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By Wiraseranee. Chompunoot, Kazuki Morita, Toru H. Okabe

"Aiming at the development of more effective recycling processes, dissolution behavior of rhodium into molten slag was investigated. Using a pure rhodium crucible and Na2O-SiO2 slag system, equilibration experiments were carried out for 18 h at 1423-1623 K under various oxygen partial pressures of 0.005-1 atm with varied slag basicity. Rhodium solubility increased with increasing oxygen potential, slag basicity, and temperature. Rhodium dissolved into slag as rhodate ion ([RhO2]-) by the endothermic reaction: Rh(s) + 3/4O2(g) + 1/2O2-(in slag) = [RhO2]-(in slag). In the dissolution reaction, the “rhodate capacity” of slag is newly-defined. The correlation between rhodate capacity and optical basicity is reported.IntroductionDue to its high chemical resistance and outstanding catalytic properties, rhodium (Rh), one of the platinum group metals (PGMs), is utilized in various applications such as catalysts, molten glass vessels and containers, and electronic devices. Owing to the rarity of Rh resources in nature, recycled Rh from scraps such as spent automobile catalytic converters is currently considered as an important source of Rh supply [1]. According to the recycling practices, Rh is currently mainly recovered from scraps along with other PGMs such as platinum (Pt) and palladium (Pd) by a dry process (e.g., smelting), a wet process (e.g., leaching and subsequent separation of PGMs from aqueous solution), or a combination of both processes [2]-[4]. Among these processes, smelting is commonly applied because PGMs can be effectively separated from a relatively large amount of various impurities coexisting in scraps. In the smelting process, Rh and other PGMs are collected in the collector metal (e.g., iron and copper), and impurities in scraps are removed into slag [4]-[6]. The process may be carried out at a temperature range of 1573-1973 K, in either an oxidizing or reducing atmosphere. Due to the high oxidation resistance at high temperatures, Rh is expected to be collected efficiently in the metal collector rather than being oxidized and forming RhOx in a molten slag. However, Rh loss into slag does occur in this process [7]."

Jan 1, 2011

By Guo Chang Jiang

In order to improve the IIAZ toughness of X-60 pipe steel, the intragranular ferrite plate (IFP) technology was used. The characteristics of IFP is claimed to be much fine ferrite plates appear inside the original austenite grains. By means of suitable Re, Zr, Ti additions in a bath with a higher initial oxygen potential, a good control of the peak temperature and the cooling rate during welding simulation, one can get a %IFP in volume over 50%, and the toughness gets up from 55 J to 160 J. It was found that the inclusions most effective in nucleating IFP are some deformable complex silicates which either entrap Re, Zr, Ti oxides or contain these elements. The greater the number of the evenly distributed and effectively nucleating inclusions, the more the %IFP in volume, and the finer the microstructure of the HAZ, so the better the relevant toughness. Generally, these silicates bahave as fine spheres along a line. The present authors revealed that these fine spheres result from the remelting of the shuttle- like silicates due to heating in the process of welding simulation. These silicates used to get a higher sulphur capacity, so MnS deposits might be observed on the periphery of the silicates. IFP was proved to be directly rooted in the [Mn] depleting zone which locates beside MnS deposits.

Jan 1, 1997

By Qian Xu, Guangshi Li, Xionggang Lu, Xingli Zou, Hongwei Cheng, Cong Xu, Changyuan Lu

The roasting of nickel-bearing sulfides is a complex but important process which has not been adequately characterized. Combination of X-ray diffraction and scanning electron microscopy has been proved to be useful for such experiments. The leaching results of nickel, copper, iron and cobalt was analyzed by ICP methods. Process possibility of polymetallic sulfide concentrates through a three-step procedure (oxidation roasting - chlorination - water leaching) was suggested. Ammonium chloride could react with nickel/copper oxides to produce intermediate complexes. At the temperature range of 280~340 oC, these complexes further decomposed to the corresponding simple chlorides. Roasting sulfide concentrate using NH4Cl is effective for complex ores.

