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By Atsushi Shibayama

The aim of this research was to develop a copper recovery process from mine tailings (0.34%Cu) using flotation followed by high-pressure oxidative leaching (HPOL) and solvent extraction. The results of HPOL using the concentrate of mine tailings obtained by flotation under the optimal conditions of the previous study shown that an efficient copper dissolution of 94.4% was achieved in an H2O media, while the copper concentration of PLS reached to be 2.9 g/L. The solvent extraction of PLS obtained from the optimal HPOL showed that 91.3% copper was recovered in stripped solution under the determined optimum conditions, in which the copper concentration achieved to be 44.8 g/L. Finally, a proposed copper recovery process from the concentrate of mine tailings was developed by combination of HPOL and solvent extraction, while a total copper recovery of 86% was achieved.

By K. Adham

For use in many existing and emerging applications, the purification of natural graphite is required to achieve +99.9% carbon content with minimum metallic impurities. Currently, the hydrofluoric acid process is used, which carries certain environmental and workplace health and safety impacts. While thermal purification of graphite at temperatures over 2500 °C is a known alternative, such high-temperature furnaces are expensive to build and operate. Using chlorine at lower temperatures to purify graphite is also known and patented, but is currently limited to treating solid synthetic graphite shapes in small-scale batch furnaces. Chlorine treatment of natural flake graphite resources can be used commercially, if certain drawbacks are addressed through process improvements that can be helped with the use of fluidized bed reactor technology.

By Shubin Wang

Copper(II) and nickel(II) are often recovered from ammoniacal alkaline solutions by solvent extraction using hydroxyoxime extractants: both copper(II) and nickel(II) are extracted from ammoniacal alkaline solutions and, from the loaded organic phase, nickel(II) is selectively stripped with a dilute acid followed by copper(II) stripping with an acid of higher concentration. Since a small portion of ammonia is co-extracted with copper and nickel, the extracted ammonia should be scrubbed using a dilute acid before metal stripping. In the present study, a mechanistic model has been developed in order to support design and control of this process. The equilibrium distribution ratios of copper(II), nickel(II), and ammonia at 298 K using LIX® 84-I (active component, 2-hydroxy-5-nonylacetophenone oxime) as the extractant are successfully correlated by considering the relevant equilibria. Based on these results, quantitative prediction of equilibrium distribution ratios in the process has been made possible, and suitable conditions for the efficient separation of copper(II) and nickel(II) are discussed.

By Xiaoming Huaa

The effect of the anodic polarization on the composition and morphology of the surface layer formed on chalcopyrite during ammonia–ammonium chloride leaching was investigated. The anodic polarization on the chalcopyrite electrode was used for oxidation and dissolution of chalcopyrite, and the resulting oxidized layers were characterized by XPS, SEM and optical microscopy. The results show that oxide layers exist on the chalcopyrite surface with or without any anodic polarization in the leaching solution at ambient atmosphere. However, the composition and morphology of the layers are strongly depended on the extent of polarization. The distribution of FeOOH and Fe2O3 within the oxidized layer was inhomogeneous for the sample at the open circuit potential (OCP). The composition and morphology of the oxidized layers which were formed at anodic potentials lower than 0.3 V versus SCE were similar to those of the chalcopyrite at the OCP. At anodic potentials above 0.4 V, the oxidized layers contained many cracks, and they were fragile and exfoliated. Furthermore, the sulfide had been oxidized to sulfur species with higher oxidation states. The oxidation of the chalcopyrite seemed to undergo a cyclically oxidative process that suggested growth and spallation of oxidation layers on chalcopyrite in a layer-by-layer sequence.

By Baptiste Laubie

Agromining is a phytotechnology aiming at producing commercial metal compounds from low-grade ores thanks to hyperaccumulating plants. The fern Dichranopteris dichotoma is a rare earth element (REE) hyperaccumulator, which naturally grows on former mine tailings in China. It accumulates up to 0.35% of REEs in its aerial parts. Different hydrometallurgical processes are currently developed to recover these elements directly from the biomass or from ashes after combustion. The process presented here consists of a direct extraction by EDTA solution, followed by precipitation with acid oxalic. Optimal precipitation pH and influence of organic matter are determined by modelling and by experimental studies. The final solid contains 4.3% of REEs, with calcium as the main cationic impurity (0.45% of the precipitate). The recovery yield is similar for major REEs and is around 70%. After optimization, upscaling of the process will allow the agromining development to recover REEs from secondary resources with more environmentally friendly techniques.

