Slot-rectangular spouted beds, with rectangular cross-section and slotted gas inlets, have been proposed as a solution to overcoming scale-up difficulties with conventional axisymmetric spouted beds. They can be utilized in gas/particle processes such as drying of coarse particles and coating of tablets. However, application of this spouted bed was limited because of instability and insufficient hydrodynamic studies. The present work is therefore aimed at the study of hydrodynamics, stability and scale-up of slot-rectangular spouted beds. The hydrodynamic study was carried out in four slot-rectangular columns of various width-to-thickness ratios combined with various slot configurations, particles of different properties and a range of operating conditions. Hydrodynamics of slot-rectangular spouted beds showed major similarity with conventional spouted beds. However, equations and mechanistic models adopted from conventional axisymmetric spouted beds generally failed to provide good predictions for the three-dimensional slot-rectangular geometry. New empirical correlations were derived for the minimum spouting velocity and maximum pressure drop for different slot configurations. Slot-rectangular spouted beds also showed more flow regimes than conventional spouted beds. Nine flow regimes, as well as unstable conditions, were identified based on frequency and statistical analysis of pressure fluctuations. Slot geometrical configuration was found to be the main factor affecting the stability of slot-rectangular spouted beds. A comprehensive hydrodynamic study on the effect of slot configuration was therefore carried out. Slots of smaller length-to-width ratio, smaller length and greater depth were found to provide greater stability. Stable criteria for the slot configuration were found consistent with the conventional axisymmetric spouted beds with extra limitation on slot length-to-width ratio and slot depth. Local distributions of pressure, particle velocity and voidage, as well as spout shape and particle circulating flux, were compared for different slot configurations. Higher slot length-to-width ratios lead to slightly higher particle circulation rates. A previously proposed scale-up method involving multiple chambers was tested in the present work using multiple slots. Instability caused by the merging of multiple spouts and asymmetric flow was successfully prevented by suspending vertical partitions between the fountains. Some criteria and guidelines were also proposed for scale-up using multiple chambers.

Polymer extrusion is an energy intensive process whereby the simultaneous action of viscous shear and thermal conduction are used to convert solid polymer to a melt which can be formed into a shape. To optimise efficiency, a homogeneous melt is required with minimum consumption of process energy. In this work, in-process monitoring techniques have been used to characterise the thermal dynamics of the single screw extrusion process with real-time quantification of energy consumption. Thermocouple grid sensors were used to measure radial melt temperatures across the melt flow at the entrance to the extruder die. Moreover, an infrared sensor flush mounted at the end of the extruder barrel was used to measure non-invasive melt temperature profiles across the width of the screw channel in the metering section of the extruder screw. Both techniques were found to provide useful information concerning the thermal dynamics of the extrusion process; in particular this application of infrared thermometry could prove useful for industrial extrusion process monitoring applications. Extruder screw geometry and extrusion variables should ideally be tailored to suit the properties of individual polymers but in practise this is rarely achieved due the lack of understanding. Here, LDPE, LLDPE, three grades of HDPE, PS, PP and PET were extruded using three geometries of extruder screws at several set temperatures and screw rotation speeds. Extrusion data showed that polymer rheology had a significant effect on the thermal efficiency on the extrusion process. In particular, melt viscosity was found to have a significant effect on specific energy consumption and thermal homogeneity of the melt. Extruder screw geometry, set extrusion temperature and screw rotation speed were also found to have a direct effect on energy consumption and melt consistency. Single flighted extruder screws exhibited poorer temperature homogeneity and larger fluctuations than a barrier flighted screw with a spiral mixer. These results highlighted the importance of careful selection of processing conditions and extruder screw geometry on melt homogeneity and process efficiency. Extruder scale was found to have a significant influence on thermal characteristics due to changes in surface area of the screw, barrel and heaters which consequently affect the effectiveness of the melting process and extrusion process energy demand. In this thesis, the thermal and energy characteristics of two single screw extruders were compared to examine the effect of extruder scale and processing conditions on measured melt temperature and energy consumption. Extrusion thermal dynamics were shown to be highly dependent upon extruder scale whilst specific energy consumption compared more favourably, enabling prediction of a process window from lab to industrial scale within which energy efficiency can be optimised. Overall, this detailed experimental study has helped to improve understanding of the single screw extrusion process, in terms of thermal stability and energy consumption. It is hoped that the findings will allow those working in this field to make more informed decisions regarding set conditions, screw geometry and extruder scale, in order to improve the efficiency of the extrusion process.

