Column flotation cells have become the most popular machine designed for industrial applications that require the separation and concentration of wanted or unwanted minerals from the rest material associated in a pulp. To achieve this process separation an air sparging device, which is required to produce bubbles in the flotation cell is required. In column flotation operations, Sparger sparging devices are employed in column flotation operations to generate small bubbles into the cell with the aim to carry the the desired mineral to the surface for later be recovered and proceeded. However, field studies suggest that air injector sparging systems are not always optimized. Two of the reasonsReasons that contributinge to the lack of optimization areis unfavorable state are: (i) ineffective internal design of the sparging system, and (ii) poor operation techniques employed inby the industrial processing industrial plants. The present project intends to better understand sparging performance into the column cell and how to optimize sparging systems more effectively. To achieve this end, With this in mind, data of for gas-water injection rate, froth addition, and inlet-pressure have been collected and analyzed. The This data not only will facilitate an insight of to better operational practices that plant operators can employ to improve column performance, but it also will make it possible to correct flaws in the design of the sparging systems currently used in column flotation operations. / Master of Science

Column flotation is commonly employed in the processing and recovery of fine mineral particles due to an increase in flotation selectivity unattainable using conventional flotation methods. Such an increase in selectivity is due to the employment of wash water, minimizing hydraulic entrainment of fine gangue particles, and the presence of quiescent operating conditions assisted by the use of various air sparging technologies. High performance air spargers increase the probability of collision and attachment between air bubbles and particles, thereby improving recovery of fine and coarse mineral particles otherwise misplaced to the tailings fraction in conventional flotation cells. Although many high-pressure spargers, including the static mixer and cavitation tube, are currently employed for the aeration of column cells, a low pressure sparger capable of providing equivalent performance while resisting a reduction in aeration efficiency does not exist. In light of escalated energy requirements for operation of air compressors necessary to provide high pressure air to existing external and internal spargers, a low-pressure and porous sparger capable of resisting plugging and scaling was developed. Following the design, construction, and optimization of such a prototype, air holdup and flotation performance testing was completed to verify the viability of the sparger as a replacement to existing aerators. Performance evaluations suggest that the sparger is capable of providing similar functionality to currently employed sparging technologies, but further work is required with regards to manipulation of the porous medium to prevent sparger fouling and sustain high aeration efficiencies. / Master of Science

The potential for improved selectivity has made column flotation cells a popular choice for upgrading fine coal. Unfortunately, recent production data from full-scale column plants indicate that many industrial installations have failed to meet original expectations in terms of clean coal recovery. Theoretical studies performed using a simple dispersion model showed that this inherent shortcoming could be largely minimized by reconfiguring the columns to operate in series as a cell-to-cell circuit. Follow-up field data showed that this low-cost modification increased flotation recovery as predicted by the dispersion model. This study presents the key findings obtained from the field investigation and provides generic guidelines for designing multi-stage column circuits. / Master of Science

Froth flotation is a widely used, cost effective particle separation process. However, its high performance is limited to a narrow particle size range, e.g., between 50 µm and 600 µm for coal and between 10 µm and 100 µm for minerals. Outside this range, the efficiency of froth flotation decreases significantly, especially for difficult-to-float particles of weak hydrophobicity (e.g., oxidized coal). Nanobubbles integrated into a specially designed column flotation expanded the particle size range for efficient froth flotation as a result of increased probabilities of particle- bubble collision and attachment and reduced probability of detachment. The major advantages of nanobubble enhanced flotation include lower collector and frother dosages since nanobubbles that are mostly smaller than 1 µm can be formed selectively on hydrophobic coal particles from dissolved air in coal slurry. Nanobubbles act as a secondary collector on particle surfaces, thereby resulting in considerably lower operating costs. A systematic parametric investigation of the proposed technology was performed to understand the effects of process variables on separation performance with a typical coal sample using a specially designed flotation column and three 10-liters conventional flotation cells. Results indicate that the combustible recovery of a -150 µm coal increased by 5-50% in the presence of nanobubbles, depending on process operating conditions. Nanobubbles also significantly improved process separation efficiency and increased the flotation rate constant by more than 40%. Theoretical evaluation of the innovative flotation technology was employed using specially designed apparatus to study the nanobubbles stability and the roles of nanobubbles on particle-bubble interactions, froth stability, and surface area flux. In addition, a detailed technical performance and economic evaluation was performed.