By Edward Peters

Scandium (Sc) has unique properties and is one of the more valuable elements in the periodic table. Scandium can be used in solid oxide fuel cells and to produce high strength aluminium alloys of value, for example, in the aerospace industry. Scandium is often grouped together with the rare earth elements (REE). Amongst others, scandium can be found in bauxite residues, so called red mud. It is possible to extract and enrich scandium from red mud by leaching and solvent extraction. Scandium can then be recovered from the pregnant strip liquor by crystallization. The strip liquor will however still contain certain impurity elements. In the present work, a method for obtaining a pure scandium solid phase by direct crystallization from the strip liquor is evaluated. It was found that Fe and Ti co-precipitate with Sc under the conditions employed.

By Cody Burcher-Jones

The recovery of rare earth elements (REEs) through heap leach/in situ techniques from so-called ion adsorption clays (IACs) is attractive due to their inherent simplicity. However, the underlying mechanisms of these processes are poorly understood. In this study, the deportment of REEs in a typical IAC material has been investigated and was found to concentrate in the phyllo-layers of the clays, especially hallyosite, and was readily desorbed by various ion-exchange reagents indicating various potential routes to liberate them. Here we are reporting the use of seawater (0.5 M NaCl), spiked with various amounts of (NH4)2SO4, and found better extraction using a reagent mixture than NaCl on its own. Further, the leaching of REEs from a bed of clay material was investigated over time to understand the rate of transport through the stagnant material. Results indicate that REE release is likely to be controlled by diffusion through the clay material, while desorption in agitated systems is rapid. A degree of fractionation between different REEs can be observed during diffusion. Nonetheless, the successful operation of in situ leach operations for this type of material would depend primarily on how easily solution cocktails can be made to flow through the bed material.

By Yury Kapelyushin

Formation of cementite in the reduction of hematite by CO–CO2 gas was studied in situ using high temperature XRD (HT XRD) analysis. Reduction of hematite was examined in the temperature range 873–1173 K by CO–CO2 gas mixture with high carbon activity. When carbon activity in the system was 1.5, cementite was formed only at 1023 K; it was not observed in experiments at 973, 1073 and 1123 K. Formation of cementite was observed at 923–1073 K when carbon activity increased to 3–5; and at 873 K when carbon activity was 10. Formation of cementite at 973–1073 K proceeded through metallic iron; however, in the reduction of hematite at 873 and 923 K, iron was not observed; cementite apparently was formed directly from wüstite. XRD spectra were used to estimate concentration of carbon in austenite in the process of cementite fromation.

By Jan Smit

Sulphidic copper concentrates are generally processed by pyrometallurgical means; while oxidative pressure leach processing of such materials has been shown to be technically feasible, there has traditionally been little incentive to choose this route in favour of a smelting option. However, for concentrates with elevated arsenic levels, oxidative pressure leaching offers distinct advantages, as smelter air emission standards and restrictions on concentrate importation have tightened. The current state of pressure leach technology allows for high copper extractions from arsenical copper concentrates, while producing an environmentally stable process residue, without atmospheric emissions of sulphur dioxide or arsenic. In its studies on pressure leaching of copper concentrates, Sherritt has shown that arsenical feed materials can be converted into environmentally stable residues, with excellent copper extractions. The results of recent batch and pilot plant test work are discussed, including the deportments of copper, arsenic and precious metals.

By E. Maziar Sauber

In order to prepare a more desirable feedstock for a rare earth elements separation refinery, cerium, a penalty element in the refinery feedstock, should be removed from the mixed rare earth elements oxide or carbonate feedstock. In this study, cerium (III) to cerium (IV) oxidation by calcium hypochlorite and subsequent precipitation was used to remove cerium from a mixed rare earth elements chloride solution. A factorial design of experiments was used to determine the effect of process variables such as temperature, pH, and oxidizer addition on the oxidation of cerium (III) using synthetic solutions. Under certain test conditions, all of the cerium was successfully removed from the chloride solution, and some REE accompanied cerium and reported to the precipitate. This proposed technology can allow for low cost removal of cerium from mixed rare earth elements chlorides.

