Browsing by Author "Huang, Kaiwu"
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- Development and Testing of a Mobile Pilot Plant for the Advancement and Scale-up of the Hydrophobic-Hydrophilic Separation ProcessSechrist, Chad Michael (Virginia Tech, 2024-06-03)Fine particle separation is a grand challenge in the mining and mineral processing industry. The industry standard process, froth flotation, is extremely robust and adaptable; however, it is inefficient for particles less than 20 microns. Owing to this limitation, some mining sectors, such as coal, opt to discard the ultrafine particles to waste impoundments as the costs to recover and dewater these materials are prohibitive. The Hydrophilic Hydrophobic Process (HHS) is one alternative to flotation that uses a recyclable solvent, rather than air bubbles, to selectively recover fine hydrophobic particles. Prior laboratory, proof-of-concept, and demonstration-scale testing has shown that the HHS process is extremely efficient, having no effective size limitation. The purpose of this research was to continue the development and improvement of the HHS process, through the design, construction, and testing of a mobile pilot plant. The pilot plant would in turn be used to demonstrate the robustness of the HHS process through a systemic study of multiple coal sources and ranks. In addition, the pilot plant would serve as a testbed for inquiry-based process intensification, the development and evaluation of design criteria for the various unit operation. Through the course of this research, a 50 lb./hr. (product rate) pilot plant was constructed and commissioned. Initial investigations focused on the shakedown and design of key unit operations, including the agglomeration and de-emulsification (i.e. Morganizing) steps. Studies showed that the initial design of these units, namely pump induced mixing in agglomeration and packed bed emulsification in the Morganizer, were not adequate to meet production demands, and as such, these stages were redesigned after appropriate fundamental evaluations. After implementing the design changes, the pilot plant was successfully operated over a 7-month period, routinely producing bituminous products with less than6% ash and less than 10% moisture as well as anthracite products with less than 3% ash and less than 4% moisture. This study also evaluated a new approach to de-emulsification using a jig based Morganizer in place of the standard oscillating column Morganizer. The jig utilizes a pulsing mechanism to move liquid to break up agglomerates versus the mechanical disk stack. Preliminary results showed that the jig Morganizer was comparable to the oscillating unit at more than half the size. This new design provides a pathway for reduced cost, footprint, and improved scalability. Lastly, this study evaluated both the HHS process and dual-scan X-ray based particle sorting as means of increasing the REE content of coal-based materials. Data from a pilot-scale x-ray sorter showed the unit was capable of preconcentrating REEs to over 300 ppm, while data from the HHS similarly showed the process was capable of REE recoveries of 85-90% and of preconcentrating REEs above 300 ppm. Altogether, these results indicate That both of these technologies are capable of efficiently and cost effectively preconcentrate REEs from wastes streams at operating coal preparation plants.
- Fundamental Studies on the Extraction of Rare Earth Elements from Ion Adsorption ClaysOnel, Oznur (Virginia Tech, 2023-10-12)Rare earth elements (REEs) are critically important for high-tech, renewable energy and defense industries. However, rare earth minerals (REMs) are stable compounds, requiring aggressive conditions to decompose them for their extraction and use. One exception is the ion-adsorption clays (IACs) that are mined in South China. They were formed in nature via the adsorption of the REE ions on clay minerals; therefore, they can be readily extracted into solution under mild conditions using the ion-exchange leaching process using (NH4)2SO4 as lixiviant. It also happens that IACs are the largest source of the heavy rare earth elements (HREEs) that are critical, especially for the defense industry. At present, more than 80% of the HREEs are produced commercially from the IACs mined in Southeast Asia. The objective of the present research was to study the fundamental mechanisms involved in the formation and processing of IACs using the ion-change leaching process. The first part of the project was the synthesis of IACs by contacting kaolinite samples with known concentrations of rare earth chloride (REECl3) solutions at different pHs and analyzing the synthetic IACs for XPS studies. It was found that the REE adsorption on kaolinite stays constant in acidic pHs. At pH 7 and above, adsorption density increases sharply, possibly due to the formation of REE(OH)3 and/or REE(OOH). The IACs formed under these conditions responded well to the ion-exchange leaching process by reducing the pH to below 7. In the second part of the study, the effect of iron (Fe3+) species co-adsorbing with REEs on the kaolinite surface was studied. Unlike the colloidal phases of IACs formed at pH > 7, the synthetic IACs formed in the presence of iron did not respond to the ion-exchange leaching process using (NH4)2SO4 as lixiviant. This problem has been solved by subjecting the synthetic IACs to a reducing condition to convert the Fe3+ to soluble Fe2+ species at pH < 7. The driving force for the standard exchange leaching process is the large differences between the hydration enthalpies of the Ln3+ ions that are in the range of -3,400 kJ/mole and that of the NH4+ ions (-320 kJ/mole). In the present work, alkylammonium ions (CnH2nNH4+) of varying chain lengths were used as novel lixiviants and obtained excellent results. Since these are surface active species, their concentrations in the vicinity of the clay minerals that are negatively charged would be substantially higher than in the bulk. As a result, it was possible to achieve the same level of leaching efficiencies as obtained using ammonium sulfate at approximately ten times lower reagent dosages. One of the problems associated with extracting REEs from coal-based clays is that the REE concentrations are typically in the range of 300 to 600 ppm, which makes it difficult to extract the critical materials economically using ion-exchange leaching and other processes. As a means to overcome this issue, the REE-bearing particles, including IACs and REMs, were liberated by blunging and subsequently upgraded using the hydrophobic-hydrophilic separation (HHS) process. The results showed that blunging outperformed grinding in liberating the REE-bearing particles from the clayey materials in coal. It was shown that one can improve blunging by increasing the disjoining in the thin liquid films present between clay and other minerals by controlling the double-layer (EDL) forces. These findings should enhance our understanding of the fundamental mechanisms involved in upgrading critical materials and thereby increase the economic viability of REE recovery from coal-based materials.