A new fine-coal cleaning circuit, with potential near-term applications, has been evaluated for treating fine coal (i.e., 28 mesh x 0). This circuit combines a surface-based separator known as Microcel™ column flotation with an enhanced gravity separator known as the Multi-Gravity Separator (MGS). The synergistic effect of combining both processes in a single circuit resulted in improved ash and pyritic sulfur rejection with minimal losses in energy recovery. In addition, technical and economic analyses of this processing scheme suggest it compares favorably with existing post-combustion desulfurization techniques. A detailed study of the MGS included the development of a model based on fundamental principles of fluid mechanics and mineral processing. The theoretical analyses identified drum speed as the most important MGS operating parameter. To validate these findings, a detailed parametric test program was conducted using coal samples from the Pittsburgh No. 8 and Illinois No. 6 seams. A statistical analysis of the test data also showed that drum speed was the most important variable in controlling the performance of the MGS. The other controlling parameters, i.e., feed percent solids, feed rate and wash-water addition rate, were found to be of lesser importance. The experimental test results were found to be in good agreement with the theoretical predictions obtained using the model. / Ph. D.

Coal in the finer particle size ranges (below 1 mm) has always suffered from poor cleaning efficiencies. This problem has been exacerbated in recent years with the increased amount of high ash fines due to continuous mining machines and the mining of dirtier coal seams. In the present work, it is proposed to improve overall plant efficiencies by processing coarser coal in column flotation than is now commonly treated by that method. Column flotation for coarse coal is supported by actual lab and plant test data that result in a full-scale column plant installation. The fundamentals of coarse particle detachment from bubbles are reviewed and a new simplified model is developed which better handles cubical and rectangular coal particles. Much of the lower efficiency of fine coal cleaning is due to poor size separation of the fine-sized raw coal which results in misplaced high ash fines reporting to the coarser size streams. By sending coarser material to column flotation, the finest size separation that takes place in a plant can be as coarse as 0.5 mm or greater. The proper use of wash water in a flotation column then becomes the best mechanism for desliming of the high ash clays. This work quantifies the benefits of removing the high ash fines from the plant product and increasing overall plant yield by increasing the amount of near-gravity coarse material. The resulting yield gain is greater than that obtained from only the increased fine coal recovery. Methods of column operation for improved coarse coal recovery are also evaluated. / Ph. D.

The core of this project was the development of a column flotation dynamic model that can reasonably predict the changes in the concentrations of all solid and bubble species, along the full column height. A dynamic model of a process is normally composed of a set of partial or ordinary differential equations that describe the state of the process at any given time or position inside the system volume. Such equations can be obtained from fundamental material and/or energy balances, or from phenomenological derivations based on knowledge about the behavior of the system. A phenomenological approach referred to as population balance modeling was employed here. Initially, a two-phase model was formulated, which represents the behavior of the gas phase in a frother solution. The column was viewed as consisting of three main regions: a collection region, a stabilized froth and a draining froth. Experiments were carried out, based on conductivity techniques, for obtaining empirical data for model validation and parameter estimation. After testing the two-phase model, the equations for the solid species were derived. Consideration of the effects of bubble loading, slurry density and slurry viscosity on bubble rise velocity and, therefore, on air fraction is included in the model. Bubble coalescence in the froth is represented as a rate phenomenon characterized by a series of coalescence efficiency rate parameters. Auxiliary equations that help describe the settling of free particles, the buoyancy of air bubbles, and the processes of attachment and detachment, were also developed and incorporated into the model. The detachment of solids from the bubbles in the froth zones was attributed to coalescence, and it was assumed to be proportional to the net loss of bubble surface area. Almost all parameters needed to solve the model equations are readily available. The set of differential equations that comprise the model can be solved numerically by applying finite difference approximation techniques. An iteration has to be performed, which involves calculating the product flowrate at steady state, modifying the tailings rate and solving the model again until a mass balance is satisfied. / Ph. D.

