Orientadores: Osvaldir Pereira Taranto, Marcelo Nitz da Costa / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Quimica / Made available in DSpace on 2018-08-12T09:06:35Z (GMT). No. of bitstreams: 1 Souza_LucianeFranquelinGomesde_M.pdf: 4524135 bytes, checksum: 1ae4c10ba2c2ed03a7393643ced61a02 (MD5) Previous issue date: 2008 / Resumo: Acetato de sódio e um sal orgânico produzido pela reação do acido acético com hidróxido de sódio. Depois da cristalização e separação os cristais úmidos são secos. Já o cloreto de potássio e um sal inorgânico extraído de rochas e águas salinas muito utilizado na industria química como fertilizante. Esses sais são higroscópicos, coesivos quando úmidos, e geralmente são secos em secadores de leitos fluidizados. No presente trabalho foi utilizado um secador de leito pulso-fluidizado (PFB) que e uma modificação do secador de leito fluidizado convencional. Neste equipamento uma taxa constante de ar e suprido para o secador. Um distribuidor de gás instalado sob a câmara de secagem promove a pulsação pela corrente de gás alternada. A principal vantagem desta técnica e o uso de uma vazão de ar menor quando comparada com outras. O PFB utilizado neste trabalho possui uma área de secção transversal de 0,18 metros quadrados e constituído de quatro seções. Inicialmente foi realizado o estudo fluidodinâmico dos sais secos e úmidos. Posteriormente as curvas de secagem do acetato de sódio e cloreto de potássio foram determinadas para diferentes condições de secagem (temperatura do ar e freqüência de pulsação). A secagem e fluidodinâmica em leito fluidizado convencional foram feitas para que a comparação com o leito pulsado fosse possível. Resultados mostraram que as taxas de secagem foram maiores na fluidizarão pulsante devido ao melhor comportamento fluidodinâmico: o fluxo intermitente ajuda a romper partículas aglomeradas e conseqüentemente prover melhor contato entre gás - partícula. / Abstract: Sodium acetate is a salt produced by the reaction of acetic acid with sodium hydroxide. After crystallization and separation, the wet crystals are dried. Potassium chloride is an inorganic salt extracted from rocks and saline water. It is mainly used in the chemical industry as a fertilizer. These salts are hygroscopic particulate materials, which are dried in fluidized beds or rotary dryers. In this work a pulsed-fluid bed (PFB) dryer was used, which is a variation of the conventional fluidized bed dryer. In this equipment, a constant airflow rate is supplied to the dryer. A gas distributor installed upstream of the drying chamber provides the pulsed-flow by alternating the gas stream. The main advantage of this technique is the lower airflow rate supplied when compared with competitive techniques. The PFB used in this work has a cross section area of 0.18 m2 and it has four sections. Initially, the fluid-dynamic study of dry and wet salts was performed. Subsequently the drying curves of sodium acetate and potassium chloride were determined for different drying conditions (inlet air temperature and pulsation frequency). Drying and Fluid-dynamic was performed in conventional fluidized bed drying, so that results could be compared. Results showed that the drying rates were higher under pulsed fluidization due to the better fluid-dynamic behavior: the intermittent flow can help to break particle agglomerates and therefore provide better contact between particles and the gas. / Mestrado / Engenharia de Processos / Mestre em Engenharia Química

According to ICH Q8 process analytic technology (PAT) should be established to monitor critical quality attributes (CQAs) during manufacturing processes. Ethinylestradiol (EE) is a highly active and low dosed steroid hormone that is prone to oxidative degradation. The stability of this compound is therefore a critical quality attribute that has to be considered during drug formulation development. Beside the stability of EE, granule particle size and moisture are CQAs influencing the tableting ability of the resulting granules and the stability of EE. Both CQAs should be monitored during the production process. The investigations described in this thesis evaluate the implementation of in-line-sensors for monitoring of particle size (spatial filtering technology, SFT) and