Jan 1, 2016

By Katsunori Yamaguchi

Secondary materials, that contain relatively high concentrations of platinum group metals, (PGMs) are treated in copper smelting process. The PGMs lost in the slag is increasing with increasing quantities of scrap treated amount. To determine the portion of the PGMs chemically dissolved and that associated with the mechanically trapped matte in the slag will be a key factor to improve the recovery of those metals. An experimental study was carried out to determine the distribution of palladium between the FeOx–SiO2 slag and the liquid Cu2S–FeS matte at 1573 K and a fixed partial pressure of SO2 of 0.1 atm. It was found that the distribution ratios are around 10−3 for platinum and palladium. The distribution ratios show a tendency to increase when the grade of matte is increased above 60 mass% Cu. In addition, the solubility of platinum in FeOx–SiO2 slag equilibrated with a pure palladium and the Pd-Cu alloy was determined at 1573 K and the range of oxygen partial pressure from 10−9 to 10−7 atm. The solubility of palladium in the slag tends to increase with increasing oxygen partial pressure and activity of CuO0.5 in the slag.

By A. V. Tarasov, A. D. Besser

A processing flowsheet has been developed for treating substandard lead-containing polymetallic bulk concentrates and intermediate flotation products containing precious metals, which comprises oxidizing roasting in a calcination kiln and electrothermic smelting generating low volumes of off-gas. The proposed flowsheet also incorporates a dust collection system and sulfur dioxide recovery from off-gas. It is proposed to implement this process by using a reaction smelting technique. For this purpose, the charge to be fed to the smelting furnace after its calcination in a drum-type rotary kiln must have a ratio of sulfide sulfur to sulfate sulfur of at least 1 :2. Electric smelting makes it possible to produce lead bullion that also collects the precious metals contained in the feed, as well as copper-lead matte and slag containing zinc. The recovery of lead into lead bullion and into matte is approximately 83% and 14%, respectively (thus the overall recovery is 97%); the total recovery of gold and silver into lead bullion and matte is 98%; th\lt of copper into matte is 89%; the recovery of zinc into slag is 96%; and that of sulfur into sulfuric acid or gypsum is 90%. After the recovery of zinc from slag, the latter can be utilized in the construction industry.

Jan 1, 2000

By David R. Sadedin

The highly negative Gibbs free energies of hydrogen atom reactions suggest that refractory oxides such as titanium dioxide should be easily reduced by hydrogen atoms. These reactions appear to be most favourable at low temperatures; oxides should be reducible even at room temperature. Since hydrogen atoms are produced in plasmas containing hydrogen a number of investigators have used hydrogen plasmas of various sorts to test these possibilities for reducing refractory oxides, in particular TiO2. None of these attempts has succeeded, a small degree of reduction being achieved in only a thin layer near the surface. A deeper consideration shows that several factors complicate the reactions expected on the basis of the negative Gibbs free energy. One factor is that the back reaction by water molecules produces molecular hydrogen, not hydrogen atoms, and the metal atoms that have been reduced may be immediately re-oxidised. In plasmas there are complications due to diffusion, thermal and charge boundary layers and charged particle reactions. Interpreting the results of hydrogen atom reactions is difficult. Hydrogen is not detectable by electron dispersive spectroscopy and amorphous products are not determinable by x-ray diffraction. Another consideration is economics. The cost of producing hydrogen atoms has a large bearing on the metals for which hydrogen atom reduction may be competitive. In this paper these factors are discussed, some necessary basic studies are highlighted and the general principles of a laboratory reactor are given, together with the results of tests using ZnFe2O4, ZnO and TiO2 as test oxides.