Le procédé Solvay génère d’énormes quantités de saumures résiduaires au pH alcalin contenant portlandite, brucite et silicates de calcium hydratés. La carbonatation conduit à un abaissement du pH, ce qui favorise la formation de deux phases majoritaires : la calcite et le gypse. L’objectif de la thèse est de valoriser les saumures résiduaires carbonatées par séparation des phases en colonne de flottation. L’étude de la carbonatation en réacteur batch, puis en colonne de carbonatation pilote montre qu’il est préférable de ne pas carbonater les saumures résiduaires jusqu’à l’équilibre thermodynamique. En effet, la mise en solution de métaux lourds intervient à partir d’un pH de l’ordre de 7,5, ce qui limiterait les rejets des saumures dans l’environnement. En outre, une carbonatation brusque et incomplète est souhaitable pour une meilleure séparation des phases par flottation. Les essais de flottation réalisés sur une colonne de 7,6 cm de diamètre et de 3 m de haut ont montré une faisabilité de la séparation des deux minéraux calciques avec l’oléate de sodium comme collecteur malgré une abondante littérature incitant à la prudence. La différence entre la taille des particules de carbonates et celle des particules de sulfates et leurs hydratations de surfaces, ainsi qu’une force ionique élevée du milieu permettent une bonne séparation des phases. Une étude des saumures synthétiques permet de mettre en évidence le rôle des cations métalliques (nature, rayon, charge…) sur la coalescence des bulles dans les conditions dynamiques et dans un milieu à forte force ionique. Une étude des paramètre de fonctionnement effectué sur une colonne de 30,5 cm de diamètre et de 10 m de haut ont permis la modélisation du procédé de flottation en colonne dans le but de proposer une procédure de dimensionnement du procédé industriel. La confrontation des résultats de simulation aux résultats réels permet la détermination des intensités des microprocessus de flottation (attachement/détachement), et conduit à la proposition d’une installation industrielle avec deux colonnes de flottation en série / Solvay process generates huge amounts of waste brines at alkaline pH containing portlandite, brucite and calcium silicate hydrates. Carbonation leads to lowering of pH which favors formation of two predominant phases: calcite and gypsum. The aim of this thesis is to develop carbonated waste brines valorization by phase separation in flotation column Study of carbonation in a batch reactor and in a carbonation pilot column shows it is preferable not to carbonate waste brines until thermodynamic equilibrium. Indeed dissolution of heavy metals occurs from a pH of about 7.5 thereby limiting discharge of brines in the environment. In addition, a sudden and incomplete carbonation is appropriate for phase separation by flotation. Flotation tests carried out in a 7.6 cm diameter and 3 m high column showed feasibility of the separation of the two calcium minerals using sodium oleate as a collector despite abundant literature for caution. The differences between the particle size of carbonates and sulfates and their surface hydration, as well as the high ionic strength of the medium allow an efficient separation of phases. Study of synthetic brines highlights the role of metal cations (nature, radius, charge…) on bubble coalescence in dynamic conditions in an environment with high ionic strength. Study of operation parameter performed on a 30.5 cm diameter and 10 m high column enabled the modeling of the column flotation process in order to provide a scale-up procedure of industrial process. Comparison of simulation results with actual results allows the determination of intensities of flotation subprocesses (attachment/detachment), and led to the proposal of an industrial plant with two flotation columns in series

