare tubular ceramic membranes by extrusion using two different compositions containing ball clays, kaolin and alumina and to fire in different sintering temperatures to be applied in microfiltration process. It was done the characterization of the ceramic compositions before sintering, particles size, thermogravimetrics analysis, chemicals analysis and X-ray diffraction. The chemicals analysis showed great amount of SiO2 and Al2O3 and the X-ray results showed the presence of kaolinite, quartz and alumina in the both compositions. The results from X-ray diffraction of the ceramic body after sintering showed the presence of mullite, alumina and quartz. The SEM images and the results from mercury porosimetry showed the presence of pores in all sintering temperatures and pore size in the range of microfiltration. The results from pure water flux, at steady state, showed that the membranes prepared with composition 1 and sintering at temperature of 1300 oC presented the highest value. To the membranes prepared with composition 2 and sintering temperature of 1150 oC presented the highest value. The pure water flux value of the membranes prepared with composition 1 was bigger than the membranes prepared with composition 2. In relation to the use of these membranes to water treatment from Epitácio Pessoa Dam, the results showed that the water turbidity decrease from 7.1 NTU to values close to zero for the all studied membranes.