Over 18 billion barrels of waste fluids are generated annually from oil and gas production in the United States. As a large amount of water is used for oilfield operations, treating and reusing produced water can cut the consumption of fresh water in well sites. This research has helped to develop a membrane process train for a mobile produced water treatment unit for treating oilfield produced brine for reuse. To design the process train, over 30 sets of combination tests at pilot laboratory scale were performed using pretreatment, microfiltration and nanofiltration processes. Membrane performance was selected based on high flux separation efficiency, high tolerance for solids and fluid treatments. Over 95 % solids rejection and greater than 80 % oil removal efficiency were obtained in all these tests. Process train (pre-treatment and membrane) performance was monitored by chemical analysis of permeate and models fitting experimental data for the process. From the results, hydrocarbon rejection was analyzed; total organic carbon rejection was 47.9 %, total carbon content averaged 37.3 % rejection and total inorganic carbon rejection was at 3.66 %. BTEX removal efficiency ranged from 0.98 % to 52.7 % with the progressive pretreatment methods of using cartridge filters. The nanofiltration membrane showed significant reduction in total dissolved solids and in both anionic and cationic species. The process train is seen to follow a sequence of treatment from cartridge and oil removal filter treatment to microfiltration treatment to ultrafiltration, followed by nanofiltration for the purpose of this research. Further research still needs to be done on to determine the kind of analytical test which will give real time feedback on effectiveness of filters. In summary, the process train developed by TAMU-GPRI possesses distinct advantages in treating oilfield produced brine using membrane technology. These advantages include high quality of permeate, reduced sludge and the possibility of total recycle water systems. The small space requirement, moderate capital costs and ease of operation associated with the use of the mobile unit membrane technology also makes it a very competitive alternative to conventional technologies.

This study was to investigate theory and application of Osmotic Distillation (OD). OD is a new novel membrane separation process used for the concentration of aqueous solutions such as fruit juices without the application of heat. The present work was undertaken to investigate flux limitations focusing on feedside, membrane and stripper side characteristics of OD. Once the limiting areas were identified, further studies were undertaken to determine methods of minimizing those limitations without losing the quality and integrity of the liquid feed. A laboratory scale OD system was used to simulate the industrial process which takes place during the production of grape juice concentrate for the fruit juice industry. Results of a UF pretreatment study showed that the use of UF membranes with pore diameters of 0.1 fÝm or less as a pretreatment for the subsequent OD of grape juice resulted in significant increases in OD flux over that observed for juice not subjected to UF. The study of the physical properties of the feed played an important role in the explanation of the OD process. The increase in OD flux was attributed to a reduction in juice viscosity as the result of the removal of protein and other high molecular weight components. Apart from an increase in OD flux, UF pretreatment of the grape juice proved to be beneficial in other areas of the OD process. HPLC measurements showed that the normal concentration of fermentable sugars in standard 68 oBrix concentrate can be achieved at a lower Brix value in feed subjected to UF pretreatment, further reducing the need to handle highly viscous feeds. UF pretreatment also resulted in an increase in juice surface tension consequently reducing the tendency for membrane wet-out to occur. The study of the deoxygenation of the feed solution shows that the removal of dissolved gases by the pre boiling method and the perstraction with chemical reaction (PCR) method both had a positive affect on OD flux. Pre boiling the brine resulted in an indirect reduction in dissolved oxygen in the feed. Pre boiling both the feed and brine, further increased the flux. Throughout the PCR study, it was evident that stripper side mass transfer of O2 was not limited by flowrate but was limited by higher stripper concentration. However, the latter had an insignificant effect when the sulfite-oxygen reaction was catalysed. The use of a catalyst and increase in temperature gave a significant improvement in overall mass transfer coefficient. Ten types of hydrophobic microporous membranes were tested for their influence on OD flux. While the pore diameter is a considerable factor in mass transport of gases through the membrane, it was also noted that the type of membrane material used had an affect on the overall mass transfer. All top three performing membranes had pore diameters of 0.2 x 10-6 m and were made from polytetrafluoroethylene (PTFE). The choice of brine to use as the stripper was based on criteria that were confirmed by the brine studies performed here. The best performing stripper solutions demonstrating the greatest improvement in OD flux over the most commonly used brines, NaCl, CaCl2 and CH3COOK were aqueous solutions of potassium salts of phosphoric acid, pyrophosphoric acid and blends thereof. These salts agreed with all the required characteristics of a suitable brine, demonstrating high solubility rates, supporting the ability to lower water vapour pressure. The study of the corrosion effects of brine salts confirmed the phosphate salts are superior demonstrating some of the lowest corrosion rates and highest pH.