For the pharmaceutical industry, the manufacture of high value pharmaceuticals from natural products, chemical synthetic routes or fermentation processes all require intensive downstream processing steps to produce a pure final product. A small footprint liquid-liquid processing method would help to reduce the capital cost and process development time of this downstream processing. In this thesis, it is hypothesised that continuous liquid-liquid extraction can be achieved using a standard hydrodynamic counter-current chromatography (CCC) instrument by switching the flow of the liquid phases between normal phase and reversed phase intermittently, so separating a feed stream into two eluant flows. A model of the process was derived and tested on three scales of instrument, from the semipreparative to the pilot scale. The method developed, Intermittent Counter-current Extraction (ICcE) was compared to dual-flow counter-current chromatography (DFCCC), the classical method of applying continuous extraction using a counter-current chromatograph. ICcE was found to be advantaged due to the more stable phase volume ratio achievable in the columns and the ability to operate the procedure on standard commercial twin-column CCC instruments which operate at high g-field. The robustness of the ICcE method was successfully demonstrated across a range of phase system polarities and at high throughput (1kg/day on a preparative instrument) with model mixtures of pharmaceutical compounds. The effectiveness of this new processing method was confirmed on three industrially relevant case studies. Firstly a polar extract from natural senna pods to extract important sennosides, secondly an intermediate polarity highly complex active pharmaceutical ingredient waste stream to recover the main active component and thirdly a non-polar natural product extract to recover macrocarpal compounds. In summary, the ICcE method now offers another tool in the range of liquid-liquid separation methods available to the pharmaceutical and other high value industries.

Traitement et séchage de sol-gels est une pratique utilisée couramment dans l'industrie en raison du grand nombre d'applications existantes pour les produits en aval. Parmi eux, un produit spécifique capte une grande attention en raison de son élevé potentiel principalement pour l’application dans l'isolation thermique résidentielles, industrielles et même l'aérospatiale. Ce type de produit, appelé aérogel est un matériau dont la structure nanoporeuse marque une très faible densité et de conductivité thermique. La production d'aérogel peut être réalisée par diverses méthodes en fonction de la technique de séchage utilisée pour évacuer le liquide retenu dans les pores de gel: Tourner autour du point triple, franchissant la ligne d'évaporation ou contourner le point critique. L'objet de cette thèse consiste à fournir la base technologique nécessaire pour le développement d'un programme de la commercialisation industrielle des aérogels. A cet effet, la poursuite soutiendra sur la compréhension et l'identification de la présente maturité technologique, le développement et la mise à l'échelle d'un processus et de produits optimisés, et l'évaluation d'un plan d'affaires pour la production commerciale d'aérogels. L'environnement dans lequel s’effectue cette thèse se compose de deux domaines différents. Une consisté dans la conception, construction et opération des équipements spécifiques au sein de SEPAREX, et l'autre était dirigé dans la participation et la gestion de quatre projets européens du 7ème framework program: AEROCOINs, AerSUS, HIPIN et RESEEPE. Tous engagée dans la recherche et le développement de divers matériaux à base d’aérogels pour des applications dans l'isolation et la rénovation des bâtiments et dans l'isolation des vaisseaux spatiaux et des satellites. SEPAREX a participé en tant qu'expert dans le procédé de séchage de ces matériaux et aussi comme expert dans la conception et la mise à l'échelle d'équipements pour le processus concerné / Processing and drying of sol-gels is a widely practice used in industry due to the large number of existing applications for the downstream products. Among them, a specific product captures a great attention due to its high potential mainly for thermal insulation as residential, industrial and even aerospace applications. This product type, called aerogel, is a nanoporous material whose structure having extremely low density and thermal conductivity. Aerogel production can be carried out by various methods depending on the drying technique used to evacuate the liquid retained within the gel pores: Turning around the triple point, crossing the evaporation line or turning around the critical point. The purpose of the present thesis is to provide the technological basis required for the development of a program for the industrial commercialization of aerogels. For this purpose, the survey shall cover the understanding and identification of the present technology maturity, the development and scaling of an optimized process and products, and evaluation of a commercial business plan for the production of aerogels. The environment in which takes place this thesis is comprised in two different areas. One consisted in designing, construction and operation of a specific equipment within SEPAREX, and the other one was led in participation and management of four European projects of the 7th framework program: AEROCOINs, AerSUS, HIPIN and RESEEPE. All of them engaged in the research and development of diverse aerogels-based materials for applications in insulation and retrofitting of buildings and insulation of spacecraft and satellites. SEPAREX participated as expert in the drying process of such materials and also as expert in the design and scale-up of equipment for the process therefore

