Brazil holds second place in world production of dicalcium phosphate, which represents the main source of phosphorus for complementing the mineral salt that makes up the daily feed for cattle, hogs and fowls. Considering the fact that the increase in consumption of phosphates due to the increased annual consumption of meat by the world population, development of the technology necessary to guarantee quality and productivity has become imperative in order to supply this competitive market. The requirement for BUNGE Fertilizantes S.A. to accompany the world trend, reflected by client suggestions for sales of bulk quantities, originated the search for a new technology to produce microgranulated dicalcium phosphate. Due to characteristics adverse to forming the microgranulated dicalcium phosphate grain (particle size, monocalcium phosphate and residual acidity), it has become necessary to apply a final product classification process to guarantee compliance with the physical specifications of the material at the moment of expediting to clients. The purpose of this dissertation is to perform a study of the classification system used for fluidization, seeking scale-up information for construction of an industrial unit to be installed at the Cajati Facilities of BUNGE Fertilizantes. Fluidization is utilized commercially in a wide range of processes such as: catalytic operations, cooling, drying, recovery, etc, it utilizes the elutriation effect in wich the relatively small components are entrained by the gas flow for physical classification of materials. Within this concept an effort was made to quantify the effects of operational and dimensional variables of the fluidized bed system: porosity of the distribuition screen, residence time and freeboard angle. In accordance with the main experimental results, a statistical analyses was made by multiple regression, thus obtaining parameters related to the isolated variables and the interactions among them. It was observed that the operational and dimensional conditions that promote the best Separation and Recovery efficiencies for the system were those for which the screen porosity was 11 %, the residence time was 5,34 minutes and the freeboard angle was 33,62o. On the basis of the optimum data obtained from the fluidization pilot system, an industrial system was designed for the Cajati Facilities, having classification capacity of microgranulated dicalcium phosphate of 100 Tons/h. The resultant Separation end Recovery efficiencies of the industrial system demonstrate an excellent application of technology for FBC (dicalcium phosphate) classification and the model obtained from the pilot project precisely predicts the efficiencies for industrial systems. Thus, the mathematic model obtained from the pilot plant can be used as a reference for design and scale-up of microgranulated dicalcium phosphate industrial classification units, having characteristics similar to those studied in this dissertation. / O Brasil ocupa o segundo lugar na produção de fosfato bicálcico, principal fonte de fósforo para complementação do sal mineral que integra a ração diária dos animais (bovinos, suínos e aves). Levando-se em consideração o crescimento do consumo de fósforo em decorrência do aumento anual do consumo de carne pela população mundial, torna-se imperativo o desenvolvimento de tecnologia para garantir qualidade e produtividade, visando atender a este mercado cada vez mais competitivo. A busca de uma nova tecnologia para a produção de fosfato bicálcico microgranulado originou-se da necessidade da BUNGE Fertilizantes S.A. acompanhar uma tendência mundial atendendo às sugestões de clientes para a venda a granel. Devido às características adversas para uma boa formação do grão do fosfato bicálcico microgranulado (diâmetro da partícula, fosfato monocálcico e acidez residual) faz-se necessário a aplicação de um processo de classificação do produto final para garantir o atendimento às especificações físicas do material no momento da expedição para os clientes. O objetivo deste trabalho é estudar um sistema de separação utilizando a fluidização, buscando informações de scale-up para o dimensionamento de uma unidade industrial a ser instalada no Complexo Industrial de Cajati da BUNGE Fertilizantes. A fluidização é usada comercialmente em uma grande variedade de processos, tais como: operações catalíticas, resfriamento, secagem, recobrimento, etc, e utiliza o efeito da elutriação, onde os componentes relativamente pequenos são arrastados pelo fluxo de gás, para a separação física dos materiais. Dentro deste conceito, busca-se quantificar os efeitos das variáveis operacionais e dimensionais de um sistema leito fluidizado: porosidade da placa distribuidora, tempo de residência e ângulo da zona de expansão. Conforme os principais resultados experimentais, foi feita uma análise estatística através de regressão múltipla obtendo-se os parâmetros relacionados às variáveis isoladas e interações entre elas. Observou-se que as condições operacionais e dimensionais que atingem as melhores eficiências de Separação e Recuperação para o sistema foram aquelas nas quais a porosidade da placa era de 11 %, o tempo de residência do material no leito de 5,34 minutos e o ângulo da zona de expansão (freeboard) de 33,62º. A partir dos dados ótimos obtidos no sistema piloto de fluidização foi dimensionado um sistema industrial para a Unidade da Bunge Fertilizantes em Cajati com capacidade de classificar 100 T/h de fosfato bicálcico microgranulado. Os resultados das eficiências de Separação e Recuperação do sistema industrial demonstram a excelente aplicação da tecnologia para classificação do FBC (fosfato bicálcico), e o modelo obtido no sistema piloto prevê, com uma boa precisão, as eficiências para sistemas industriais. Desta forma o modelo matemático levantado para o sistema piloto de leito fluidizado pode ser usado como referência para o dimensionamento ( scale-up ) de unidades industriais de classificação de fosfato bicálcico microgranulado, com características semelhantes ao estudado neste trabalho. / Mestre em Engenharia Química

