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By Takahiko Okura

Most non-ferrous raw materials are associated with sulphur. To extract the metals, the sulphur is recovered typically as sulphuric acid or liquid SOz, On the other hand, natural gas may contain over 20% of hydrogen sulphide (HzS) and a huge quantity of elemental sulphur is produced through oil and gas refining processes in the world. A large fraction of the sulphur mined from natural sources is eventually returned to the earth as fertilizers, by-products of desulphurisation and neutralisation processes, or as fugitives to the atmosphere. However, the supply and demand for sulphur are in imbalance. Such situation urges to develop a new smelting process without sulphuric acid production. This paper briefly reviews the global sulphur balance and the technologies for recovering elemental sulphur. The core of this paper is a proposal to convert SO2 gas to elemental sulphur by using organic materials. Some results of thermodynamic calculations and experiments are presented.

Jan 1, 2003

By Ejike Emmanuel, Nwoye Chukwuka, Ogwuegbu Martin, Asuwaji Ayuk, Onyedika Gerald

"Microwave pre-treatment of cassiterite ore prior to leaching was carried out in an attempt to obtain high grade of Sn02 and to conserve the total energy expended during processing. Microwave treatment was selected due to the presence of associated minerals which behaves differently to microwave energy. Studies in this work showed that microwave pretreatment of cassiterite ore can be applied to increase the recovery of tin oxide within 5 minutes of leaching. Microwave treatment of the ore resulted in mineral liberation at all particle sizes. Tin oxide was separated from the major impurities via leaching in potassium hydroxide solution and precipitation, resulting in 98% Sn02 at pH 7.IntroductionIn the nineties, the available techniques used for ore processing and analysis in Nigeria was the solution methods of either alkaline fusion or acid digestion [1,2]. A process in which cassiterite is made acid soluble by reduction to SnO2 , which stabilizes by glass formation and the tin was extracted by leaching the glass with sulphuric acid, followed by electrowinning was reported [3,4]. In another study, Baba et al [5] studied the dissolution kinetics of a Nigerian casiterite ore in hydrochloric acid solution. The effects of acid concentration,temperature, particle size and stirring speed were examined. It was found that the dissolution rates of cassiterite depends on hydrogen ion concentration, H+, stirring speed and ore particle dimensions. These were believed to report low data due to incomplete solubilization of the ore minerals in aqeous medium [6]. Analytical chemists have used microwave heating devices routinely for the dissolution of metals, minerals and various chemical products in chemical analysis [7,8]. It offers faster heating rate and consequently faster dissolution rate than conventional heating. The principle of the dissolution of analytical samples has been applied to the leaching of various minerals contained in an ore or concentrate sample. Some researchers [9, 10] conducted microwave assisted leaching of laterite ores containing oxides of nickel, cobalt, and iron. The metals of these mineral components were converted into their chlorides by microwave heating (1200 W, 2450 MHz, Nz atmosphere) a mixture of the ore and ammonium chloride between l 77°C and 312° C for 4-5 min, followed by water leaching at 80° C for 30 min. Nickel and cobalt extractions were 70% and 85%, and respectively, and are comparable with roasting at 300°C in a conventional rotary kiln for 2 hours."

Jan 1, 2013

By S. Seetharaman

A mathematical model has been developed to evaluate the viscosities of melts at high temperatures. The viscous flow in liquid is described by the equation, {n = Aexp(AG*/RT)} based on the absolute reaction rate theory. The Gibbs energy of activation,{ AG* } is considered to be a function of the temperature as well as the composition of the melt. The model has been applied successfully to various metallic and slag systems from unary to quaternary. On the basis of this model, a relationship has been suggested to relate the Gibbs activation energy of viscosity to the Gibbs energy of mixing in binary metallic melts. The viscosities predicted from available thermodynamic data in the case of a number of binary metallic systems using this correlation show satisfactory agreement with the reported experimental values.