Le marché des alicaments est en pleine évolution et fait l'objet de recherches importantes dans le secteur agroalimentaire. Cette thèse a pour objectif de caractériser expérimentalement un procédé de production de caramels riches en dianhydrides de fructose (DAF) à l'échelle laboratoire en vue d'une extrapolation à l'échelle semi-pilote par CFD (Computational Fluid Dynamics). Ces caramels ont été préparés à partir d'un sirop de fructose en présence d'une résine qui joue le rôle de catalyseur. L'influence du titre en fructose, de la teneur en résine et de la température a été étudiée. Dans un premier temps, une étude a été menée pour établir des lois de vitesse à partir d'un mécanisme de réaction simplifié. Le suivi cinétique permet d'atteindre jusqu'à 50% de DAF selon les conditions opératoires. Dans un second temps, la caractérisation des fluides prenant part lors de la réaction de caramélisation a été étudiée. Un changement de comportement a été observé lors de la réaction. Le fluide newtonien devient non-newtonien (rhéofluidifiant). Dans un troisième temps, le comportement hydrodynamique du système a été analysé par CFD afin de proposer un semi-pilote présentant des résultats similaires à ceux mesurés à l'échelle laboratoire. La proposition issue du calcul numérique basé sur les nombres adimensionnels est un réacteur discontinu de géométrie cylindrique muni d'un agitateur de type semi-circulaire. Le mélangeur statique a été aussi envisagé. Dans ce cas, la vitesse radiale du fluide (0,2 m.s-1) est le facteur d'extrapolation. Enfin, la faible consommation énergétique de ce réacteur continu présente unvéritable atout pour produire des caramels à l'échelle industrielle. / The functional food market (foods with beneficial properties for health) is increasing and is subject of important research in the food industry. The goal of this thesis has been experimental characterization of caramels with high proportion of di-fructose anhydrides (DFA) processes, using laboratory-scale experiments with the aim to design a semi-pilot-scale reactor by CFD (Computational Fluid Dynamics). These caramels were prepared from a solution of fructose syrup with a resin catalyst. The influence of the ratio fructose/water, proportion of resin and temperature were studied. In a first step, a study was carried out to establish the kinetics laws from a simplified reaction mechanism. The results showed a DAF’s yield of up to 50% depending on the operating conditions. In a second step, the fluids involved in caramelization reaction were characterized. A behavior change outcome was observed during the reaction: the Newtonian fluid becomes non-Newtonian (rheofluidifying). In a third step, the hydrodynamic behavior was analyzed by CFD in order to propose a semi-pilot-scale reactor with similar results to laboratory scale. The numerical modeling based on non-dimensional numbers proposes a batch reactor with cylindrical geometry equipped with a stirrer of semi-circular type. The static mixer was also contemplated. In this case, the radial velocity of fluid (0.2 m.s-1) is the scale up factor. Finally, the low energy consumption of this continuous reactor represents a real advantage to produce caramel to industrial scale / El mercado de los alimentos funcionales (alimentos con propiedades benéficas para la salud) está en plena evolución y ha sidoobjeto de investigación en la industria alimentaria. Esta tesis tiene como objetivo caracterizar experimentalmente un proceso aescala de laboratorio para producir caramelos con alto contenido en dianhídridos de fructosa (DAF), con el fin de extrapolar a unaescala semi-piloto utilizando CFD (Computational Fluid Dynamics). Estos caramelos son obtenidos a partir de jarabe de fructosautilizando una resina como catalizador. Se estudió la influencia de la proporción de fructosa, la proporción de resina y de latemperatura. En una primera etapa, se realizó un estudio para establecer las leyes de velocidad a partir de un mecanismo dereacción simplificado. El seguimiento cinético permitió alcanzar un rendimiento de hasta 50% en DAF dependiendo de lascondiciones operatorias. En una segunda etapa, se realizó una caracterización de los fluidos implicados en la reacción decaramelización. Un cambio en el comportamiento del fluido durante la reacción fue observado. El fluido newtoniano se comportacomo fluido no-newtoniano (adelgazante). En una tercera etapa, el comportamiento hidrodinámico del sistema fue analizadomediante CFD, a fin de proponer un reactor semi-piloto que presente resultados similares a los calculados para la escalalaboratorio. La propuesta resultante del modelo matemático basado en los números adimensionales, es un reactor por lotes con unageometría cilíndrica y un agitador de tipo semicircular. Un mezclado estático fue también conceptualizado. En este caso, lavelocidad radial del fluido (0,2 m.s-1) fue el factor de extrapolación del proceso. Por último, el bajo consumo de energía de estereactor continuo representa una verdadera ventaja para la producción de caramelos a nivel industrial.