granule moisture (microwave resonance technology, MRT) during the fluid bed granulation process and the influence of process-variations on the stability of EE. The aim of these investigations was to develop an effective and mild fluid bed granulation process for a new model formulation based on microcrystalline cellulose as replacement for lactose as main filler excipient. The EE degradation products 6-alpha-hydroxy-EE, 6-beta-hydroxy-EE, 9(11)-dehydro-EE and 6-oxo-EE were quantified as an index for the stability of EE. It could be demonstrated that the surface of the filler substance influences the stability of EE due to the impact of water molecules. Hence, spraying sequence was determined to be a useful tool to improve the stability of EE. Correlations could be established for 6-oxo-EE with granule moisture and thermic parameters. The implementation of the SFT-sensor in the granulation process was successful. Measurement with the MRT-sensor for monitoring of granule moisture has to be improved.:Chapter I 1 1 Introduction Chapter II 41 2 Materials and Methods Chapter III 54 3 In-line Monitoring of Particle Size in a Fluid Bed Granulator: investigations concerning positioning and configuration of the sensor Chapter IV 72 4 Influence of in line monitored fluid bed granulation process parameters on the stability of Ethinylestradiol Chapter V 90 5 Influence of filler excipients on stability of EE Chapter VI 105 6 Discussion and Conclusion Chapter VII 131 7 Summary Chapter VIII 138 8 Zusammenfassung Reference List 146 Appendix 158

No description available.

Made available in DSpace on 2014-06-11T19:24:46Z (GMT). No. of bitstreams: 0 Previous issue date: 2010-03-12Bitstream added on 2014-06-13T20:13:00Z : No. of bitstreams: 1 catelam_kt_me_sjrp.pdf: 2505612 bytes, checksum: 6d1f12a789582003771152e325b4032a (MD5) / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / Este projeto teve como objetivo estudar a influência de diferentes processos de desidratação (secagem em leito pulso-fluidizado, atomizador – “spray dryer” e em liofilizador) de polpa de maracujá na qualidade do produto final em pó. Todos estes processos visam à obtenção do produto em pó, apresentando vantagens e desvantagens em nível de manuseio e custos. Entretanto, são escassos na literatura estudos que comparem estes processos com foco na qualidade do produto final. O leite desnatado foi utilizado para avaliar sua eficiência na substituição de parte dos aditivos comumente utilizados na produção deste tipo de produto, como, por exemplo, a maltodextrina e a goma Arábica, os quais têm como função a diminuição das dificuldades tecnológicas encontradas na secagem de sucos de frutas e outros produtos com alta quantidade de açúcar devido à higroscopicidade, termoplasticidade e capacidade de caramelização. Inicialmente, realizaram-se as análises físico-químicas da polpa de maracujá e do leite desnatado, onde foram obtidos resultados muito próximos aos da literatura, sendo que as pequenas diferenças obtidas foram atribuídas à variedade do maracujá utilizado, época e local de cultivo e no caso do leite em pó desnatado, devido provavelmente às diferentes marcas comerciais analisadas na literatura. A secagem da polpa de maracujá sem aditivos, em diversas condições operacionais, levou a um rendimento praticamente nulo, fazendo com que o processo fosse considerado inviável nestas condições. Conseguiu-se obter o pó com a polpa de maracujá e os aditivos no secador por atomização (“spray dryer”). Utilizando a maltodextrina como aditivo, o maior rendimento (23.32%) obtido foi para a proporção de 1:4:4 (polpa de maracujá:maltodextrina:leite desnatado) ou seja, 50% dos sólidos de aditivo substituído por leite desnatado... / The aim of this research was to study the influence of different drying methods (pulsed fluid bed dryer, spray dryer and freeze dryer) of passion fruit pulp in the quality of final powder product. All these processes have the purpose to obtain a powder product, showing advantages and disadvantages in terms of handmade and costs. Nonetheless, the literature has a few studies related to comparison between these processes, focusing final product quality. Skim milk was utilized to evaluate its efficiency on partial substitution of additives commonly used in