Jan 1, 1994

By A. Treverrow, G. A. Brooks, H. K. Worner

"The work by H.K Worner and co-workers at CRA in the 1960s, and early 1970s, established that molten metals could be refined continuously utilising counter current flow of metal and slag. Womer also demonstrated that counter current refining could produce highly refined metal products. These developments coincided with the advent of high intensity metallurgical reactors in both the ferrous and non-ferrous industries (e.g. BOS, Q-BOP and later Sirosmelt) that utilised high levels of gas injection to produce rapid stirring and very fast reaction. These new generation of high intensity metallurgical reactors allowed high tonnage rates through relatively small volume vessels.Whilst, it is well known that the counter current flow of reacting phases offers the potential of efficient mass transfer and high purity products, the application of counter current reactors to molten metal/slag systems has been criticized on the basis that they suffer from either low intensity or, alternately, from poor refining due to excessive dispersion. These criticisms relate to the balance between intensity and the refining capacity of a reactor. That is, whilst high levels of mixing transversely to the direction of flow promotes high mass transfer, longitudinal mixing (dispersion) is detrimental to refining. Of course, mixing in one direction invariably leads to mixing in other directions, thus creating a playoff between high mass transfer and excessive dispersion.This balance between intensity and refining has been the subject of recent studies overseas, and at"" the University of Wollongong, using cold modelling techniques to evaluate the effect of mixing on dispersion in a counter current refining launder. These studies have shown that for a given geometry and mixing regime, dispersion decreases with increasing flow of liquid phases. This means that whilst high mass transfer cannot be achieved in a refining launder without sacrificing the degree of refinement, there is no impediment to achieving high productivity through such a system, in fact, high through puts may favour good refining. Thus, it may be possible to match a high productivity smelting operation with a equally productive counter current refining stage."

Jan 1, 1996

By Rodney L. Williamson

Optimal estimation theory has been applied to the problem of estimating process variables during vacuum arc remelting (V AR), a process widely used in the specialty metals industry to cast large ingots of segregation sensitive and/or reactive metal alloys. Four state variables were used to develop a simple state-space model of the V AR process: electrode gap (G), electrode mass (M), electrode position (X) and electrode melting rate (R). The optimal estimator consists of a Kalman filter that incorporates the model and uses electrode feed rate and measurement based estimates of G, M and X to produce optimal estimates of all four state variables. Simulations show that the filter provides estimates that have error variances between one and three orders-of-magnitude less than estimates based solely on measurements. Examples are presented that verify this for electrode gap, an extremely important control parameter for the process.

Jan 1, 2001

By J. T. I. Poijärvi

Outokumpu Harjavalta Metals Oy operates copper and nickel smelters, three sulphuric acid plants and nickel refinery at Harjavalta and copper refinery and precious metal plant at Pori. The by-products of these plants are presented in this paper. The by-products of the smelters include products from slag cleaning of flash smelting furnaces and converters, flue dusts and smelter off-gases. Weak acid and sludges from cleaning of smelter off-gases and acids are the by-products of the acid plants. The by-products out of the copper refinery are crystallized metal sulphates and sludges from electrolyte purification, on which a co-production process of the copper tankhouse is based. The main by-products of the precious metals plant are products from anode slime treatment and platinum metal group concentrates in the recovery of precious metals. Sludges from nickel matte leaching and precipitates from solution purification are the by-products of the nickel refinery. The formation, treatment and processing as well as the research work done for the utilization instead of dumping of the by-products in the production of copper and nickel will also be discussed in this paper.

Jan 1, 1995

By M. D. Stephens

A new, one-step process for extracting titanium from titaniferrous materials has been demonstrated. In the process, depleted uranium tetrafluoride (DUF 4), a solid, is mixed with ilmenite (FeTi03) and heated to 900°C. Titanium is extracted in the vapor phase as titanium tetrafluoride (TiF4) and the DUF4 is converted to uranium-iron oxide. The process has been found to selectively fluorinate the titanium in ilmenite and is capable of producing high purity TiF 4 with very low iron content. TiF 4 can be collected by condensation or through reaction with a fluoride salt such as NH4F, KF, or NaF. The TiF4 produced from the process can be used to make titanium metal, titanium oxide, or fluorotitanate compounds. Since the fluorination process is highly selective for titanium, it avoids many of the separations and waste issues common to other titanium extraction processes.

Jan 1, 2001

By B. C. Blakey

Unlike most hydrometallurgical slurries, those containing significant concentrations of goethite are typically highly viscous and shear-thinning, even at solid volume fractions below 5%. The viscosity may also depend upon time. These characteristics must be taken into consideration in slurry transport and heating. The technical literature is replete with apparent contradictions regarding the viscous behavior of these slurries, which may be due, in part, to variations in viscosity-measuring techniques. We present techniques that yield consistent results suitable for use in process design. A striking degree of time-dependent behavior is demonstrated for a laterite slurry. Reliable methods to design and analyze tubular transport and heating systems for time-independent slurries are summarized. Rules of thumb are then offered to account for the effects of time-dependency.