Orientadores: Maria Helena Andrade Santana, Lucimara Gaziola de la Torre / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Química / Made available in DSpace on 2018-08-16T11:16:49Z (GMT). No. of bitstreams: 1 Trevisan_JuliaExaltacao_M.pdf: 7656590 bytes, checksum: c2da607d637d0d57546aa48d6017dcbe (MD5) Previous issue date: 2010 / Resumo: Este trabalho apresenta um estudo comparativo de processos escalonáveis dos tipos "top-down" (cominuição) e "bottom-up" (síntese), visando a produção de lipossomas funcionais para a vacinação gênica contra a tuberculose. Na abordagem "top-down" os lipossomas foram produzidos através da alimentação de uma dispersão de fosfolipídios em água e simultânea cominuição através de cisalhamento produzido por agitadores mecânicos dos tipos Caules (C) e Ultra-turrax® (U-T). Os lipossomas provenientes do U-T foram posteriormente submetidos a maiores níveis de cisalhamento, pela passagem através de microcanais tortuosos a pressões da ordem de 100 atm, em microfluidizador (M). A influência das variáveis operacionais sobre o diâmetro, polidispersidade e potencial zeta foi analisada através de planejamento estatístico fatorial e superfícies de resposta. Para C e U-T, os efeitos do cisalhamento prevaleceram em relação à vazão de alimentação. Para M, a pressão exerceu maior influência que o número de passagens. A taxa de cisalhamento aplicada variou na faixa de 102 a 7.106 s-1, produzindo diâmetros médios de 957 a 90 nm, polidispersidades de 0,60 a 0,25 e potenciais zeta de -60 a -44 mV. O diâmetro médio dos lipossomas variou com o inverso da raiz quadrada da taxa de cisalhamento. No processo "bottom-up" os lipossomas foram produzidos continuamente na interface etanol/fosfolipídio e água, formada por focalização hidrodinâmica em microcanal reto de 0,14 mm de largura. A velocidade de formação dos lipossomas variou com a razão água/etanol, concentração e composição lipídica. As propriedades físico-químicas originais dos lipossomas funcionais foram aproximadamente reproduzidas em ambos os processos escalonáveis. Comparativamente, o processo "top-down" é mais robusto, de fácil operação, permite utilizar altas concentrações lipídicas (400 mM), com obtenção de maior produtividade. Porém é descontínuo e requer maior consumo energético. O processo "bottom-up" é menos robusto, opera de forma estável a mais baixas concentrações lipídicas (100 mM), porém a produção é contínua e com menor consumo energético / Abstract: The work presents a comparative study of scalable process with a top-down (comminution) and bottom-up (synthesis) approach, aiming the production of functional liposomes for the genetic vaccination against tuberculosis. For the top-down approach, liposomes were produced through the feed of a phospholipid in water solution and simultaneous comminution by cowls (C) and Ultra-Turrax® (U-T) mechanical dispersers. The liposomes obtained by U-T were then submitted to greater levels of shear through the processing in tortuous microchannels under a pressure in the order of 100 atm, in a microfluidizer (M). The influence of the operational variables on the diameter, polydispersity and zeta potential was analyzed through statistics factorial planning and response surface. For C and U-T the effects of shear overcame the effects of feed flow rate, and for M the effects of shear had greater influence than the number of passes.The applied hear rate varied in the range of 102 a 7.106 s-1, resulting in liposomes with mean diameter of 957 to 90 nm, polydispersity of 0,60 to 0,25 and zeta potential of -60 to -44 mV. The mean diameter varied with the inverse of the square root of the shear rate applied. In the bottom-up process liposomes were produced continuously at the interface ethanol/phospholipid and water, formed by the hydrodynamic focusing in a straight microchannel with 0,14 mm of width. The liposome formation velocity varied with the ethanol/water flow ratio, the lipid concentration and composition. The original physico-chemical properties of the functional liposomes were approximately reproduced in both scalable approaches. Comparatively, the top-down approach was more robust, easy to operate and allows the use of high lipid concentration (400 mM), achieving a greater productivity. However, it is discontinuous and requires a higher energetic consumption. The bottom-up approach is less robust, is stably operated with lower lipid concentration (100 mM), but it is a continuous production with a low energetic consumption / Mestrado / Desenvolvimento de Processos Biotecnologicos / Mestre em Engenharia Química