this kind of processes like maltodextrin and Arabic gum, which have the function of minimizing technologies difficulties in drying fruit juices and other products with high quantity of sugar due to hygroscopicity and termoplasticity in high temperatures and humidity. Initially, physicochemical analysis of passion fruit pulp and skim milk showed values close to those described by literature, with little differences due to passion fruit varieties used, time and place of culture. For skim milk the differences can be explain due to existence of a lot of commercial marks. Drying of passion fruit pulp without additives in many operations conditions had a small yield, becoming process impracticable in these conditions. It was obtained powdered passion fruit and additives in spray dryer. Using maltodextrin the greater yield (23.32%) was obtained for 1:4:4 ratio (passion fruit pulp:maltodextrin:skim milk) that is 50% of solids from additives substituted by skim milk. To Arabic gum the best results (21.96%) was obtained to 1:2:6 (passion fruit pulp:Arabic gum:skim milk) with 75% of solids from additives substituted by skim milk. The total substitution of additives (maltodextrin or Arabic gum) by skim milk also showed good results (15.5%). These better yield were obtained in 120°C and feed flow 0.4 l/h considering ratio of pulp... (Complete abstract click electronic access below)

Resumo: Este projeto teve como objetivo estudar a influência de diferentes processos de desidratação (secagem em leito pulso-fluidizado, atomizador - "spray dryer" e em liofilizador) de polpa de maracujá na qualidade do produto final em pó. Todos estes processos visam à obtenção do produto em pó, apresentando vantagens e desvantagens em nível de manuseio e custos. Entretanto, são escassos na literatura estudos que comparem estes processos com foco na qualidade do produto final. O leite desnatado foi utilizado para avaliar sua eficiência na substituição de parte dos aditivos comumente utilizados na produção deste tipo de produto, como, por exemplo, a maltodextrina e a goma Arábica, os quais têm como função a diminuição das dificuldades tecnológicas encontradas na secagem de sucos de frutas e outros produtos com alta quantidade de açúcar devido à higroscopicidade, termoplasticidade e capacidade de caramelização. Inicialmente, realizaram-se as análises físico-químicas da polpa de maracujá e do leite desnatado, onde foram obtidos resultados muito próximos aos da literatura, sendo que as pequenas diferenças obtidas foram atribuídas à variedade do maracujá utilizado, época e local de cultivo e no caso do leite em pó desnatado, devido provavelmente às diferentes marcas comerciais analisadas na literatura. A secagem da polpa de maracujá sem aditivos, em diversas condições operacionais, levou a um rendimento praticamente nulo, fazendo com que o processo fosse considerado inviável nestas condições. Conseguiu-se obter o pó com a polpa de maracujá e os aditivos no secador por atomização ("spray dryer"). Utilizando a maltodextrina como aditivo, o maior rendimento (23.32%) obtido foi para a proporção de 1:4:4 (polpa de maracujá:maltodextrina:leite desnatado) ou seja, 50% dos sólidos de aditivo substituído por leite desnatado... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: The aim of this research was to study the influence of different drying methods (pulsed fluid bed dryer, spray dryer and freeze dryer) of passion fruit pulp in the quality of final powder product. All these processes have the purpose to obtain a powder product, showing advantages and disadvantages in terms of handmade and costs. Nonetheless, the literature has a few studies related to comparison between these processes, focusing final product quality. Skim milk was utilized to evaluate its efficiency on partial substitution of additives commonly used in this kind of processes like maltodextrin and Arabic gum, which have the function of minimizing technologies difficulties in drying fruit juices and other products with high quantity of sugar due to hygroscopicity and termoplasticity in high temperatures and humidity. Initially, physicochemical analysis of passion fruit pulp and skim milk showed values close to those described by literature, with little differences due to passion fruit varieties