Jan 1, 2000

By A. Tsubouchi, F. Noguchi, T. Takasu

"A high current density operation is desired to improve the productivity in copper electrorefining. However, a lot of problems still remain such as passivation at anode, dendritic deposition at cathode and impurity behavior during the electro refining.Effects of the current densitY on the morphology of copper deposition on the cathode, and passivation at the anode were investigated at various fluid velocity of electrolyte in the present study.Although a granular appearance of the copper deposition was obtained with increasing high current density, it was depressed by an increase of the fluid velocity of the electrolyte. A uniform deposition on the cathode was also observed when the fluid velocity of the electrolyte become higher. It was ascertained that passivation at the anode was suppressed by circulating electrolyte during electrolysis. INTRODUCTIONIt is desirable to operate at high current density in copper electrorefining in order to improve plant productivity without enlarging the size of electrodes(1). However, there are many problems in copper electrorefining at high current density with the usual commercial practice, for example, anode passivation, dendritic deposition and an increase of impurities in the cathode.In general, it is effective to agitate the electrolyte in order to suppress these problems(2). Smith et a1.(3) have performed electro refining experiments at various current densities in the range of 8 to 32 Aldm2 and at electrolyte fluid velocities in the range of 40 to 120 mlmin, and they obtained well consolidated, void free copper even at high current density in a high electrolyte velocity. However, they did not discuss the recovery ratio and the passivation behaviour at the anode. Walsh et a1.(4)(5)(6) experimented with the rotating cylinder electrode, and ascertained that electrolysis can be carried out at high current densities under the condition of pure electrolyte.With regards to anode passivation, there are several papers by previous workers(7)(8). Our group ascertained the process of producing anode slime during electrolysis(9). However, these experiments were carried out without forced circulation of electrolyte. Therefore, in the present study, to solve these problems, we electrolyzed at current densities in the range of 4 to 50 Aldm2 with circulating electrolyte in the range of 0 to 48 mlrnin. The effect of electrolyte fluid velocity on the surface morphology of deposited copper at cathode and passivation at anode were investigated when electrolysis were carried out with circulating electrolyte at high fluid velocity and at high current density."

Jan 1, 1997

By Eren Hüseyin Obuz

In this study, the leaching kinetics of rare-earth elements were investigated using HCl and HNO3 solutions. A standard crushed complex ore was utilized as raw material. The complex ore (particle size of under 54 μm) contains REE (Ce, La, Nd, Pr, etc.). Different leaching durations were selected for the kinetic studies. The highest leaching efficiency was obtained in HCl solution, and the leaching mechanism was identified to diffusion through a product layer. The rate constants of Ce, La, Nd, and Pr were calculated as 1.08 × 10−2, 0.86 × 10−2, 1.87 × 10−2, and 1.34 × 10−2 h−1, respectively.

By Susanne Pignolet-Brandom

Reflected light microscopy, and scanning electron microscope energy dispersive spectroscopic analysis and backscatter electron images were used to determine if a "slick dross" with undesirable handling properties has an assemblage of phases distinct from normal dross. This study has found that in the normal dross the most abundant lead phases are lead sulfide and lead metal and the most common copper phases are copper-iron sulfide and copper sulfide. In the slick dross, the most abundant copper phase is copper-lead sulfide and the most common lead phases are copper-lead sulfide and lead sulfide. The resulting mineralogical information has provided additional insight into the causes of the handling problem and the reaction mechanism for the formation of normal and slick dross

Jan 1, 1988

By Merete Tangstad, Fei Li

This paper studies the quartz and carbon black pellets at elevated temperature with varying temperature and gas atmosphere. High-purity quartz and commercial ultra-pure carbon black was mixed (carbon content wt.15%), and then pelletized into particles of 1-3mm in diameter. The stoichiometric analysis of the pellet during heating is studied in thermogravimetric analysis (TGA) furnace at different temperature in CO and Ar atmosphere. The microstructure, phase changes and element content of sample before/after heating is characterized by X-ray diffraction, scanning electron microscope, X-ray fluorescence and LECO analyzer. The reaction process can be divided into two stages. Higher temperature and argon atmosphere are the positive parameters for SiC formation.

Jan 1, 2016

By J. S. Pitsillos

A new furnace tapping technique involving the simulation of a control valve at the exit to a furnace is being investigated. The purpose of this new tapping technique is to regulate the flowrate of liquid furnace products( slags, metals and mattes). Numerical modelling and experimental work has been carried out on tapping of slags leaving a SIROSMELT reactor and the results found to be in good agreement. Numerical modelling has also enabled prediction of the important industrial conditions for the onset of blockage from the shape of the pressure versus flowrate curves. Slag launder experiments have been carried out and a one-dimensional heat transfer model was used to evaluate the effectiveness of launder covers and different coolants. From the experimental results and mathematical model some launder design guidelines such as inclination angle, covers and coolants have been developed.