Jan 1, 2006

By V. I. Lakshmanan

"Historically flowsheets are developed for efficient separation of metals for economic recovery. With increasing emphasis on reduction, reuse and recycle (3Rs) efficient methods are sought to recover values from a variety of feeds where cost of collection, transportation, local consumer behaviour and regulatory guidelines dictate the development of economically viable flowsheets. Innovative understanding of potential market applications can provide means to develop value added end products. The paper with examples will discuss the use of innovative-separation technologies to obtain value added end use materials from secondary sources.IntroductionFlowsheets are developed for the efficient separation of materials of value for economic recovery. However with increasing societal pressures and regulatory initiatives for stricter environmental guidelines, there is strong need to provide focus to recover materials efficiently and economically in an environmentally accepted manner. North American industries are increasingly caught between demands for high technology value added products and responsibility for environment. An aspect that is receiving increasing attention is Design for Environment'. This incorporates a system wide approach for product design and incorporates environmentally preferable features such as recyclability, disassembly, maintainability, reusability and use of safe materials as part of a product's design objectives.The present paper with case histories will address innovative flowsheet development to convert wastes into recyclables value added products or for minimising generation of waste materials. Case HistoriesProcess for Separating Fibres from Composite Materials 1In the automotive industry, sheet molded compound (SMC) is used to produce panels, bumpers and the like. During the manufacture and at the end of life, considerable waste materials are generated which are potentially recyclable. Fibre reinforced plastics where fibre substrate impregnated with thermosetting resin, find applications in several manufacturing processes and are potentially recyclable at the end of life."

Jan 1, 1996

By Gopalakrishna B. Prabhu, David L. Bourell

"Three mol% Yttria-Stabilized Tetragonal Zirconia (YSTZ) was prepared by a sol-gel synthesis technique using zirconium tetrachloride and hydrated yttrium chloride precursors. After drying and annealing at 823K, the particle size was in the range 10 to 20 nm. The zirconia powder was sintered using a uniaxial hot press at an applied stress of 20 to 40 MPa. One hour, isothermal sintering was performed in air after initial heating at 50K/min. Theoretical density was obtained at densification temperatures above 1498K. After sintering, grain coarsening characteristics were studied using constant heating rate anneals followed by quenching, based on a model for grain coarsening in a linear heating rate cycle. The microstructural change was studied using SEM and TEM and the phases were determined using x-ray diffraction.IntroductionThe ability to sinter nanocrystalline materials to full density several hundred degrees below the normal sintering temperatures is one reason for their current interest. [1-5] Yttria Stabilized Tetragonal Zirconia (YSTZ) of grain size of about 300 nm has exhibited superplasticity, with elongations as large as 800%.[6-7] Fine grain size is critical for superplasticity. Retention of the fine grain size during sintering of nanocrystalline powder is important if a material is to exhibit superplasticity or to exhibit physical or mechanical properties associated with the ultra fine structure. This paper investigates the sintering behavior and the grain coarsening characteristics ofnanocrystalline YSTZ.Techniques for synthesizing nanocrystalline materials have been studied in great detail earlier. [8-12] The techniques used to synthesize nanocrystalline zirconia include alkoxide synthesis [9], the chloride method [11], the peroxide method [13] and the acetone-toluene method. [13] In this paper the method used in the synthesis of zirconia is the chloride technique. With this precipitation technique, either zirconium chloride or oxychloride and a corresponding yttrium salt or even pure yttria are used."

Jan 1, 1994

By Samantha Moodley, Rauf Hurman Eric, Cevat Kucukkaragoz, Aditya Kale

"Two titania slags, rutile and synthetic rutile were chlorinated with petroleum coke and CO in a small bubbling fluidized bed reactor. The study aims to identify differences in chlorination mechanism, compare conversion rates, blowover and the chlorination of impurities for the various titania feedstocks at different temperatures.Chlorination rates were highest at 1000ºC; rutile chlorination significantly increases as temperature increases from 800ºC to 1000ºC. At 1000ºC, synthetic rutile had the highest chlorination conversion rate; this was followed by Slag B which in turn was more reactive than Slag A and rutile. The mechanism for slag, synthetic rutile (SR) and rutile chlorination differs. Synthetic rutile feed is porous, providing a larger surface area for the chlorination reaction, hence the highest conversion rates was attained. Titania slag becomes porous with the initial chlorination of FeO and MnO whilst rutile remains solid. As the porosity of slag particles increases so does its tendency to be elutriated. Ti2O3 is oxidized within the early stages of chlorination during the chlorination of FeO and MnO. Ti2O3 not oxidized is then rapidly chlorinated.IntroductionTitanium dioxide (TiO2) is the most common compound of titanium, about 95 - 98% of extracted titanium minerals is processed into TiO2 white pigment [1]. Two processing routes exist for the production of TiO2 pigments, i.e., sulphate and chloride based processes. In the chloride process, titania feedstock is fed to a fluidized bed reactor together with reductant and chlorine gas. A temperature of 1000 - 1300ºC is maintained in the reaction zone and apart from silica, zirconia, uranium and thorium, virtually all the metal oxides in the feed are converted to their respective chlorides [2]. Chlorine is recovered and recycled back to the reactor."