By A. René Silva

The separation of Fe(III) from simulated Ni(II) solutions using different ion exchange resins was studied. The resins tested included cation exchangers with sulfonic and carboxylic groups and chelating resins with iminodiacetic, aminophosphonic, and mixed sulfonic and phosphonic groups. The dosage of resins was varied from 0.1 to 0.5 g/mL to study the impact of resin type and dosage on iron separation from simulated nickel leach solution containing 25 g/L Ni(II) and 25 g/L Fe(III) at pH 1.5. Also, the effects of different metal ion concentrations, Fe (III):Ni(II) ratios in solution, pH, and adsorption times were investigated. Experimental results demonstrate that all the chelating resins selected favored the adsorption of Fe(III) over Ni(II) with high Fe(III) loading. Soft cation exchange resins also favored the adsorption of Fe(III) over Ni(II), but no significant Fe(III) loading was observed. In contrast, strong cation exchange resins did not show adsorption preferences. The most efficient separation was observed using resin with aminophosphonic groups at resin dosage of 0.2 g/mL, having a Fe(III) adsorption over 94% and Ni(II) adsorption below 5%.

By Georgios Kolliopoulos

Water is a critical commodity of our generation and a key compound for the chemical and mining industries. Sustainable industrial development is directly associated with the ability to recover clean water from contaminated sources. Forward Osmosis (FO) is a low-energy footprint membrane process allowing the recovery of clean water from high salinity effluent streams. In FO, water is recovered spontaneously into a concentrated draw solution (CDS). Energy is required to separate the recovered water from the resulting dilute draw solution (DDS). In the current work, the fundamentals of the FO process and the most important aspects affecting its performance are discussed. An energy comparison of FO and conventional water recovery technologies is presented. Finally, the opportunities FO presents in the field of hydrometallurgy are analyzed.

By R. T. Seaman

Pressure oxidative treatment of whole ores and/or mineral concentrates is used to leach or liberate metals of value for downstream recovery. Silver, when present, is often lost in processing, precipitating as a cyanide-insoluble jarosite in the residue. Depending on pressure oxidation conditions, the degree of silver loss to jarosite can vary dramatically. Batch bench-scale testwork is often performed to define that loss, and then assess the implications in continuous operations. This paper focusses specifically on the impact of CESL pressure oxidation conditions on silver recovery, and discusses limitations of batch bench-scale testing as well as means of overcoming these limitations to better predict silver recovery in the scale up from bench-scale to continuous operations. Since silver is only partially soluble in both sulphate and chloride media, it will gradually leach and deport to a jarosite as oxidation progresses. When a silver-insoluble anion, for example iodide, is dosed prior to oxidation, there is a marked improvement in silver recovery from batchgenerated residue; however, that benefit is not consistently seen in continuous operations. The difference has been attributed to the dynamic solution conditions in the batch test, specifically the first few moments of oxidation. Using these principles, a predictive correlation has been established between initial leach concentrations of iron and acid and ultimate silver recovery with iodide addition.

By A. M. T. S. Bandara

The solubility of rare earth (RE) salts in aqueous solutions depends on many factors including the type of cations and anions in solution, their concentrations, temperature and the type of solid precipitated. Experiments were conducted using anhydrous La2(SO4)3 and Ce2(SO4)3⋅8H2O as solids and lanthanum(III) perchlorate prepared by dissolving La2O3 in HClO4 solutions as RE-sources. Solutions of H2SO4, H3PO4 and their mixtures in the presence or absence of Na+, Ca2+, Fe(III) or Al(III) as perchlorates served as test solutions. Saturated solutions and precipitated solids were assayed and characterized using standard techniques to show that the La(III) and Ce(III) ions precipitate as hydrated sulphates, phosphates or double salts with sodium, depending upon the solution composition. The change in solubility of RE-salts with solution composition and temperature is the result of the composite effect of changes in solubility products (pKSP) of salts, pKa of acids and other equilibrium constants for ion-association.

By In-Hyeok Choi

Currently, spent V2O5–WO3/TiO2 catalysts contribute significant amounts of solid waste following increasing levels of global demand. V2O5–WO3/ TiO2 catalysts usually consist of TiO2 anatase as a supporting oxide, vanadium as a catalytic agent, and other promoters such as tungsten, silicon, and calcium. Although vanadium is the main catalytic agent, a relatively high content of tungsten (WO3, 7–10 wt%) typically exists compared to vanadium (0.5–1.5 wt%). Considering the irreplaceable properties and industrial importance of tungsten, a feasible method for the recycling of spent V2O5–WO3/TiO2 catalyst should be established to utilize it as a secondary source. This paper presents a process to recover tungsten from spent V2O5–WO3/TiO2 catalyst. The processes proposed here involving roasting, decomposition using HCl, ammonia leaching, and crystallization. Within the process, ammonium paratungstate (71 wt% as WO3) is obtained as a final product. The total yield rate of tungsten from feedstock was found to be 96.3%.