- Modeling Flotation from First Principles Using the Hydrophobic Force as a Kinetic ParameterGupta, Mohit (Virginia Tech, 2024-03-15)Flotation is regarded as the best available separation method for the recovery of valuable minerals such as chalcopyrite (CuFeS2), sphalerite (ZnS), etc., from mined ores. Practically all metals humans use today are produced by flotation. The process relies on controlling the stability of the thin liquid films (TLFs) of water formed between minerals and air bubbles (wetting film), air bubbles (foam film), and mineral particles (colloid films). In flotation, a desired mineral is rendered hydrophobic by surfactant coating as a means to destabilize the TLFs, so that they can be attached to the hydrophobic air bubbles. A TLF ruptures when the disjoining pressure (or surface forces per unit area) of the film becomes negative, i.e., Π < 0. Thermodynamically, a wetting film can rupture when the contact angle (θ) of a mineral surface is larger than zero. It would, therefore, be reasonable to consider the roles of the surface forces to better understand the fundamental mechanisms involved in flotation. The surface forces considered in the present work included the electric double layer (EDL), van der Waals (vdW), and attractive hydrophobic (HP) forces. A flotation model has been developed by using the hydrophobic force as a kinetic parameter, which made it possible to track the fates of mineral particles of different of size, surface liberation, and contact angle to predict both recovery and grades for the first time. The model has been validated against the plant survey data obtained from an operating copper flotation plant. The simulation results obtained using the first principles model have been utilized to address the limitations of current flotation practices. One such limitation is the presence of slow-floating target minerals present in the cleaner-scavenger tails (CST) that are routinely recycled back to the rougher flotation bank as circulating loads (CLs) to allow longer retention times for the slow-floating particles for additional recovery. The simulation results show also that opening a flotation circuit by treating the CST streams separately in an advanced circuit can substantially improve the plant performance. One of the major limitations of flotation is that the coarse particles in a feed stream are difficult to recover due to the low hydrophobicity associated with poor surface liberation. A new flotation model developed in the present work suggests various ways to address the problem. One is to increase the hydrophobicity of the composite (poorly liberated) particles using the Super Collectors that can increase the contact angles to 150 -170o. Simulation results obtained using the model developed in the present work show significant financial benefits of using Super Collectors. Flotation is controlled by surface forces as noted above. As particle size becomes larger than 150 µm, however, the gravitational force comes into the picture and can override the surface forces. A new flotation cell has been developed to mitigate the effects of the extraneous force by decreasing the effective specific gravity (SG) by attaching air bubbles to facilitate levitation and by creating a pulsation to allow particles to move according to SGs independent of particle size, which should help increase the upper particle size limit of flotation. Surface forces in foam and oil-in-water emulsion films have been measured at different temperatures to determine the changes in thermodynamic properties of the thin liquid films (TLFs) of water confined between two bubbles and two oil drops. The results show that the films are destabilized by the attractive hydrophobic forces created during the course of building H-bonded structures in confined spaces, which entails decreases in enthalpy (H < 0) and entropy (TS < 0), the second term representing the thermodynamic cost of building the structures.
- The Production of Low Ash Coals Using the Hydrophobic-Hydrophilic Separation Process with Novel DevelopmentsYoumans, Nathan Charles (Virginia Tech, 2023-06-06)
- Solvent recovery from solvent-fine coal slurries by filtration and steam strippingHuylo, Michael; Huang, Kaiwu; Noble, Aaron; Yoon, Roe-Hoan; Qiao, Rui (Frontiers Media, 2023-08-22)Dewatering of fine coal is a significant industrial challenge with economic and environmental implications. Due to the lack of suitable dewatering technologies, fine coal particles are often discarded to waste impoundments, leading to substantial loss of valuable natural resources while creating environmental problems. The hydrophobic-hydrophilic separation (HHS) process is a unique solution to this problem. In this process, a recyclable solvent is used to simultaneously remove inorganic impurities (ash) and water from a run-of-mine fine coal slurry. A small amount of recyclable oil (or solvent) is added to a fine coal slurry so that the solvent can spontaneously displace the water from the surface of coal particles. The spent solvent is subsequently recovered and recycled in a closed loop. Here, we report the results obtained using two different solvents, i.e., pentane and hexane, to de-ash and dewater ultrafine coal and recover the spent solvent by filtration, followed by steam stripping. Most of the spent solvent can be recovered during the filtration step at 20 psig N₂ and at a 60 s filtration time. The residual solvent left in the cake was then recovered using steam under different conditions. The results showed that the residual solvent concentration could be reduced to <1,400 ppm after 10 s of steam stripping at 150°C and 15 psig.