Jan 1, 1991

By Broggi Andrea

Condensates produced by SiO(g) and CO(g) have a crucial importance in silicon production. Condensation will follow the reactions 3 SiOðgÞ+COðgÞ→ 2 SiO2 + SiC and 2 SiO ðgÞ→Si+SiO2. Solid compounds generated during silicon production contain Si, SiO2 and SiC in different microstructures and amounts. In industrial systems, condensates limit the SiO(g) escape to the off-gas system. On the other hand, they can block the gas flowing from the high temperature zone, hence the necessity of studying an optimized condensation process. This review discusses SiO(g) condensation and its interaction with CO(g). The report gives an overview of the condensates found both at laboratory and at industrial scale. The two main compounds are the Si–SiO2 and the SiOx–SiC mixtures. The hypothesis on the mechanism of formation of SiC–SiOx condensates is presented through a wide selection of performed works. The advantages and disadvantages of the former experimental procedures are discussed.

By Na Wang, Chao Du, Hongmin Zhu, Kai Huang, Shuqiang Jiao

"Niobium aluminides were directly synthesized by a sodiothermic reduction process of NbC15 - AlCb which was dispersed into LiCl - KCl - NaCl - CaCb melts. The melt supplied a homogenous reaction medium which was substantially beneficial to the co-reduction of Nb and Al to form niobium aluminides in situ. The reduction was performed at 500°C for 4 hours. The products were analyzed by X-ray diffraction (XRD) and scanning electron microscope (SEM). The corresponding results indicated that niobium aluminides powders were successfully synthesized.1. IntroductionNiobium aluminides have received considerable attention as high-temperature structural materials, due to their high melting points, relatively low density, high strength, excellent oxidation and creep resistance [1-4]. Figure 1 shows that there are three intermetallic compounds in the Nb - Al binary [5], which includes Nb3Al (A15 structure, Cr3Si type), Nb2Al (D8b structure, cr-CrFe type) and NbAb (D022 structure, TiAb type). These niobium aluminides have been used in turbine blades or in stationary gas turbines [6-8]. However, despite their attractive features, the ir applications are still limited by the long and costly fabrication process [9, 10].Niobium aluminides were industrially fabricated by the mechanically alloyed process [11-13]. Traditionally, niobium is extracted from Nb2O 5 or K2NbF7 by a metallothermic reduction process while aluminum is produced by the Hall-Heroult process of Ah03 electrolysis. Based on the extraction of Nb and Al, respectively, niobium aluminides is synthesized by a mechanical powder alloying process. The present process for making niobium aluminides requires a set of complicated equipment, has high production cost and time consuming [14, 15].The purpose of this work is to present the simple, economic and direct synthesis of niobium aluminides powders utilizing a sodiothermic reduction from NbC15 - Al Cb dispersed into molten salts."

Jan 1, 2011

By O. Barbosa F.

The thermochemistry of the systems SCN-H2O, Au-SCN-H2O and Ag-SCN-H2O is discussed. Potential-pH diagrams at 25°C are drawn for each system considering several sets of concentrations of the species involved. The information provided by the potential-pH diagrams is.complemented by distribution curves for each series of gold and silver complexes with thiocyanate. The analysis includes comparisons between the thiocyanate systems and the analogous cyanide systems, pointing out analogies and differences between the leaching of gold and silver with thiocyanate and with cyanide. The possibility of using soluble oxidizing agents such as ferric ions, hydrogen peroxide and Caro's acid is evaluated. The thermodynamic data used in the calculations and the chemical reactions represented in the Pourbaix diagrams are all reported in three Appendices. The overall results indicate the thermodynamic conditions for gold and silver leaching by thiocyanate.

Jan 1, 1989

By J. D. Budai, D. H. Lowndes, D. P. Norton, D. K. Christen, B. C. Chakoumakos, J. R. Thompson, B. C. Sales