used, time and place of culture. For skim milk the differences can be explain due to existence of a lot of commercial marks. Drying of passion fruit pulp without additives in many operations conditions had a small yield, becoming process impracticable in these conditions. It was obtained powdered passion fruit and additives in spray dryer. Using maltodextrin the greater yield (23.32%) was obtained for 1:4:4 ratio (passion fruit pulp:maltodextrin:skim milk) that is 50% of solids from additives substituted by skim milk. To Arabic gum the best results (21.96%) was obtained to 1:2:6 (passion fruit pulp:Arabic gum:skim milk) with 75% of solids from additives substituted by skim milk. The total substitution of additives (maltodextrin or Arabic gum) by skim milk also showed good results (15.5%). These better yield were obtained in 120°C and feed flow 0.4 l/h considering ratio of pulp... (Complete abstract click electronic access below) / Orientador: Javier Telis Romero / Coorientador: Carmen Sílvia Fávaro Trindade / Banca: João Borges LAurindo / Banca: Célia Maria Landi Franco / Mestre

L'amélioration de la dissolution des médicaments peu solubles présente de nombreux défis.Dans cette thèse, un procédé d'extrusion-sphéronisation a été étudié en profondeur pour améliorer la dissolubilité du médicament avec une formulation de nano-émulsion. Le but du travail de thèse est de décrire les propriétés et les procédés de fabrication de minigranules permettant d'augmenter la solubilité des principes actifs peu solubles dans l'eau et donc d‘améliorer leur biodisponibilité lors de l'administration par voie orale, pour deux modèles de molécules différentes qui sont l‘acide folique (vitamine peu soluble dans l'eau) et le kétoprofène (anti-inflammatoire non stéroïdien qui présente une solubilité limitée dans les fluides gastriques à cause de son pKa (classe II dans le système de classification biopharmaceutique – BCS, ayant une action anti-inflammatoire, antalgique et antipyrétique). Cette étude décrit la préparation par extrusion-sphéronisation, caractérisation et étude de dissolution in vitro d'acide folique et de pastilles de kétoprofène revêtues de Acryl-EZE®, Advantia® Performance dans un minicoatère à lit fluidisé. Les résultats des essais ont montré la faisabilité de la préparation de pastilles enrobées entériques contenant un AINS et que, en revêtant le système multiparticulaire avec Acryl-EZE® 93A92545 et Advantia® Performance190024HA49 à un gain pondéral de 17,5%, 12,0%, respectivement, du médicament à partir des pastilles peuvent être obtenus. Les résultats des essais de dissolution ont indiqué que dans un milieu acide, le revêtement de film a entraîné un retard dans la libération du médicament, alors qu'aucun retard n'a été observé dans un milieu tampon à pH 6,8. / Improvement in dissolution of poorly soluble drugs has many challenges.In this thesis, an extrusion-spheronization process was thoroughly studied forimproving dissolubility of drug with nano-emulsion formulation.The aim of the thesis work is to describe the properties and manufacturing processes ofpellets to increase the solubility of poorly soluble active ingredients in water and thus improvetheir bioavailability when administered orally: folic acid (water-insoluble vitamin) andketoprofen (Non-steroidal anti-inflammatory, having anti-inflammatory, analgesic andantipyretic action, class II in the Biopharmaceutical Classification System).This study describes the preparation by extrusion-spheronization, characterisation andin vitro dissolution study of folic acid and ketoprofen pellets. Ketoprofen pellets coated withAcryl-EZE®, Advantia® Performance in a fluid-bed minicoater. The results of the tests showedthe feasibility of the preparation of enteric-coated pellets containing a NSAID and that bycoating the multiparticulate system with either 17.5% Acryl-EZE® 93A92545 or with 12%Advantia® Performance 190024HA49 weight gain, an enteric release of the drug from thepellets can be obtained. The results of dissolution testing indicated that in acidic media, entericfilm coating resulted in a delay in the release of the drug, while no delay was observed in pH6.8 buffer media.

Preparation of geopolymer composites from industrial wastes of energy power stations and metalurgy.