Orientador: Maria Angela de Almeida Meireles / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos / Made available in DSpace on 2018-08-16T14:58:26Z (GMT). No. of bitstreams: 1 Prado_JulianaMartindo_D.pdf: 100413689 bytes, checksum: 97d764a34b988429121c4bc52191c70c (MD5) Previous issue date: 2010 / Resumo: O objetivo do presente trabalho foi avaliar a viabilidade técnica e econômica da instalação de uma planta industrial de extração supercrítica (SFE) em território nacional. Para o desenvolvimento deste trabalho o cravo-da-índia (Eugenia caryophyllus) foi selecionado como matéria-prima modelo. A validação da metodologia proposta foi realizada utilizando matérias-primas de perfil agronômico e tipo de extrato diferentes do cravo: gengibre (Zingiber officinale), resíduo de cana-de-açúcar (Saccharum spp), cidrão (Aloysia triphylla) e semente de uva (Vitis vinifera). Para os experimentos em escala de laboratório foram utilizadas duas unidades SFE com extratores de diferentes volumes, de 4,6 a 290 mL, a fim de se obterem dados de rendimento global e cinéticos. Os parâmetros de processo obtidos através do ajuste das curvas de extração foram utilizados para adaptar o processo da escala laboratorial para a operação de uma planta piloto com extrator de 5 L. As análises químicas dos extratos foram realizadas por cromatografia gasosa, cromatografia em camada delgada e outras técnicas, a fim de determinar o perfil fitoquímico dos produtos obtidos. Os dados de rendimento global, juntamente com a composição química dos extratos, foram analisados a fim de selecionar a temperatura e a pressão ótimas de operação para duas matérias-primas: cravo (313 K/15 MPa) e gengibre (313 K/30 MPa). Após a determinação das curvas cinéticas de extração em escala de laboratório para as cinco matérias-primas, utilizou-se o critério de aumento de escala de manutenção da proporção entre massa de solvente e massa de matéria-prima (S/F) constante. Foi possível reproduzir com sucesso, em escala piloto 14-17 vezes maior, as curvas previamente determinadas em escala de laboratório para todas as matérias-primas. Foi realizado ainda o estudo da etapa de separação dos extratos em escala piloto, utilizando três separadores em série operando sob diferentes condições de temperatura e pressão. Extratos de diferentes aspectos físicos e composições químicas foram obtidos pela simples manipulação das condições operacionais dos separadores, caracterizando diferentes produtos. A estabilidade do extrato de gengibre armazenado a 255 K foi avaliada; durante os 4 primeiros meses de armazenamento houve significativa alteração na composição química do extrato, e nos 18 meses posteriores esta apresentou-se estável. A partir do custo de manufatura dos extratos calculado, foi demonstrado que o processo SFE no Brasil é economicamente viável para extratores industriais com volume de 50 a 500 L, dependendo da matéria-prima a ser processada. Reunindo dados técnicos e econômicos, para SFE de cravo-da-índia a 313 K/15 MPa, 52 min e S/F de 3,6 apresentam a melhor relação entre custo, rendimento e qualidade do produto. Para o resíduo de cana, os parâmetros otimizados foram 60 min e S/F de 4,8 a 333 K/35 MPa. Para SFE de semente de uva a 313 K/35 MPa, 240 min e S/F de 6,6 foram os parâmetros selecionados / Abstract: The objective of the present work was to evaluate the technical and economical viability of installing an industrial scale supercritical fluid extraction (SFE) plant in Brazil. In this work, clove (Eugenia caryophyllus) was selected as model raw material. The validation of the methodology proposed was done using raw materials of different agronomic profiles and extract types: ginger (Zingiber officinale), sugarcane (Saccharum spp) residue, lemon verbena (Aloysia triphylla) and grape (Vitis vinifera) seed. For lab scale experiments, two SFE units with extraction vessels of different volumes were used, of 4.6 to 290 mL, to obtain global yield and extraction kinetics data. The process parameters established by fitting the extraction curves were used to adapt the process from lab