Jan 1, 2012

By Qian Xu, Xionggang Lu, Xingli Zou, Zhongfu Zhou, Shuhua Geng, Hongwei Cheng

Herein we report an electrochemical route from oxides (SiO2, TiO2)/sulfide (MoS2)/carbon mixture precursors to Mo-Si-Ti-C composites in molten salt. The electrochemical process was carried out in molten CaCl2 at 800 °C with a potential of 3.1 V, and a graphite-based anode was used in the electroreduction process. The reaction mechanism and the influences of the stoichiometry of the initial mixture precursor on the morphology and phase composition of the final products were investigated. It has been found that Mo5Si3/MoSi2/Mo3Si/Mo, Mo5Si3/MoSi2/Mo2C/SiC, and Mo5Si3/Mo2C/Ti3SiC2/TiC/Mo composites can be electrosynthesized directly from their oxides/sulfide/carbon mixture. The preliminary experimental results suggest that the electroreduction process can be used for the controllable electrolytic production of alloys/carbide-containing composites from oxides/sulfides/carbon precursors.

Jan 1, 2016

By Roger W. Lee

The commissioning of the prototype Imperial Smelting Furnace (ISF) in 1950 was a technological breakthrough in the pyrometallurgical smelting of zinc and provided significant advantages over the existing retort processes. However, for most zinc concentrates the electrolytic zinc process continued to be more economic. Therefore, the Imperial Smelting Process (ISP) specialised in smelting zinc and lead concentrates that were less amenable for treatment by either the electrolytic zinc process or the lead blast furnace. Subsequently, improved mineral processing techniques led to a decrease in the availability of these concentrates so the treatment of secondary materials in the ISP assumed greater importance. This was facilitated by the development of techniques such as hot briquetting and tuyere injection. In 2002 over 1 million tonnes of zinc and 400,000 tonnes of lead were produced by the ISP. However, in the 2002-3 the economics of the Process became extremely difficult because of low metal prices and increased operating costs. This resulted in the closure of four ISP smelters in 2003 and two in 2005. Nevertheless, two new ISP smelters are scheduled for commissioning in China in 2006 where local economic conditions continue to favour the process. The economics of the process are examined particularly in respect of smelter margin and operating costs. The need to increase the smelter margin means that the future of the process will be closely linked to its ability to consume secondary materials and an examination will be made of its potential for conversion to 100% secondary operation. Apart from a reduction in raw materials costs, a substantial reduction in operating costs would ensue from not operating sinter and sulphuric acid plants.

Jan 1, 2006

By Dae Jin Ha

Sticking phenomenon occurring during hot rolling of two STS 430JlL ferritic stainless steels was analyzed by hot-rolling simulation tests. The sticking started from the initial nucleation stage in which the rolled materials were stuck onto the roll specimen surface, proceeded to the growth stage in which stuck fragments grew further, and reached the saturation stage. The modified 430JlL steel had a smaller number of sticking nucleation sites and slower growth rate than the conventional 430JlL steel because of higher high temperature hardness, thereby leading to less serious sticking. When the simulation test was conducted at 1070 °c, Cr oxides were formed on the surface of the rolled materials, and thus the sticking was drastically reduced because of the increased surface hardness of the rolled materials. In order to prevent the sticking, high-temperature properties of the rolled materials should be enhanced when rolled at 900°C or 1000 °C, and rolling conditions and alloying compositions, under which the oxide formation was promoted, were more important than high-temperature properties when rolled at higher temperatures than 1000 oC.

Jan 1, 2008

By Susanne Pignolet-Brandom

QEM*SEM is an automated scanning electron microscope/computer system that characterizes samples with regard to mineral modal abundances, mineral grain and particle sizes, mineral associations, and particle surface areas. Additional information, based on the classification of particles according to the area percentage of a mineral of interest, can be obtained for samples of particulates. QEM*SEM is capable of analyzing a wide variety of materials although it was originally developed for applications to the minerals industry.