By T. Feldmann

Despite the ubiquity of applications for germanium, there is a lack of practically useful solubility data in acidic solutions. Previous studies were done at ambient temperature and only for commonly used acids (H2SO4, HCl). Hence, an investigation of the solubility of GeO2 in different acids was undertaken. Several inorganic and organic acids were studied in the concentration range of 1–11 mol/L and at 23, 40, and 60 °C. In the case of H2SO4 and HCl previous data was confirmed. Lower acidity resulted in a higher solubility for Ge at all tested temperatures. Tests done at 40 and 60 °C and low to moderate acidity levels, gave slightly increased solubility values at higher temperatures compared to 23 °C. This wasn’t the case at higher acidity levels, i.e., the solubility curves at different temperatures converge at high acidity. Lastly, a relationship of water activity and GeO2 solubility in different acid media was established.

By Shivendra Sinha

Total pressure oxidation (TPOX) is widely outreached leaching practice for base metals from sulfide minerals, wherein high temperature (T ∼ 200 °C) and oxygen pressure (pO2 ∼ 25 bar) are required. These aggressive conditions intensify the oxygen mass transfer, and therefore facilitate metal dissolution. However, challenging-cum-negative aspects of such practice are energy and material intensive requirements and high oxygen demand. Thus, the present study explores the novel emulsified medium for enhancement of oxygen mass transfer, which assists faster metal dissolution at significantly lower temperature and pressure condition. It is possible to achieve quantitative dissolution (>95%) of Cu, Ni and Co from mixed sulfide minerals at T ∼ 95 °C and pO2 ∼ 2 bar using an emulsion of 2.5% (v/v) n-Hexadecane in dilute sulfuric acid. In addition, n-Hexadecane was found to be inert, stable and immiscible in a pressurized leaching system, thus can be easily separated and recycled in subsequent leaching stages. Thus, this study offers an energy efficient route for low temperature-pressure leaching of sulfides.

By Alexandra Anderson

A computational fluid dynamic (CFD) model has been developed using ANSYS Fluent 17.0 to help identify areas of high wear within the refractory lining of a secondary lead reverberatory furnace. Once a base case simulation was validated using data from an operational furnace, areas of potentially high refractory wear were determined through the calculation of the temperature and velocity distributions within the furnace and on the hot face of the refractory lining. The CFD model was used to assess whether the predicted areas of high refractory wear could be minimized through changes burden geometry. The results showed that shape of the burden geometry greatly affected the overall flow patterns and heat transfer within the furnace.

By Colin Dessemond

Since 1950, the traditional process has been dominating the production of lithium compounds from spodumene ores to sustain the lithium market because of its economic viability and the markets need for technical grade (99.5% purity) product. This traditional process includes thermal conversion, acid roasting and lithium leaching. However, this process has not been challenged and very few studies have tried to explain its limitation (95% lithium yield) or optimize the thermal treatment. Here, α to β spodumene conversion and lithium extraction were performed in a rotary kiln on a 2 mm to 2 cm spodumene concentrate instead of a micrometric one using a 1050 °C, 30 min conversion treatment and 250 °C, 30 min, 30% H2SO4 excess leaching treatment. X-Ray Diffraction analyses were performed on the converted material to determine the conversion rate by Rietveld analysis. It was observed after thermal treatment that the α-spodumene particles fractured and divided while the impurities remained compact. A sifting was performed after thermal treatment and it was determined that 65% of the initial mass became finer than 180 μm. X-Ray diffraction analyses and lithium content measurement were performed on both fractions and it was determined that the finer fraction had a very high lithium content of 3.24 wt%. Lithium extractions were performed on both fractions separately. While the coarser fraction’s lithium yield was only 61% the finer fraction’s lithium yield went up to 99% without any additional treatment. These observations may open more economical ways for the traditional process by potentially bypassing two third of costly steps such as grinding.

By G. T. Lapidus

One of Society’s major concerns with hydrometallurgical processing is the large amount of water that is quintessential to its nature. This is especially troubling in arid areas, where the population struggles to procure potable water for their daily needs. For that reason, it has become our responsibility to conceive, design and implement processing schemes that not only use as little water as possible, but recycle streams within the plant itself and minimize waste that exits its perimeter. With this in mind, the conference will center on the importance of selecting the appropriate chemical systems and integrating material balances to avoid reagent overkill and to detect impurity accumulation. The three “R’s” (reuse, recycle and recovery) of aqueous solutions within the processes are emphasized. Examples of processes for the recovery of lead, copper, precious and PG metals from minerals and waste materials will be presented.