A indústria têxtil utiliza elevados volumes de água em seus processos, principalmente na etapa de tingimento, em que são utilizadas também quantidades elevadas de corantes e auxiliares têxteis. A presença desses produtos no efluente gera um efeito prejudicial e claramente visível ao ambiente, pois causam alteração nos parâmetros da qualidade da água do corpo receptor. O presente estudo apresenta o pós-tratamento de um efluente têxtil, objetivando o reciclo deste efluente para água de processo de tingimento. Para isso foi utilizada uma combinação de processo físico-químico de coagulação/floculação (CF) e processo de separação por membrana (PSM) de Ultrafiltração (UF) e Osmose Inversa (OI). Os parâmetros analisados antes e após os tratamentos foram: turbidez, condutividade elétrica, demanda química de oxigênio (DQO), carbono orgânico total (COT) e cor. Na etapa de CF foram testados dois tipos de coagulantes, o Sulfato de Alumínio e o Cloreto Férrico, nas concentrações de 30, 50, 70 e 100 mg.L-1. Foram testadas três concentrações de floculante comercial: 0,2, 0,3 e 0,4 mg.L-1. Os experimentos foram conduzidos em pH 7. As etapas de PSM foram conduzidas em módulo plano de Ultrafiltração e em módulos plano e espiral na membrana de Osmose Inversa. O melhor desempenho foi obtido com a dosagem de 50 mg.L-1 do coagulante cloreto férrico e a de 0,3 mg.L-1 de floculante comercial, que apresentou uma redução de 98% na turbidez com relação ao efluente de alimentação. No PSM de Ultrafiltração a remoção de cor não foi satisfatória por ainda apresentar coloração. No PSM de Osmose Inversa com o módulo plano o objetivo da remoção de cor foi atingido com sucesso na análise visual, porém, a vazão de permeado mostrou-se muito baixa inviabilizando o processo. No PSM de Osmose Inversa em módulo espiral a cor foi removida com sucesso, a turbidez ficou abaixo de 1 NTU, a DQO ficou abaixo do limite de detecção do equipamento e a vazão de permeado foi satisfatória. Assim, o estudo aponta como resultado a aplicação CF combinado à OI no tratamento eficaz deste efluente. / The textile industry uses large volumes of water in their processes, especially in the dyeing step, which are also used large quantities of coloring agents and textile auxiliaries. The presence of these products in the effluent generates a harmful effect and clearly visible to the environment because they cause changes in the parameters of the receiving body of water. This paper presents the post-treatment effluent from a textile industry, in order to recycle it as process water for dyeing. A combination of physico-chemical process were carried out applying coagulation / floculation (CF) and Ultrafiltration (UF) membrane separation process (MSP) and reverse osmosis (RO). The parameters analyzed before and after treatments were: turbidity, electrical conductivity, chemical oxygen demand (COD), total organic carbon (TOC) and color. In CF stage two types of coagulants were tested, aluminum sulphate and ferric chloride at concentrations of 30, 50, 70 e 100 mg.L-1. Three concentrations of commercial floculants were evaluated: 0,2, 0,3 e 0,4 mg.L-1. The experiments were conducted at pH 7. MSP steps were conducted in plan Ultrafiltration module, and in the Reverse Osmosis membrane, plan and spiral modules were tested. The best performance was obtained with a dosage of 50 mg.L-1 of the coagulant ferric chloride and 0.3 mg.L-1 commercial flocculant, which showed a 98% reduction in turbidity in respect to the raw effluent. MSP Ultrafiltration color removal was not satisfactory because color was still present. In MSP Reverse Osmosis using the plan module the goal of color removal was successfully achieved in the visual analysis, however, the membrane flow was extremely low compared with the UF permeate flow and prevented the process. The color in MSP Reverse Osmosis spiral module has been successfully removed, the turbidity was below 1 NTU, the COD was below the detection limit of the the equipment and the permeate flow was satisfactory. In this way, the study showed the best application for this effluent is CF combined with RO.