Jan 1, 1988

By Omid Marzoughi

In this research, both the kinetics and the mechanisms of the roasting of a sphalerite concentrate from the Bafgh mining complex in Iran were investigated. The oxidation process was performed in a muffle furnace in air and the effects of time and temperature on the degree of oxidation of the zinc sulfide sample were quantitatively studied. The experimental data were fitted to the shrinking core model. In the temperature range of 650–800 °C, the rate-controlling step was the chemical reaction between the zinc sulfide and oxygen with an activation energy of 103 kJ mol−1. On the other hand, in the temperature range of 850–950 °C, the rate-controlling step was oxygen diffusion with an activation energy of 50 kJ mol−1. Also, the roasting process was studied using thermogravimetric (TGA) and derivative thermogravimetric (DTGA) techniques.

By Liu Chunpeng

Under an inert atmosphere, the temperature enhancement of nickel bearing pyrrhotite irradiated by microwave was measured with a special metal-sheathed thermocouple and the non-isothermal rate equations were obtained. Under the controlled oxygen potential of the reacting gas in the microwave field, over 90% sulfur contained in the pyrrhotite is converted into elemental sulfur directly, the iron and the nickel are transformed into FeO,, NiO, NiFe,O, and FeSiO,. According to the experimental data the rate of the elemental sulfur produced is in diffusional control and the non-isothermal equation derived is

Jan 1, 1993

By Du Sichen, S. Seetharaman, J. A. Bustnes

"The present study deals with the kinetic studies of reduction of some selected transition metal tungstates with hydrogen. The measurements were carried out by the isothermal thermogravimetric method. Shallow powder beds were employed in order to avoid the effects due to transport phenomena affecting the reaction rate. In this way, the chemical reaction rates could be selectively studied. The experiments were carried out in the temperature range 873 - 1173 K. From the experimental data, the activation energies were evaluated and were found to be around 88 kJ / mol in the case of both iron as well as cobalt tungstates indicating the similarities in W-O bonds in both cases. The activation energies obtained are discussed in the light of the position of the transition metal in the periodic table as well as the thermodynamic stabilities of the various tungstates.IntroductionThe tungsten containing hard metals, characterized by high density, belong to a class of two-phase metal matrix composites. While these types of materials have traditionally found their applications within the defence industry as armour-piercing projectiles, counterbalance in helicopters and military aircrafts, outer casings of hand-grenades, etc., commercial applications for this class of alloys also exist, including radiation shields, penetrators for the oil industry, turbines for turbo-jet engines and a wide range of sports related parts. A possible route to the production of these alloys is to reduce the tungstates such as FeW04, Co W04 and NiW04 using a reductant like hydrogen or carbon monoxide. In order to have a better understanding of the processes involved in the production, it is important to have a knowledge of the reduction kinetics for these tungstates. According to the knowledge of the present authors, while the reduction ofNiW04 by hydrogen gas has been investigated earlier in the present laboratorypl no systematic reduction study has been carried out previously for the tungstates of iron, cobalt."