scale to a pilot plant equipped with a 5 L extractor. The chemical analyses of the extracts were done by gas chromatography, thin layer chromatography and other techniques, to determine the phytochemical profile of the products obtained. Global yield and chemical composition data were evaluated to determine optimum extraction temperature and pressure for two raw materials: clove (313 K/15 MPa) and ginger (313 K/30 MPa). After determining the overall extraction curves at lab scale for the five raw materials, the scale-up criterium adopted was maintaining solvent to feed ratio (S/F) constant. The curves previously determined at lab scale were successfully reproduced for 14-17 fold scale-up to pilot scale for all raw materials. The separation step of SFE process was studied at pilot scale, using three separators displayed in series, operating under different temperature and pressure conditions. Extracts of different physical aspects and chemical compositions were obtained by manipulating the separators operation conditions, characterizing different products. The stability of ginger extract stored at 255 K was evaluated; during the first 4 months of storage there was significant alteration of the extract¿s chemical composition, and during the next 18 monts it was stable. From manufacturing cost calculated for the extracts, it was demonstrated that the SFE process is economically viable in Brazil for industrial scale extractors of 50 to 500 L, depending on the raw material processed. Gathering technical and economical data, for clove, SFE at 313 K/15 MPa, 52 min and S/F of 3.6 presents the best relation between cost, yield and product quality. For sugarcane residue, the optimized parameters were 60 min and S/F of 4.8 at 333 K/35 MPa. As for grape seed, SFE at 313 K/35 MPa, 240 min and S/F of 6.6 were the selected parameters / Doutorado / Mestre em Engenharia de Alimentos

Orientador: Maria Angela de Almeida Meireles / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos / Made available in DSpace on 2018-08-12T20:43:53Z (GMT). No. of bitstreams: 1 Prado_IvorMartindo_M.pdf: 4325447 bytes, checksum: 55d908ce9e06c61099119b0e52a49ba1 (MD5) Previous issue date: 2009 / Resumo: O presente trabalho teve por objetivo validar um modelo do processo supercrítico aplicado a avaliação econômica utilizando-se um simulador comercial de processos (SuperPro Designer®) a partir de dados obtidos na literatura para a cúrcuma (Curcuma longa L.) e dados laboratoriais obtidos para o alecrim-pimenta (Lippia sidoides) e estudar os efeitos de aumento de escala no custo de manufatura (COM) do extrato vegetal de planta condimentar obtido por tecnologia supercrítica em equipamentos de extração supercrítica de diferentes capacidades. A validação do modelo de extrator SFE foi realizada utilizando-se o simulador de processos SuperPro Designer® que consiste de um conjunto de ferramentas capaz de estimar parâmetros econômicos e de processos, provido de um amplo banco de dados contendo substâncias simples e compostas comumente encontradas nas indústrias de alimento, química e farmacêutica. A montagem do modelo ocorreu utilizando os equipamentos disponíveis no banco de dados do simulador, porém por se tratar de um processo não convencional de extração o simulador não compreende um modelo de extrator SFE, sendo necessário adaptar esta operação unitária a um equipamento disponível, apto a realizar as funções necessárias. O aumento de escala foi avaliado utilizando-se o modelo SFE proposto que permitiu utilizar as ferramentas de aumento de escala disponíveis no simulador SuperPro Designer®. Nesta etapa assumiu-se que a relação entre a massa de solvente e a massa de alimentação permanece constante quando o modelo passa da escala laboratorial para a escala industrial, sendo assim, a relação entre rendimento e tempo de processo será igual para ambos os casos. Os fluxograma das plantas SFE estudadas no aumento de escala foram unidades semi-contínuas contendo dois extratores variando suas capacidades de 0,005 m3 a 1 m3. Os custos dos equipamentos utilizados na estimativa de custo foram comparados os preços praticados no mercado americano e chinês. Para a estimativa do custo de manufatura (COM) do processo SFE pelo simulador foram utilizados os modelos da etapa de avaliação do aumento de escala e a curva global de