"Artificially-layered structures, consisting of (Sr,Ba,Ca)CuO2 layers in the tetragonal, ""infinite layer"" crystal structure, have been grown by pulsed-laser deposition. Superlattice chemical modulation is observed for structures with SrCuO2 and (Sr,Ca)CuO2 layers as thin as a single unit cell (~3.4 Å). In addition, novel thin film superconductors were formed by using the constraint of epitaxy to stabilize SrCuO2/BaCuO2 superlattices in the infinite layer structure. Using this approach, two new structural families, Ba2Srn-1CUn+l O2n+2+ d) and Ba4Srn-1CUn+3O2n+6+ d, have been synthesized which superconduct at temperatures as high as 70 K. These results represent not only the synthesis of new structural families of superconductors, but also demonstrate that pulsed-laser deposition and epitaxial stabilization can be effectively used to engineer artificially-layered thin-film materials.Advances in the understanding of epitaxial thin-film growth of the cuprates have heightened interest in creating artificially layered superconductors.(1-3) The layered structure of the copper oxide superconductors opens the possibility of forming novel materials by carefully controlling the epitaxial growth of sub-units of the crystal structures. Thin-film growth methods offer unique opportunities for the atomic engineering of new high-temperature superconducting (HTSc) materials through the ability to form artificially layered crystal structures.(4,S) Moreover, the surfaces of single-crystal substrates provide an ""atomic template"" that can be used to stabilize epitaxial films in metastable crystal structures.An important development in forming new HTSc compounds by artificially-layered epitaxy has been the epitaxial growth of (Sr,Ca)CuO2 films in the so-called infinite layer structure.(6-17) This material, which can be considered the parent compound of all of the copper oxide superconductors, has a relatively simple, layered structure consisting of CUO2 planes separated by planes of alkaline earth elements.(18) Bulk synthesis of (Sr,Ca)CuO2 with the tetragonal, infinite layer structure generally requires the use of high pressure and high temperature bulk processing techniques.(19-24) However, recent experiments show that this metastable compound can be epitaxially stabilized at less than atmospheric pressure, resulting in the growth of tetragonal (Sr,Ca)CuO2 single crystal thin films of the infinite layer defect perovskite structure by pulsed-laser deposition (PLD) over a wide range of growth conditions.(6-17)"

Jan 1, 1994

By N. Kanari

One of the criteria to define the market value of chromite concentrate is its chromium to iron ratio. Changing this ratio for a definite chromite mineral is impossible by physical processing. This study investigated the possibility of increasing this ratio through the carbochlorination and the oxychlorination of chromite concentrates. Experiments are carried out up to 1000 °C. The characteristics of samples and reaction products are determined by SEM, XRD and chemical analysis. The carbochlorination of a chromite concentrate at about 600 °C leads to the . selective partial elimination of iron allowing a higher Cr/Fe ratio of the treated concentrate. Selective extraction of iron could also be achieved at about 950 °C by oxychlorination. In this case, a part of chromium contained in the concentrate is recovered as chromium oxychloride. The obtained residue had high content of Cr, Mg and A1 oxides. Such material has probably better chemical and thermal properties that may. be useful for foundary and refractory applications. Two flow-sheets for the beneficiation of the chromite concentrates using carho- and oxychlorination are suggested.

Jan 1, 1997

By N. Tsuchida

Sumitomo Metal Mining Co. Ltd. (SMMC) is currently developing the flowsheet to treat stockpiled limonite, a type of laterite ore, at Rio Tuba on southern Palawan Island, Philippines. The new plant will be commissioned at the end of 2004. Rio Tuba Nickel Mining Corporation (RTNMC) has been mining saprolite since 1977, and the limonite ore located above the saprolite ore body has been stockpiled separately according to nickel and magnesium content. Ore from these stockpiles will be blended and used for the operation. The annual production of nickel will be 10,000 metric tons for the next twenty years. The proposed process consists of ore preparation, high pressure acid leach (HPAL), counter- current decantation wash, impurity removal and sulfide precipitation. Precipitated mixed sulfide will be processed to electrolytic nickel by the Matte Chlorine Leach Electrowinning (MCLE) process at Niihama, Japan. SMMC has established new technologies during the process development, such as zinc removal and sulfide precipitation. Applying this technology, preferential removal of zinc can be achieved by hydrogen sulfide gas with negligible loss of nickel. Precipitation of nickel by hydrogen sulfide gas is carried out at low temperature. Slow kinetics is selected for control of the particle size of the precipitated mixed sulfide. Keywords: HPAL, Zinc Removal, MS Production

Jan 1, 2004

By D. M. Hausen

Applications of process mineralogy to the exploitation of molybdenum ores begins with early exploration and continues through the evaluation of mineralized prospects, to amenability testwork and pilot plant studies, to the development of a mineable orebody and to the development of a viable process for recovery. After plant construction, a broad range of products from a wide selection of sampling locations, i.e. grinding circuit, flotation cells, smelters and roasting kilns. etc., are evaluated analytically and microscopically, followed by periodic troubleshooting of problem points. The various crystalline phases of molybdenum that occur naturally and throughout various hydrometallurgical and pyrometal1urgica1 processes are identified and characterized by a variety of instrumental methods, including XRD-XRF, optical and electron microscopy, infrared spectrographic and differential thermal analysis.

Jan 1, 1989