Jan 1, 1996

By H. Saint-Raymond, F. Gruy, P. Gardin, M. Cournil

"The control of inclusion elimination is getting more and more important to obtain clean steel. This paper presents a methodology under development for predicting cluster growth and elimination in ladle - RH system. The first key point is to express the collision efficiency, which is very specific for alumina cluster due to the non-wetting fluid. Second, a description of the two-phase flow in the system is necessary. In our calculations with Fluent CFD package and Lagrangian approach for bubbles, bubble growth is implemented, which improves the predictions. Using global reactor decomposition makes possible the prediction of the time evolution of cluster distribution. Important effect of fractal dimension is demonstrated.IntroductionElaboration of new steel grades requires not only to have a high purity in terms of C, O and N content but also to eliminate particles such as alumina or slag droplets. Flow optimisation making easier inclusion elimination is then a key figure to satisfy cleanliness requirements. Mathematical models of flow and inclusion behaviour are widely used for this purpose (1, 2). But having a predictive tool is still a challenge, because the number of phases is important in steelmaking industry: liquid steel, slag layer, bubbles and inclusions (with a large range of composition and rheology). The paper presents the methodology which is developed at IRSID to predict oxygen content evolution during RH degassing.The main mechanisms which have to be considered are :-inclusion growth by turbulent aggregation of elementary inclusions (keeping in mind that liquid steel is a non-wetting medium for inclusions); the difficulty is to express collision efficiency for alumina particles,-inclusion removal by flotation; the difficulty for alumina clusters stems from the complex morphology of particle; fortunately, the use of fractal concept makes it possible to cope with this problem.The paper describes the general modelling of inclusion removal taking into account the previous mechanisms. Hydrodynamic parameters are obtained by means of Fluent CFD package and a specific coding is developed for cluster growth."

Jan 1, 2001

By R. V. Kumar

"The use of sensors to monitor gaseous species in industrial processes is discussed. All of the existing systems have disadvantages. Sensors, based upon solid electrolytes, which can be placed directly into the gas stream are attractive but many also respond to oxygen, need to be sealed at high temperatures and require a separate reference. This paper describes sensors, usually based upon two electrolytes, which do not respond to oxygen and do not require high temperature gas seals or separate references. The application of these sensors to the measurement of carbon dioxide, sulphur dioxide and trioxide and hydrogen chloride is described. These sensors can be placed directly into the gas stream at elevated temperatures.IntroductionOn-line gas sensing is becoming more important as concerns regarding the environment mount. There are many established techniques for monitoring gases in industrial processes, with applications in safety monitoring, chemical analysis or process and emission control. Flue gas analysis involves the greatest technical complexity, requiring several sophisticated capital-intensive spectroscopic instruments for different species as well as needing highly skilled operators. There are also several instruments, based upon aqueous electrochemistry, which are available for the analysis of the gases S03, S02, N02 but these require that the gases are sampled at high temperature and cooled, prior to analysis. These instruments cannot be considered as giving on-line measurements of the gas composition. Furthermore, the power requirement of these instruments frequently precludes battery operation for field and domestic use."

Jan 1, 1997

By L. A. Bertram, F. J. Zanner

"The goal of this paper is to present a tool to simulate transient melting of the electrode tip. This capability is needed to develop and test furnace control algorithms since experimental determination is difficult and expensive. Simulation incorporates parameters (including arc voltage, arc current, electrode gap and furnace pressure) from previous quasi steady experiments with 460 mm diameter Inconel 718 electrodes.Cathode heating rates (determined by classical as well as experimental arc models) are linked to these independent variables. After radiative loss adjustments to the heating, transient one dimensional melting is computed. IntroductionThe vacuum arc remelting (VAR) process attempts to improve the physical and chemical homogeneity of a static-cast electrode by remelting and solidification in a quasisteady manner. To achieve steadiness of furnace operation requires automatic controls based on inputs measuring physically relevant state variables of the process. Previous industrial scale VAR studies (1,2,3) involving stainless steels, superalloys, and other alloys have provided a basis on which control strategies of some generality can be proposed (4). Of these measurements, the data for Inconel 718 is the most complete, so discussion in this paper is restricted to this alloy.Studies of the In 718 alloy subjected to the VAR process have established that melt rate M (kg/hr) depends not only on the melt current 1m (kA) supplied to the furnace, but also on ambient gas pressure of CO, PCO (micron), and electrode gap ge (mm) as well (1):"

Jan 1, 1986

By Ross R. Bhappu

A theoretical and experimental investigation into pyrometallurgical refining of chloride leach/electrowin copper is described. The two techniques investigated were (i) vaporization and (ii) gaseous halogenation. Experiments were carried out with a packed bed of electrowon copper crystals and a boat of melted copper crystals. Nitrogen gas and Freon 12/nitrogen mixtures were used as the carrier and reac.tive gases. Vaporization was found to be effective in removing Bi, Pb and S while halogenation was effective. in removing As, Bi, Pb, S and Sb. Silver resisted all attempts at removal. Iron was removed but less effectively than the other impurities.

Jan 1, 1985