Les procédés de réutilisation des eaux usées doivent être robustes, fiables et rentables pour que leur utilisation se démocratise et devienne complémentaire des traitements des eaux de surface. Le couplage d’un procédé biologique et de procédés membranaires représente une solution prometteuse pour répondre à ces challenges. Cette étude se focalise sur l’impact des conditions de fonctionnement du procédé secondaire (en particulier par bioréacteur à membrane BAM) sur le colmatage du procédé tertiaire de nanofiltration (NF) ou d’osmose inverse (OI) ainsi que sur le devenir des micropolluants et microorganismes tout au long de la chaine de traitement. Dans un premier temps, des expériences à court terme de filtration avec différentes membrane NF et d’OI ont été réalisées afin de caractériser les interactions entre effluents secondaires et membranes. Il a ainsi été observé de très fortes rétentions de tous les micropolluants ciblés par la Directive Cadre Européenne. En termes de colmatage, la chute de flux de l’OI, essentiellement liée pour ces essais de courte durée à une augmentation de pression osmotique puis à un dépôt de cristaux minéraux, peut être maîtrisée en contrôlant le pH et la concentration en carbonate et phosphate de l’effluent secondaire. Par ailleurs, des chutes de flux plus importantes sont observées lors des filtrations réalisées avec les membranes de NF qui sont plus sensibles au colmatage irréversible. Dans un second temps, l’optimisation de la filière de traitement des eaux usées urbaines couplant un bioréacteur à membranes à un procédé d’OI a été réalisée à partir d’une unité pilote fonctionnant en continu. La sélection de conditions opératoires adéquates a permis de faire fonctionner le procédé d’OI pendant plus de quatre mois sans qu’aucune maintenance ne soit réalisée. Une faible chute de flux de l’OI, linéaire sur toute la période de filtration, essentiellement dû à l’adsorption de molécules organiques à la surface de la membrane, a été observée. Sur l’ensemble de la période d’essais, la filière BAM/OI permet d’obtenir un abattement optimal en micropolluants présents. Lorsque des micropolluants sont injectés à des concentrations plus élevées (simulation d’une brusque dégradation de la qualité des eaux en entrée de filière) dans le bioréacteur, une chute de l’activité de la biomasse couplée à un relargage de produits microbiens solubles peut être observée. Néanmoins, ces pics de pollution n’ont eu aucun impact sur le colmatage de la membrane du BAM ni sur celle de l’OI. La filière BAM-OI permet donc de garantir un taux de rejet élevé et une productivité d’environ 15 L.h-1.m2 quelles que soient les fluctuations de la composition de l’eau usée urbaine à traiter. / In order to be competitive compare to surface water treatments, wastewater reuse needs robust, reliable and profitable combination of technologies. The combination of bioreactors and membrane processes seems to be a promising solution to these challenges. This study focus on the impact of the operating conditions of the secondary treatment (particularly the membrane bioreactor (MBR)) on the nanofiltration (NF) and reverse osmosis (RO) tertiary treatments as well as the fate of micropollutants and microorganisms along the treatment line. Firstly, short term filtration experiments with various NF and RO membranes were performed in order to characterize the interactions between secondary treatment effluents (STE) and membranes. High retentions of micropollutants listed by the European water framework directive were observed. During these short term experiments, RO flux decline is mainly due to an increase of osmotic pressure and then a precipitation of salts that can be solved by controlling the pH and thus the carbonate and phosphate concentration of the STE. In addition, higher flux declines are observed with NF because of a higher irreversible fouling behavior. Secondly, continuous long term tests were performed on a pilot unit combining a MBR and a RO processes. The appropriate selection of operating conditions allowed treating wastewater during more than four months without any maintenance. A linear low flux decline, mainly due to adsorption of organic molecules at the membrane surface was observed. During this filtration period, the MBR/RO process presented very high micropollutant retentions. When micropollutants are injected at higher concentration (simulation of sudden fluctuation of feed composition) into the MBR, a drop of biomass activity combined with soluble microbial products release can be observed. Nevertheless, these peaks of pollution did not cause any additional fouling of MBR as well as RO membranes. MBR/RO process is then a reliable technology that can guaranty high retention and productivity (around 15 L.h-1.m-2) whatever the fluctuations of the feed composition.