This master thesis designes the calculation of fluid boiler with specific part - the circular fluid bed. The heat is given by combustion of wood biomass. The thesis is devided into several parts. All necessary elementary results are going to be reached within these parts: an analysis of solid fuel, stechiometry calculation, discussion on output limits and the environmental point of view, definition of elemental heat losses and general heat efficiency, calculation and design of a combustion part and its heat loads and calculation of enthalpies with different ash concentrations. All these phases get to a successful design of the fluid boiler heat balance and sizes of heat-flow surfaces. The composition of the boiler shows the added drawing.

[ES] Los altos costes energéticos, las constantes medidas regulatorias aplicadas por las administraciones para mantener bajos los costes sanitarios, así como los cambios en la normativa sanitaria que se han introducido en los últimos años, han tenido un impacto significativo en la industria farmacéutica y sanitaria. El paradigma Industria 4.0 engloba cambios en el modelo productivo tradicional de la industria farmacéutica con la inclusión de tecnologías que van más allá de la automatización tradicional. El objetivo principal es lograr medicamentos más rentables mediante la incorporación óptima de tecnologías como la analítica avanzada. El proceso de fabricación de las industrias farmacéuticas tiene diferentes etapas (mezclado, secado, compactado, recubrimiento, envasado, etc.) donde una de las etapas más costosas energéticamente es el proceso de secado. El objetivo durante este proceso es extraer el contenido de líquidos como el agua mediante la inyección de aire caliente y seco en el sistema. Este tiempo de secado normalmente está predeterminado y depende del volumen y el tipo de unidades de producto farmacéutico que se deben deshidratar. Por otro lado, la fase de precalentamiento puede variar dependiendo de varios parámetros como la experiencia del operador. Por lo tanto, es posible asumir que una optimización de este proceso a través de analítica avanzada es posible y puede tener un efecto significativo en la reducción de costes en todo el proceso de fabricación. Debido al alto coste de la maquinaria involucrada en el proceso de producción de medicamentos, es una práctica común en la industria farmacéutica tratar de maximizar la vida útil de estas máquinas que no están equipados con los últimos sensores. Así pues, es posible implementar un modelo de aprendizaje automático que utilice plataformas de analítica avanzada, como la computación en la nube, para analizar los posibles ahorros en el consumo de energía. Esta tesis está enfocada en mejorar el consumo de energía en el proceso de precalentamiento de un secador de lecho fluido, mediante la definición e implementación de una plataforma de computación en la nube IIOT (Industrial Internet of Things)-Cloud, para alojar y ejecutar un algoritmo de aprendizaje automático basado en el modelo Catboost, para predecir cuándo es el momento óptimo para detener el proceso y reducir su duración y, en consecuencia, su consumo energético. Los resultados experimentales muestran que es posible reducir el proceso de precalentamiento en un 45% de su duración en tiempo y, en consecuencia, reducir el consumo de energía hasta 2.8 MWh por año. / [CAT] Els elevats costos energètics, les constants mesures reguladores aplicades per les administracions per mantenir uns costos assistencials baixos, així com els canvis en la normativa sanitària que s'han introduït en els darrers anys, han tingut un impacte important en el sector farmacèutic i sanitari. El paradigma de la indústria 4.0 engloba els canvis en el model de producció tradicional de la indústria farmacèutica amb la inclusió de tecnologies que van més enllà de l'automatització tradicional. L'objectiu principal és aconseguir fàrmacs més rendibles mitjançant la incorporació òptima de tecnologies com l'analítica avançada. El procés de fabricació de les indústries farmacèutiques té diferents etapes (mescla, assecat, compactació, recobriment, envasat, etc.) on una de les etapes més costoses energèticament és el procés d'assecat. L'objectiu d'aquest procés és extreure el contingut de líquids com l'aigua injectant aire calent i sec al sistema. Aquest temps de procediment d'assecat normalment està predeterminat i depèn del volum i del tipus d'unitats de producte farmacèutic que cal deshidratar. D'altra banda, la fase de preescalfament pot variar en funció de diversos paràmetres com l'experiència de l'operador. Per tant, podem assumir que una optimització d'aquest procés mitjançant analítiques avançades és possible i