extração (OEC) para a cúrcuma obtida da literatura. Os tempos de ciclos do processo foram selecionados de acordo com o menor valor de estimativa do custo de manufatura segundo a avaliação da curva global de extração (OEC), no caso da cúrcuma o tempo utilizado foi de 37 minutos enquanto que no caso do alecrim-pimenta o tempo utilizado foi de 100 minutos por ciclo. Verificou-se que quando se trabalha com equipamentos de grande capacidade de produção o custo de manufatura não apresenta diferenças significativas independentemente do custo da unidade SFE, ou seja, o custo de equipamentos americanos ou chineses. Isto ocorre devido à grande participação do custo de matériaprima (CRM) no COM, enquanto que os custos de investimento (FCI) não apresentaram grande influência no custo final de manufatura / Abstract: Using the commercial simulator SuperPro Designer® the present work had for objective of validate a process model of supercritical solvent extraction (SFE) using data from literature for turmeric (Curcuma longa L.) and studying the effect of scale-up in the cost of manufacture (COM) in vegetal extract obtain via supercritical fluid extraction. The validation of the supercritical fluid extractor (SFE) was carried out using the process simulator SuperPro Designer® that consist in a set of tools capable to estimate economic parameters of processes; the simulator contains a large data base with simple substances and complex mixtures found in food chemistry and drug industries. The assembly of the model occurred using the available equipments in the data base of the simulator, however since we are dealing with a non conventional extraction process, the SFE equipment was not available in the simulator, and thus, it was necessary to develop the extraction unit before caring out the simulations. The scale-up was evaluated using the proposed model SFE that allowed the use of the available tools for scale up of the simulator SuperPro Designer®. In this stage it was assumed that the ratio between the mass of solvent and the feed mass remains constant for the laboratorial scale and the industrial scale units, therefore, the ratio between yield and process time will be equal in both cases. The flow diagram of the SFE units contains two extractors with capacities varying from 0,005 m3 to 1 m3. The costs of the SFE units were taken from manufactures in USA and China. To estimate the cost of manufacturing (COM) for the extract produced by the SFE process data for the overall extraction curve (OEC) from literature for turmeric was used. The cycles of process used in the estimate of cost had been chosen in accordance with the times that had presented lowest cost evaluated along of the overall curve of extraction (OEC), in the case of turmeric the process time used was 37 minutes whereas in the case of the alecrim-pimenta the time was used 100 minutes per cycle. It was verified that for equipment of larger capacity of production the cost of manufacturing (COM) is not significantly affected by the cost of the SFE unit (American and Chinese). This occurs due the fact that the cost of the raw material cost (CRM) predominates in the COM, while of the fixed costs of investment (FCI) represents a smaller fraction of the final COM / Mestrado / Mestre em Engenharia de Alimentos

Este trabalho estudou a aplicação de oito métodos clássicos de escalonamento de tanques condicionadores, testando sua validade para dois tanques de geometria semelhante, mas com diferentes volumes (V1=10 e V2=49 decímetros cúbicos). No interior dos tanques, operavam impulsores (diâmetro D1=0,078m x D2=0,132m) que exibiam três distintos desenhos (2 pás versus 4 pás inclinadas em 45 graus versus turbina de Rushton). Sua rotação (N1 no tanque menor x N2 no tanque maior) visava à suspensão de partículas grossas de apatita (diâmetro médio = 254 micrometros) em polpas com 40% de sólidos em massa. Para balizar o escalonamento, adotou-se como variável de controle a mínima rotação do impulsor (Njs) que é capaz de fazer com que nenhuma partícula repouse no fundo do tanque por mais do que 1 ou 2 segundos (Critério 1-s), além de perfis axiais de distribuição de sólidos e a extensão da Zona Turbulenta versus Zona Quiescente no interior dos tanques. A diferença entre o valor previsto de Njs para o tanque de 49 decímetros cúbicos (N2) pelos métodos de escalonamento versus o valor de Njs (N2) determinado experimentalmente foi expressa como erro percentual (E). Consideraram-se como adequados para a aplicação que constitui o objetivo desta dissertação todos os métodos que exibiram E menor que 10%. Para o impelidor de 2 pás inclinadas, a adequação do método baseado na constância da razão potência/volume (E=2%) e também do método empírico de Rautzen (E=6%), indica a expressão N2=N1.