- Surface Forces in Thin Liquid FilmsHuang, Kaiwu (Virginia Tech, 2020-01-10)Thin liquid films (TLFs) of water are ubiquitous in daily lives as well as in many industrial processes. They can be formed between two identical phases, as in colloid films between two macroscopic surfaces and foam films between two air bubbles; and between two dissimilar phases, as in wetting films. Stability of the colloids, foams, and wetting films is determined by the surface forces in the TLFs. Depending on the nature of the surfaces involved, the stabilities can be predicted using combinations of three different forces, i.e., the van der Waals, electrical double layer (EDL), and hydrophobic forces. The objective of the present work is to study the roles of these forces in determining the stabilities of the TLFs of water confined between i) an air bubble and a hydrophobic surface and ii) an oil drop and a hydrophobic surface, with particular interest in studying the role of the hydrophobic force. The first part of the study involves the measurement of the surface forces in the TLFs confined between bitumen drops and mineral surfaces. Deformation of bitumen drops has been monitored by interferometry while it approaches a flat surface. By analyzing the spatiotemporal film profiles, both the capillary and hydrodynamic forces have been calculated using the Young-Laplace equation and the Reynolds lubrication approximation, respectively, with the surface forces being determined by subtracting the latter from the former. The results are useful for better understanding the effects of electrolyte and pH on bitumen liberation and recovery by flotation and for developing a filtration model from first principles. The second part of the study involves the surface force measurement in wetting (flotation) films. Surface forces in the TLFs of water on silica surfaces have been measured using the force apparatus for deformable surfaces (FADS) using an air bubble as a force sensor. The measurements have been conducted in the presence of various cationic surfactants such as dodecylamine hydrochloride (DAH), and alkyltrimethylammonium chloride (CnTACl), electrolytes, and polymers. The results show that film stability and hence the kinetics of film thinning can be greatly improved by the control of bubble ζ-potentials, whose role in flotation has long been neglected in flotation studies. Force measurements have also been conducted in the TLFs of water confined between oil drops and hydrophobic surfaces. Stability of this type of film plays an important role in a process of using oil drops rather than air bubbles to collect hydrophobic particles from aqueous phase. The force measurements conducted in the present work show that hydrophobic forces are much stronger in water films formed between oil drops and hydrophobic surfaces than in water films formed between air bubbles and hydrophobic surfaces, which can be attributed to the differences in the Hamaker constants involved.
- Validation and Application of a First Principle Flotation ModelHuang, Kaiwu (Virginia Tech, 2015-08-18)A first principle flotation model has been derived from the basic mechanisms involved in the bubble-particle and bubble-bubble interactions occurring in flotation. It is a kinetic model based on the premise that the energy barrier (E1) for bubble-particle interaction can be reduced by increasing the kinetic energy (Ek) for bubble-particle interaction and by increasing the hydrophobic force in wetting films. The former is controlled by energy dissipation rate (𝜀), while the latter is controlled by collector additions. The model consists of a series of analytical equations to describe bubble generation, bubble-particle collision, attachment and detachment, froth recovery, and bubble coalescence in froth phase. Unlike other flotation models that do not consider role of hydrophobic force in flotation, the first principle model developed at Virginia Tech can predict flotation recoveries and grades from the chemistry parameters such as 𝜁-potentials, surface tension (𝛾), and contact angles (𝜃) that may represent the most critical parameters to control to achieve high degrees of separation efficiencies. The objectives of the present work are to i) validate the flotation model using the experimental data published in the literature, ii) incorporate a froth model that can predict bubble coarsening due to coalescence in the absence of particles, iii) develop a computer simulator for a froth model that can predict bubble coarsening in the presence of particles, and iv) study the effects of incorporating a regrinding mill and using a stronger collector in a large copper flotation circuit. The model validation has been made using the size-by-class flotation rate constants (kij) obtained from laboratory and pilot-scale flotation tests. Model predictions are in good agreement with the experimental data. It has been found that the flotation rate constants obtained for composite particles can be normalized by those for fully liberated particles (kmax), which opens the door for minimizing the number of flotation products that need to be analyzed using a costly and time-consuming liberation analyzer. A bubble coarsening froth model has been incorporated into the flotation model to predict flotation more accurately. The model has a limitation, however, in that it cannot predict bubble-coarsening in the presence of particles. Therefore, a new computer simulator has been developed to predict the effects of particle size and particle hydrophobicity on bubble coarsening in froth phase. In addition, the first principle flotation model has been used to simulate flotation circuits that are similar to the Escondida copper flotation plant to study the effects of incorporating a re-grinding mill and using a more powerful collector to improve copper recovery. The flotation model developed from first principles is useful for predicting and diagnosing the performance of flotation plants under different circuit arrangements and chemical conditions.