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / Irreplaceable element for life, phosphorus is the main component of apatite, a mineral present in phosphate rock. The increasing in agriculture productivity would not be possible without the use of fertilizers. However, being a non-renewable resource, the phosphorus is susceptible to depletion. The exploitation of economically mineable deposits of phosphate ore leads to large losses of phosphorus in the stage of processing. In contrast, the demand for fertilizers in the country only increases. Currently, more than half of world production of phosphate concentrate is produced by flotation. The column flotation has been adequate to the processing of complex and low grades ores, that is the case of Brazilian deposits, and also fine size ranges. However, difficulty in concentrating ores of igneous origin may be aggravated in the presence of dissolved ions in process water used in flotation, since the recirculated water increases the ionic concentration. According to the literature, the process of concentration of apatite is strongly affected by the presence of ionic species, since they interact with the surface of apatite particles by changing the efficiency of the flotation process. Thus, the aim of this work was to evaluate the influence of water contaminated with ions F-, Ca2 +, Mg2 + and PO43- provides in the performance of apatite flotation or, in other words, in recovery, P2O5 content and selectivity of the process, to the coarse and fine ores carried out in a flotation column. And through central composite design (CCD), the influence of these ions in the apatite recovery and P2O5 content for low and high concentrations of contaminants. The results showed that the individual effect of each ion studied provided a substantial decrease in recovery, with different sensitivity to the size ranges studied. The most expressive decreases in apatite recovery are related to contaminants calcium and phosphate, where the first had a maximum reduction in the recovery of 58 and 51% for the coarse and fine, respectively, since the calcium consume the collector, reducing the amount available for the apatite collection. Phosphate confirms its strong depressant effect on the apatite particles, since for the coarse particles, there was a reduction in maximum recovery of 55% and 59% for the fines. For the contaminant magnesium, it is clear the critical effect on the process selectivity, related to the gangue minerals Fe2O3 and SiO2, since P2O5 content, in the presence of this ion, suffered a considerable decrease (up to 8 percentage points), independent of particle size. Magnesium, that also react with the collector, was responsible for the sharp increase in the consumption of NaOH, used to adjust the pulp pH, reaching up to 4 times higher compared to the standard test. The influence of fluoride ion represented an increase in the ratio of selectivity P2O5/SiO2, especially for the fine material, indicating a possible depressing effect on the silicate gangue. For the CCD, carried out at low contaminants concentrations, it is clear the interactions between calcium and magnesium with phosphate, contributing to the increase in the recovery, and between magnesium and fluoride, which contributed to the increase in the P2O5 content. This behavior is probably due to the fact that these ions form insoluble compounds among them, removing these ionic species from the system. As for the CCD performed to high contaminants concentrations, all the flotation tests resulted in very low values of recovery and grade. This fact may be associated with the formation of colloidal precipitates in large quantities, leading to indiscriminate coating of the mineral particles present, including apatite, preventing the reagents action. / Elemento insubstituível para a vida, o fósforo constitui o principal componente da apatita, mineral presente na rocha fosfática. O crescente aumento da produtividade na agricultura não seria possível sem o uso dos fertilizantes. Entretanto, por ser um recurso não-renovável, o fósforo está suscetível ao esgotamento. A exploração dos depósitos economicamente lavráveis de minério fosfático leva a grandes perdas de fósforo na etapa de beneficiamento. Contrariamente, a demanda por fertilizantes no país só aumenta. Atualmente, mais da metade da produção mundial de concentrado fosfático é produzido por flotação. A coluna de flotação tem se mostrado adequada ao beneficiamento de minérios complexos e de baixos teores, caso das reservas brasileiras, e também de granulometria mais fina. No entanto, a dificuldade em concentrar minérios de origem ígnea pode ser agravada quando em presença de íons dissolvidos na água de processo empregada na flotação, uma vez que a água recirculada aumenta a concentração iônica presente. De acordo com a literatura, o processo de concentração da apatita é fortemente afetado pela presença de espécies iônicas, uma vez que estas interagem com a superfície da partícula de apatita alterando a eficiência do processo de flotação. Sendo assim, este trabalho teve por objetivo avaliar a influência que a água contaminada com os íons F-, Ca2+, Mg2+ e PO43- acarreta no desempenho da flotação em coluna de apatita, ou seja, na recuperação, teor de P2O5 e seletividade do processo, para minério de granulometria grossa e fina, e, por meio de planejamento do tipo composto central (PCC), a influência destes mesmos íons na recuperação e teor de P2O5 para baixas e altas concentrações de contaminantes. Os resultados obtidos permitem concluir que o efeito individual de cada íon estudado proporcionou uma substancial queda na recuperação, apresentando diferente sensibilidade em relação à faixa granulométrica empregada. Os resultados mais expressivos de queda na recuperação são referentes aos contaminantes cálcio e fosfato, onde o primeiro teve uma redução máxima na recuperação de 58 e 51% para o material grosso e fino, respectivamente, em virtude do cálcio consumir o coletor, reduzindo a quantidade disponível para a coleta de apatita. O fosfato confirma seu forte efeito depressor sobre as partículas de apatita, visto que, para os grossos, houve uma redução máxima na recuperação de 55% e de 59% para os finos. Para o contaminante magnésio, fica claro o efeito crítico na seletividade do processo, em relação aos minerais de ganga Fe2O3 e SiO2, uma vez que o teor de P2O5, quando em presença deste íon, sofreu uma considerável queda (até 8 pontos percentuais), independente do tamanho de partícula. O magnésio, além de reagir também com o coletor, foi responsável pelo aumento acentuado no consumo de NaOH, utilizado para regular o pH da polpa, chegando a ser 4 vezes maior, comparado ao teste branco. A influência do íon fluoreto representou um aumento na razão de seletividade P2O5/SiO2, principalmente para o material fino, indicando possível efeito depressor sobre a ganga silicatada. Para o PCC realizado a baixas concentrações de contaminantes, fica evidenciado as interações entre os cátions cálcio e magnésio com fosfato, contribuindo para o aumento da resposta recuperação, e entre magnésio e fluoreto, onde colaborou para o aumento da resposta teor. Este comportamento, provavelmente, é devido ao fato destes íons formarem compostos insolúveis entre si, sequestrando estas espécies iônicas do sistema. Já para o PCC realizado a altas concentrações de contaminantes, todos os ensaios de flotação resultaram em valores extremamente baixos de recuperação e teor. Este fato pode estar associado à formação de precipitados coloidais em grande quantidade, levando a recobrir indiscriminadamente as partículas minerais presentes, inclusive a apatita, impedindo a ação dos reagentes. / Mestre em Engenharia Química