Abstract Blackcurrants (Ribes nigrum L.) are widely consumed due to their favourable taste and health-promoting effects. The berries and extracts from different parts of the plant show anticarcinogenic, antioxidative and anti-inflammatory properties, and are effective in reducing the risk of cardiovascular disease and in promoting brain health. These health-promoting benefits are due to high concentrations of valuable compounds such as anthocyanins and flavonols in blackcurrants. However, these compounds are sensitive to heat and processing and some are lost when the berries are processed into products such as jams, purees and juices. Industrial processing of juices is a multistep process that typically includes enzyme treatment, pressing, pasteurisation, clarification and usually also thermal concentration. Alternative minimal processing technologies are required to preserve the health-promoting compounds in products by avoiding the use of high temperatures and extensive clarification. Integrated membrane technology, i.e. combined ultrafiltration and reverse osmosis, was used in this thesis for the production of blackcurrant juice concentrate. Pre-treatment methods, such as enzymatic treatment, ultrafiltration, enzymatic treatment combined with ultrafiltration and centrifugation to increase the filtration efficiency in reverse osmosis were evaluated. Processing was modelled to define the resistances, using the resistance-in-series model. The preservation and concentration of anthocyanins and flavonols were analysed. The results indicated that the main resistance in the reverse osmosis process was polarisation resistance, while membrane resistance was lower and fouling resistance was one order of magnitude lower than the other resistances. The filtration efficiency results showed that the highest flux was achieved by ultrafiltered blackcurrant juice, but that the resulting juices were substantially lower in anthocyanins and flavonols, which were retained on the ultrafiltration membrane. Therefore, replacing ultrafiltration with centrifugation as the clarification method for juices is recommended. Value-added processing of blackcurrant was conceptualised by valorisation of the marc left in the berry pressing process for extraction of anthocyanin compounds. Conventional extraction was compared with microwave-assisted extraction (MAE), with the latter optimised using response surface methodology to achieve maximum efficiency in extracting anthocyanins. The optimum parameters found for MAE were: microwave power 700 W, extraction time 10 minutes, pH 2 adjusted with hydrochloric acid and a solid to solvent ratio of 0.05. Conventional extraction showed the best results when carried out at 80 °C for 300 minutes in aqueous solution with pH 2 adjusted by hydrochloric acid. Under these conditions, recovery of anthocyanins was still 10% lower than with MAE for only 10 minutes of extraction time. / Tiivistelmä Mustaherukoita käytetään paljon niiden hyvän maun ja terveyttä edistävien vaikutusten ansiosta. Marjoilla ja marjakasvin eri osien uutteilla on osoitettu olevan antikarsinogeenisia, antioksidatiivisia ja tulehduksia estäviä ominaisuuksia ja ne ovat tehokkaita pienentämään sydän- ja verisuonisairauksia. Ne edistävät myös aivojen terveyttä. Marjojen arvokkailla yhdisteillä kuten antosyanideillä ja flavonoleilla on terveyttä edistäviä vaikutuksia. Mustaherukassa on runsaasti näitä yhdisteitä. Hillojen, soseiden ja mehujen prosessoinnissa menetetään näitä hyödyllisiä yhdisteistä, koska ne ovat herkkiä lämmölle ja prosessoinnin vaikutuksille. Mehujen prosessoinnissa käytetään entsyymikäsittelyjä, puristusta, pastörointia, selkeytystä ja usein myös lämpökonsentrointia. Tuotteiden terveyttä edistävien yhdisteiden säilyttämiseksi tarvitaan uudenlaisia hellävaraisia prosessointitekniikoita ilman korkeita lämpötiloja ja voimakasta selkeyttämistä. Tässä työssä tutkittiin yhdistettyjen kalvotekniikoiden kuten ultrasuodatuksen ja käänteisosmoosin käyttöä mustaherukkatiivistemehun prosessoinnissa. Esikäsittelymenetelmiä, mm. entsyymikäsittelyä, ultrasuodatusta, entsyymikäsittelyn ja ultrasuodatuksen yhdistelmää sekä sentrifugointia, arvioitiin käänteisosmoosin suodatustehokkuuden parantamisessa. Suodatusvastuksen määrittämiseksi prosessi mallinnettiin käyttäen sarja -vastus mallia. Antosyanidien ja flavonolien säilyminen ja konsentroituminen prosesseissa määritettiin. Tulokset osoittivat, että suurin vastus käänteisosmoosissa aiheutui polarisaatiovastuksesta, kun taas kalvon vastus oli pienempi. Mallinnus osoitti myös, että likaantumisen aiheuttama vastus oli yhtä magnitudia alhaisempi kuin muut vastukset. Suodatusteho osoitti, että suurin virtaus saavutettiin ultrasuodatetulla mustaherukkamehulla. Ultrasuodatetussa mehussa oli kuitenkin huomattavasti vähemmän antosyaniineja ja flavonoleja, mikä johtui näiden yhdisteiden tarttumisesta ultrasuodatuskalvoon. Näin ollen, tämän työn tulokset suosittelevat ultrasuodatuksen korvaamista sentrifugoinnilla mehun kirkastusprosessissa. Mustaherukkamehun tuotannossa muodostuu sivutuotteena ns. puristekakkua, joka sisältää runsaasti antosyaaneja. Työssä kehitettiin antosyaanien talteenottoa tästä sivutuotteesta vertaamalla tavanomaista uuttotekniikkaa mikroaaltoavusteiseen uuttoon. Prosessi optimoitiin vastepintamenetelmällä mahdollisimman suuren antosyaanien uuttotehokkuuden saavuttamiseksi. Optimaaliset parametrit saatiin mikroaaltoavusteisessa uutossa teholla 700 W, uuttoajalla 10 minuuttia, kiintoaines-liuotin -suhteella 0,05 pH-arvossa 2, mikä saavutettiin lisäämällä suolahappoa. Tavanomaisessa uutossa parhaat antosyaanisaannot saavutettiin suolahappo-vesiliuoksella pH-arvossa 2 uuttamalla 300 minuuttia lämpötilassa 80 °C. Antosyaanisaanto oli kuitenkin tavanomaisessa uutossa optimiolosuhteissa 10% pienempi kuin mikroaaltoavusteisessa uutossa 10 minuutin uuttoajalla.