pot tenir un efecte significatiu de reducció de costos en tot el procés de fabricació. A causa de l'elevat cost de la maquinària implicada en el procés de producció de fàrmacs, és una pràctica habitual a la indústria farmacèutica intentar maximitzar la vida útil d'aquestes màquines que no estan equipats amb els darrers sensors. Així, es pot implementar un model d'aprenentatge automàtic que utilitza plataformes de analítiques avançades com la computació en núvol, per analitzar l'estalvi potencial del consum d'energia. Aquesta tesis està enfocada a millorar el consum d'energia en el procés de preescalfament d'un assecador de llit fluid, mitjançant la definició i implementació d'una plataforma IIOT (Industrial Internet of Things)-Cloud computing, per allotjar i executar un algorisme d'aprenentatge automàtic basat en el modelatge Catboost, per predir quan és el moment òptim per aturar el procés i reduir-ne la durada, i en conseqüència el seu consum energètic. Els resultats de l'experiment mostren que és possible reduir el procés de preescalfament en un 45% de la seva durada en temps i, en conseqüència, reduir el consum d'energia fins a 2.8 MWh anuals. / [EN] High energy costs, the constant regulatory measures applied by administrations to maintain low healthcare costs, and the changes in healthcare regulations introduced in recent years have all significantly impacted the pharmaceutical and healthcare industry. The industry 4.0 paradigm encompasses changes in the traditional production model of the pharmaceutical industry with the inclusion of technologies beyond traditional automation. The primary goal is to achieve more cost-efficient drugs through the optimal incorporation of technologies such as advanced analytics. The manufacturing process of the pharmaceutical industry has different stages (mixing, drying, compacting, coating, packaging, etc..), and one of the most energy-expensive stages is the drying process. This process aims to extract the liquid content, such as water, by injecting warm and dry air into the system. This drying procedure time usually is predetermined and depends on the volume and the kind of units of a pharmaceutical product that must be dehydrated. On the other hand, the preheating phase can vary depending on various parameters, such as the operator's experience. It is, therefore, safe to assume that optimization of this process through advanced analytics is possible and can have a significant cost-reducing effect on the whole manufacturing process. Due to the high cost of the machinery involved in the drug production process, it is common practice in the pharmaceutical industry to try to maximize the useful life of these machines, which are not equipped with the latest sensors. Thus, a machine learning model using advanced analytics platforms, such as cloud computing, can be implemented to analyze potential energy consumption savings. This thesis is focused on improving the energy consumption in the preheating process of a fluid bed dryer by defining and implementing an IIOT (Industrial Internet of Things) Cloud computing platform. This architecture will host and run a machine learning algorithm based on Catboost modeling to predict when the optimum time is reached to stop the process, reduce its duration, and consequently its energy consumption. Experimental results show that it is possible to reduce the preheating process by 45% of its time duration, consequently reducing energy consumption by up to 2.8 MWh per year. / Barriga Rodríguez, R. (2023). Optimization of Fluid Bed Dryer Energy Consumption for Pharmaceutical Drug Processes through Machine Learning and Cloud Computing Technologies [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/195847

Autoclaved sand aerated concrete is a modern building material with high thermal insulation properties. Only sand is used as the primary silicate component of aerated concrete in the Czech Republic. For the more favourable economic and ecological properties of aerated concrete, the use of secondary raw materials is used in this work. The secondary raw materials examined included fluidized bed and fly ash, slag and glass recycled. The aerated concrete composite with secondary admixtures was developed under hydrothermal conditions of a laboratory autoclave for 7 and 12 hours at 190°C. From the secondary raw materials tested, a 10% glass recycler additive yielded the highest strength. Other additives that have a positive effect on mechanical properties include SAKO and Oslavany. From the results of the work it is evident that the use of secondary raw materials increases the strength, improves the rheology of the mixture and supports the formation of tobermorite.