This study aimed to evaluate the effect of the use of phytase exoenzyme and other mineral sources on the bioavailability of phosphorus , increased dietary energy and nutrient digestibility . The treatments were : sorghum with inorganic phosphate ( SFB ) , maize with inorganic phosphate ( MFB ) , sorghum meal, meat and bone meal ( SFco ) , sorghum with phytase ( SFV ) and without energy recovery and amino acids ( SFNV ) . 1400 birds were for performance reviews , which were determined feed intake , body weight , feed conversion real and traditional and viability . For the analysis of digestibility at 15 days were used 80 birds , which were subjected to total collection , now for carcass composition and mineralization of tibia were used 6 birds per treatment , where we proceeded to determine the dry matter , crude protein , ether extract , ash , gross energy housing , and calcium and phosphorus of tibia and carcass. Data were subjected to analysis of variance and means were compared by Tukey test at 5 % and viability Kruskal-Wallis test . There were no statistical differences in performance at 7 days of age and only 14 live weight was lower for the MFB , however at 42 days , body weight was greater for the SFB compared to the MFB . Digestibility at 15 days there was no statistical difference. For carcass composition, the SFV showed higher percentage of ether extract. The percentage of calcium MFB FCS and were lower compared with the SFNV and equal to SFco and SFV , and the phosphorus content of the SFV and SFNV showed higher values. The exogenous phytase enzyme is able to hydrolyze phytate and release phosphorus from vegetable source for assimilation by animals , thus acting as a substitute for vegetable sources of phosphorus. / Objetivou-se avaliar o efeito da utilização da exoenzima fitase e de outras fontes minerais sobre a biodisponibilização do fósforo, o incremento de energia da ração e a digestibilidade de nutrientes. Os tratamentos foram: Sorgo com fosfato bicálcico (SFB), milho com fosfato bicálcico (MFB), sorgo com farinha de carne e ossos (SFCO), sorgo com fitase com (SFV) e sem valorização de energia e aminoácidos (SFNV). Foram 1400 aves para as análises de desempenho determinou-se o consumo de ração, peso vivo, conversão alimentar real e tradicional e a viabilidade. Para as análises de digestibilidade aos 15 dias foram utilizadas 80 aves, que foram submetidas a coleta total de excretas, já para a composição de carcaça e mineralização das tíbias foram utilizadas 6 aves por tratamento, onde procedeu-se a determinação dos teores de matéria seca, proteína bruta, extrato etéreo, matéria mineral, energia bruta da carcaça, e cálcio e fósforo das tíbias e carcaça. Os dados foram submetidos a análise de variância e as médias comparadas pelo teste de Tukey 5% e a viabilidade pelo teste Kruskal-Wallis. Não houve diferenças estatísticas para o desempenho aos 7 dias de idade e aos 14 somente o peso vivo foi menor para o MFB, já aos 42 dias, o peso vivo foi maior para o SFB comparado com o MFB. A digestibilidade aos 15 dias não houve diferença estatística. Para a composição da carcaça, o SFV apresentou maior valor da porcentagem de extrato etéreo. A porcentagem de cálcio do SFB e MFB foram menores comparado com o SFNV e iguais para SFCO e SFV, e para o teor de fósforo, o SFV e SFNV apresentaram maiores valores. A enzima fitase exógena é capaz de hidrolisar o fitato de origem vegetal e liberar o fósforo para assimilação pelos animais, atuando assim como substituta de fontes vegetais de fósforo. / Mestre em Ciências Veterinárias

Roll compaction is a continuous process commonly used in the pharmaceutical industry for dry granulation of moisture and heat sensitive powder blends. It is intended to increase bulk density and improve flowability. Roll compaction is a complex process that depends on many factors, such as feed powder properties, processing conditions and system layout. Some of the variability in the process remains unexplained. Accordingly, modeling tools are needed to understand the properties and the interrelations between raw materials, process parameters and the quality of the product. It is important to look at the whole manufacturing chain from raw materials to tablet properties. The main objective of this thesis was to investigate the impact of raw materials, process parameters and system design variations on the quality of intermediate and final roll compaction products, as well as their interrelations. In order to do so, we have conducted a series of systematic experimental studies and utilized chemometric tools, such as design of experiments, latent variable models (i.e. PCA, OPLS and O2PLS) as well as mechanistic models based on the rolling theory of granular solids developed by Johanson (1965). More specifically, we have developed a modeling approach to elucidate the influence of different brittle filler qualities of mannitol and dicalcium phosphate and their physical properties (i.e. flowability, particle size and compactability) on intermediate and final product quality. This approach allows the possibility of introducing new fillers without additional experiments, provided that they are within the previously mapped design space. Additionally, this approach is generic and could be extended beyond fillers. Furthermore, in contrast to many other materials, the results revealed that some qualities of the investigated fillers demonstrated improved compactability following roll compaction. In one study, we identified the design space for a roll compaction process using a risk-based approach. The influence of process parameters (i.e. roll force, roll speed, roll gap and milling screen size) on different ribbon, granule and tablet properties was evaluated. In another study, we demonstrated the significant added value of the combination of near-infrared chemical imaging, texture analysis and multivariate methods in the quality assessment of the intermediate and final roll compaction products. Finally, we have also studied the roll compaction of an intermediate drug load formulation at different scales and using roll compactors with different feed screw mechanisms (i.e. horizontal and vertical). The horizontal feed screw roll compactor was also equipped with an instrumented roll technology allowing the measurement of normal stress on ribbon. Ribbon porosity was primarily found to be a function of normal stress, exhibiting a quadratic relationship. A similar quadratic relationship was also observed between roll force and ribbon porosity of the vertically fed roll compactor. A combination of design of experiments, latent variable and mechanistic models led to a better understanding of the critical process parameters and showed that scale up/transfer between equipment is feasible.