L'objectif de ce travail de recherche est l'étude du transport des ions et des molécules d'eau à travers de membranes bicouche lipidique et des membranes polymériques. Dans une première partie, ce transport a été réalisé à travers des systèmes synthétiques auto-organisés, dont la sélectivité est en étroite relation avec le type d'architecture supramoléculaire formée grâce à des liaisons faibles. Le but est d'obtenir des systèmes qui peuvent imiter les fonctions de transport des protéines membranaires. Ce mimétisme fonctionnel est obtenu par l'auto-assemblage de molécules organiques contenant le cycle imidazole et la fonction urée, qui peuvent s'auto-assembler et créer des voies sélectives de transport des ions. Pour créer l'équivalent de la membrane cellulaire, nous avons utilisé des vésicules lipidiques unilamellaires. Ensuite, nous avons déterminé une relation entre l'activité des composés et leur structure. Pour ce faire, le transport des ions est étudié à l'aide d'une méthode de spectroscopie de fluorescence, et le transport d'eau par diffusion dynamique de la lumière utilisant la technique de « stopped flow ». Le but de la deuxième partie est la fabrication et la caractérisation des nouvelles membranes composites sous forme de couches minces, qui permettraient un bon compromis entre le flux d'eau et le rejet de sel. Dans ce cadre, la synthèse d'une série d'hydrazides en tant que précurseurs moléculaires a été réalisée, pour remplacer la métaphenylène diamine (MPD) classiquement utilisée. Ici aussi les liaisons hydrogène jouent un rôle important, car le principe de la séparation repose sur la création d'une organisation interne hautement réticulée. Les polymères synthétisés par polymérisation interfaciale ont été caractérisés par des méthodes de spectroscopie infrarouge, analyses thermogravimétriques et diffraction des rayons X. Les membranes composites ont été caractérisées par microscopie électronique à balayage, microscopie à force atomique et mesures d'angle de contact. Les performances membranaires ont été testées en filtration frontale d'eau et de solutions salines. / The aim of this work is the study of ion and water transport either across bilayer membranes or polymeric membranes used for reverse osmosis. In the first part, this transport through self-assembled synthetic systems was studied; the transport selectivity is in strong relation with the supramolecular structure, formed by weak intra and intermolecular bonds. Ion transport is studied by fluorescence spectroscopy and water transport is studied by light scattering using “stopped flow” technique. The objective is to obtain systems that could imitate transport functions of biomolecules as transmembrane proteins. This functional mimicry is achieved through self-assembly of organic molecules containing imidazole cycle and urea function that can self-assembly and form selective pathways for ion transport. To create the equivalent of the cell membrane, we used unilamellar lipid vesicles. Then, we determined a structure - transport activity relationship for a series of synthesized compounds. For the second part of this work we described the fabrication and the characterization of new thin film composite membranes for water desalination that can present a good balance between permeability and salt rejection. A series of hydrazides as molecular precursors was synthesized in order to replace the metaphenylene diamine (MPD), classically used. Again, hydrogen bonds play an important role, because the rejection is due to a high cross-linking. The polymers synthesized by interfacial polymerization were characterized by infrared spectroscopy, thermogravimetric analysis, and X-Ray diffraction. The membrane films were characterized by scanning electron microscopy, atomic force microscopy and contact angle measurements. Membrane performances were then tested in cross-flow filtration of water and saline solutions.