(D1/D2) com seu expoente da relação entre os diâmetros variando entre 0,67 e 0,75 para a aplicação desejada. Considerando o impulsor de 4 pás inclinadas, a adequação do método da constância da razão potência/volume (E=4%); assim como dos métodos empíricos de Rautzen (E=0%) e Zwietering (5%), sugere o uso da expressão N2=N1.(D1/D2) com seu expoente da relação entre os diâmetros variando entre 0,67 e 0,85. Para a turbina de Rushton, o único método que exibiu E menor que 10% foi o da constância da relação potência/volume (E=8%), cuja expressão é N2=N1.(D1/D2) com seu expoente da relação entre os diâmetros igual a 0,67. Uma vez que a determinação do valor real de N2 foi baseada numa técnica experimental influenciada pelas limitações do observador, pode-se inferir que uma expressão geral de escalonamento do tipo N2=N1.(D1/D2) com seu expoente da relação entre os diâmetros igual a 0,75 atende aos propósitos desta aplicação. Por outro lado, o uso da relação P/V provê um critério mais objetivo para se balizar o escalonamento, haja vista que ele se adequou a todos os três tipos de impelidores contemplados por este estudo. / This work has studied the application of eight classical methods appointed by literature to accomplish the scale-up of stirred tanks which aimed to suspend slurries of 40% of solids, containing coarse (mean diameter=254 micrometers) apatite particles. The validity of the methods was accomplished by using two tanks of similar geometry but different capacity (V1=10 e V2=49 cubic decimeter), together with impellers of different diameter (D1=0,078m versus D2=0,132m) and design (turbine of 2 or 4 blades inclined at 45 degrees and Rushton turbine). To assist the process of validation, the impeller speed (Njs) under which no particle rests on the bottom of the tank for more than 1-2 seconds (1-s Criterium) was used together with the axial profile of solids percent distribution plus the extension of the turbulent versus quiescent zones within the two tanks. For any of the eight scale-up methods, the difference between the predicted value of Njs (N2) for the 49 cubic decimeter tank and the actual value (experimental) of the same variable was determined and its magnitude was expressed in terms of the percent error (E). The methods that yielded E less than 10% were considered as suitable for the aimed application. Considering the 2-inclined blade impeller, low value of E yielded by the method based on the constancy of the ratio power/volume (E=2%) and also by the empiric method of Rautzen (E=6%) indicate that the expression N2=N1.(D1/D2) with its exponent of the relation between diameters ranging between 0,67 and 0,75 is suitable for the desired application. Regarding the 4-inclined blade impeller, because the method based on the constancy of the ratio power/volume (E=4%) and also the empiric methods of Rautzen (E=0%) and Zwietering (E=5%) yielded the lowest values of E, the expression N2=N1.(D1/D2) with its exponent of the relation between diameters ranging between 0,67 and 0,85 is suitable for the aimed application. Moreover, for the Rusthon turbine, only the method based on the constancy of the ratio power/volume (E=8%) was adequate for the aimed application and, thus, the expression N2=N1.(D1/D2) with its exponent of the relation between the diameters equal to 0,67 is suitable for the purpose of this dissertation. Once the actual value of N2 is determined by visual observation, it is not possible to get very accurate results. This way, a generic scale-up expression is proposed: N2=N1.(D1/D2) with its exponent of the relation between the diameters equal to 0,75. On the other hand, the ratio P/V may provide a more objective criterium for scale-up, because the three sort of impellers used in this study yielded E less than 10% when the power/volume method was applied for the purpose of scale-up.

Résumé confidentiel / Résumé confidentiel