O objetivo deste estudo foi analisar o desempenho de um sistema de captação e tratamento de água do rio Sarapuí, por meio de uma estação de tratamento composta por um sistema de pré-tratamento convencional, ligado a um sistema de separação por membranas de osmose inversa, no Município de Belford Roxo RJ, instalado para fornecer água de processo a instalações industriais. Foi verificado que a água captada encontra-se em condição bastante degradada e que a unidade de tratamento removeu, em média, 97% do teor dos poluentes presentes na água, enquadrando-a nos parâmetros requeridos pelo processo industrial. Foi possível comprovar que o processo de separação por osmose inversa pode ser utilizado em escala industrial, proporcionando ganhos econômicos consideráveis, além de evitar o consumo de água potável para fins de processos industriais e, ainda, contribuir para a retirada de carga orgânica de uma fonte degradada / The objective of this study was to analyze the performance of a system to capture and treat water from Sarapuí river through a treatment system consisting of a conventional pré-treatment stage, linked to a reverse osmosis separation system membranes, in the city of Belford Roxo - RJ, installed to provide process water for industrial plants. It was found that the water is captured in highly degraded condition and the treatment plant removed an average of 97% of the pollutants in the water, fitting the parameters required by the industrial process. It could be demonstrated that the separation process by reverse osmosis can be used on an industrial scale, providing significant economic gains, and avoid the consumption of potable water for industrial processes and also contribute to the removal of organic pollutants from a degraded source

A indústria têxtil utiliza elevados volumes de água em seus processos, principalmente na etapa de tingimento, em que são utilizadas também quantidades elevadas de corantes e auxiliares têxteis. A presença desses produtos no efluente gera um efeito prejudicial e claramente visível ao ambiente, pois causam alteração nos parâmetros da qualidade da água do corpo receptor. O presente estudo apresenta o pós-tratamento de um efluente têxtil, objetivando o reciclo deste efluente para água de processo de tingimento. Para isso foi utilizada uma combinação de processo físico-químico de coagulação/floculação (CF) e processo de separação por membrana (PSM) de Ultrafiltração (UF) e Osmose Inversa (OI). Os parâmetros analisados antes e após os tratamentos foram: turbidez, condutividade elétrica, demanda química de oxigênio (DQO), carbono orgânico total (COT) e cor. Na etapa de CF foram testados dois tipos de coagulantes, o Sulfato de Alumínio e o Cloreto Férrico, nas concentrações de 30, 50, 70 e 100 mg.L-1. Foram testadas três concentrações de floculante comercial: 0,2, 0,3 e 0,4 mg.L-1. Os experimentos foram conduzidos em pH 7. As etapas de PSM foram conduzidas em módulo plano de Ultrafiltração e em módulos plano e espiral na membrana de Osmose Inversa. O melhor desempenho foi obtido com a dosagem de 50 mg.L-1 do coagulante cloreto férrico e a de 0,3 mg.L-1 de floculante comercial, que apresentou uma redução de 98% na turbidez com relação ao efluente de alimentação. No PSM de Ultrafiltração a remoção de cor não foi satisfatória por ainda apresentar coloração. No PSM de Osmose Inversa com o módulo plano o objetivo da remoção de cor foi atingido com sucesso na análise visual, porém, a vazão de permeado mostrou-se muito baixa inviabilizando o processo. No PSM de Osmose Inversa em módulo espiral a cor foi removida com sucesso, a turbidez ficou abaixo de 1 NTU, a DQO ficou abaixo do limite de detecção do equipamento e a vazão de permeado foi satisfatória. Assim, o estudo aponta como resultado a aplicação CF combinado à OI no tratamento eficaz deste efluente. / The textile industry uses large volumes of water in their processes, especially in the dyeing step, which are also used large quantities of coloring agents and textile auxiliaries. The presence of these products in the effluent generates a harmful effect and clearly visible to the environment because they cause changes in the parameters of the receiving body of water. This paper presents the post-treatment effluent from a textile industry, in order to recycle it as process water for dyeing. A combination of physico-chemical process were carried out applying coagulation / floculation (CF) and Ultrafiltration (UF) membrane separation process (MSP) and reverse osmosis (RO). The parameters analyzed before and after treatments were: turbidity, electrical conductivity, chemical oxygen demand (COD), total organic carbon (TOC) and color. In CF stage two types of coagulants were tested, aluminum sulphate and ferric chloride at concentrations of 30, 50, 70 e 100 mg.L-1. Three concentrations of commercial floculants were evaluated: 0,2, 0,3 e 0,4 mg.L-1. The experiments were conducted at pH 7. MSP steps were conducted in plan Ultrafiltration module, and in the Reverse Osmosis membrane, plan and spiral modules were tested. The best performance was obtained with a dosage of 50 mg.L-1 of the coagulant ferric chloride and 0.3 mg.L-1 commercial flocculant, which showed a 98% reduction in turbidity in respect to the raw effluent. MSP Ultrafiltration color removal was not satisfactory because color was still present. In MSP Reverse Osmosis using the plan module the goal of color removal was successfully achieved in the visual analysis, however, the membrane flow was extremely low compared with the UF permeate flow and prevented the process. The color in MSP Reverse Osmosis spiral module has been successfully removed, the turbidity was below 1 NTU, the COD was below the detection limit of the the equipment and the permeate flow was satisfactory. In this way, the study showed the best application for this effluent is CF combined with RO.

A indústria têxtil utiliza elevados volumes de água em seus processos, principalmente na etapa de tingimento, em que são utilizadas também quantidades elevadas de corantes e auxiliares têxteis. A presença desses produtos no efluente gera um efeito prejudicial e claramente visível ao ambiente, pois causam alteração nos parâmetros da qualidade da água do corpo receptor. O presente estudo apresenta o pós-tratamento de um efluente têxtil, objetivando o reciclo deste efluente para água de processo de tingimento. Para isso foi utilizada uma combinação de processo físico-químico de coagulação/floculação (CF) e processo de separação por membrana (PSM) de Ultrafiltração (UF) e Osmose Inversa (OI). Os parâmetros analisados antes e após os tratamentos foram: turbidez, condutividade elétrica, demanda química de oxigênio (DQO), carbono orgânico total (COT) e cor. Na etapa de CF foram testados dois tipos de coagulantes, o Sulfato de Alumínio e o Cloreto Férrico, nas concentrações de 30, 50, 70 e 100 mg.L-1. Foram testadas três concentrações de floculante comercial: 0,2, 0,3 e 0,4 mg.L-1. Os experimentos foram conduzidos em pH 7. As etapas de PSM foram conduzidas em módulo plano de Ultrafiltração e em módulos plano e espiral na membrana de Osmose Inversa. O melhor desempenho foi obtido com a dosagem de 50 mg.L-1 do coagulante cloreto férrico e a de 0,3 mg.L-1 de floculante comercial, que apresentou uma redução de 98% na turbidez com relação ao efluente de alimentação. No PSM de Ultrafiltração a remoção de cor não foi satisfatória por ainda apresentar coloração. No PSM de Osmose Inversa com o módulo plano o objetivo da remoção de cor foi atingido com sucesso na análise visual, porém, a vazão de permeado mostrou-se muito baixa inviabilizando o processo. No PSM de Osmose Inversa em módulo espiral a cor foi removida com sucesso, a turbidez ficou abaixo de 1 NTU, a DQO ficou abaixo do limite de detecção do equipamento e a vazão de permeado foi satisfatória. Assim, o estudo aponta como resultado a aplicação CF combinado à OI no tratamento eficaz deste efluente. / The textile industry uses large volumes of water in their processes, especially in the dyeing step, which are also used large quantities of coloring agents and textile auxiliaries. The presence of these products in the effluent generates a harmful effect and clearly visible to the environment because they cause changes in the parameters of the receiving body of water. This paper presents the post-treatment effluent from a textile industry, in order to recycle it as process water for dyeing. A combination of physico-chemical process were carried out applying coagulation / floculation (CF) and Ultrafiltration (UF) membrane separation process (MSP) and reverse osmosis (RO). The parameters analyzed before and after treatments were: turbidity, electrical conductivity, chemical oxygen demand (COD), total organic carbon (TOC) and color. In CF stage two types of coagulants were tested, aluminum sulphate and ferric chloride at concentrations of 30, 50, 70 e 100 mg.L-1. Three concentrations of commercial floculants were evaluated: 0,2, 0,3 e 0,4 mg.L-1. The experiments were conducted at pH 7. MSP steps were conducted in plan Ultrafiltration module, and in the Reverse Osmosis membrane, plan and spiral modules were tested. The best performance was obtained with a dosage of 50 mg.L-1 of the coagulant ferric chloride and 0.3 mg.L-1 commercial flocculant, which showed a 98% reduction in turbidity in respect to the raw effluent. MSP Ultrafiltration color removal was not satisfactory because color was still present. In MSP Reverse Osmosis using the plan module the goal of color removal was successfully achieved in the visual analysis, however, the membrane flow was extremely low compared with the UF permeate flow and prevented the process. The color in MSP Reverse Osmosis spiral module has been successfully removed, the turbidity was below 1 NTU, the COD was below the detection limit of the the equipment and the permeate flow was satisfactory. In this way, the study showed the best application for this effluent is CF combined with RO.

Orientadores: Maria Regina Wolf Maciel, Mario Eusebio Torres Alvarez / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Quimica / Made available in DSpace on 2018-08-11T16:17:30Z (GMT). No. of bitstreams: 1 Araujo_WilsonAndaleciode_D.pdf: 2993508 bytes, checksum: 29abb03a65a80f6c9835367e0cb49d50 (MD5) Previous issue date: 2008 / Resumo: Os processos de separação com membranas (PSM) têm sido considerados como alternativa a processos clássicos de separação. Esta é uma área de estudo que apresenta uma forte interdisciplinaridade. Há um crescente interesse nestes processos para diversas aplicações como, por exemplo, tratamento de efluentes industriais, desalinização de águas, purificação e concentração de correntes da indústria alimentícia. A separação, em geral, não envolve mudança de fase, o que significa economia no consumo de energia e operações a temperaturas moderadas. Na tecnologia de separação com membranas, os componentes das misturas líquidas ou gasosas são separados ao permearem de forma seletiva através de uma membrana. As membranas podem ser poliméricas ou cerâmicas. A corrente de alimentação é dividida em duas correntes de saída: a que permeou através da membrana (permeado) e a corrente concentrada retida (¿retentate¿). Estes processos têm sido aplicados no processamento de bebidas, sucos, e aromas. Neste trabalho, dois PSM foram estudados, a Osmose Inversa (OI) e a Pervaporação (PV). Experimentos em escala piloto foram realizados empregando-se o processo de OI (membrana de poliamida) para a concentração de suco de laranja a 20°Brix. Avaliou-se a retenção de compostos de voláteis (acetaldeído, metanol e etanol) monitorando-se as correntes de alimentação e permeado. Os resultados de retenção de aromas obtidos não foram satisfatórios. A membrana apresentou baixas retenções para os voláteis monitorados na temperatura usada para realização dos experimentos. Na segunda etapa do trabalho, o processo de PV foi avaliado para recuperação de um importante éster do suco de laranja, o etil butirato. O software PERVAP, um simulador Fortran essencialmente preditivo, foi empregado no estudo de desempenho do processo para duas membranas, polidimetilsiloxano (PDMS) e polioctilmetilsiloxano (POMS). Realizou-se a predição de propriedades de membranas poliméricas para incremento da capacidade preditiva do simulador. Foram empregados métodos de contribuição de grupos para predição das propriedades dos polímeros. Os dados de viscosidade preditos para o POMS viabilizaram a realização de cálculos para obtenção de parâmetros requeridos para operação do simulador. A abordagem proposta proporcionou maior versatilidade ao simulador / Abstract: The membrane separation processes (MSP) have been considered as alternative for conventional separation processes. In this research area a strong interdisciplinarity is observed. There is an increasing of interest for these processes considering many aplications (e.g., industrial wastewater treatment, water desalination, purification and concentration of food industry streams). The separation usually does not requires phase change, which means energy savings and moderate temperatures. A membrane separation system separates an inlet stream into two effluent streams known as the permeate and the retentate. The permeate is the portion of the fluid that has passed through the membrane. Whereas the retentate stream contains the constituents that have been rejected by the membrane. The membrane can be polymeric or ceramic. These processes have been applied for processing beverages, juices and aromas. In this work, two of these processes were studied, Reverse Osmosis (RO) and Pervaporation (PV). Pilot scale experiments were accomplished using RO (poliamide membrane) for concentrating single strength orange juice at 20ºBrix. The retention of volatile compounds (acetaldehyde, methanol and ethanol) was evaluated by monitoring feed and permeate streams. The retention results obtained were unsatisfactory. The membrane presented low retention for monitored volatiles under studied temperature conditions. In the second stage of this work, the PV process was evaluated for recovering an important ester of orange juice, the ethyl butyrate. The PERVAP software, an essentially predictive Fortran simulator, was used for evaluating process performance considering two membranes, polydimethylsiloxane (PDMS) and polyoctylmethylsiloxane (POMS). It was accomplished the prediction of properties for polymeric membranes targeting the software predictivity improvement. Viscosity data predicted for POMS was crucial for calculating parameters required by simulator. The predictive approach proposed improved the software versatility / Doutorado / Desenvolvimento de Processos Químicos / Doutor em Engenharia Química