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By Alex I. Kociubczyk, Wilky Desrosin, Lucía Mabel Boycho, Alicia E. Ares, Carlos E. Schvezov

In the present research, commercially pure Sn and Zn, and Sn-Zn alloys (Sn-1wt.%Zn, Sn- 2wt.%Zn, Sn-4wt.%Zn, Sn-8wt.%Zn and Sn-8.9wt.%Zn, weight percent) were obtained by a horizontal directional solidification process with two opposite senses and heat extraction. The solidification process was realized using a horizontal furnace with two heat extraction systems at both ends. The temperature was measured using eight K-type thermocouples and an electronic recorder of temperature data. The resulting structures were analyzed using optical microscopy. From the solidification process the thermal and metallographic parameters were determined in all samples. The presence of defects in the solidified pieces was observed. Internal defects pretended to be dependent not only on the composition of the alloys under consideration but also on the size of the structures formed, also, on the velocities and accelerations of interphases, and on the variation of thermal gradients. A model of the phenomenon from the first principles is presented.

Jan 1, 2015

By Sheng-li Wu, Guo-liang Zhang, Bo Su

The mineralogical characteristics of iron ores can influence their high temperature sintering performance. In this study, eight iron ore samples from Brazil, Australia, and South Africa were characterized by their chemical composition, mineral types, particle morphology, and gangue dispersity. Meanwhile the influence rules between the mineralogical characteristics and the high temperature characteristics were evaluated and analyzed. The results showed that the effect of SiO2 on assimilation characteristic of iron ores was relatively complex, Al2O3 and LOI of iron ores had negative correlation with assimilation temperature of iron ores, the dense slab-flaky mineral granule restrained to the assimilation characteristics of iron ores; liquid phase of iron ores with high SiO2 content and low Al2O3 content had high fluidity, and the higher dispersity of gangue minerals in iron ores was good to the fluidity of liquid phase.

Jan 1, 2015

At its Copper Cliff Smelter, Inco Limited processes a bulk copper-nickel concentrate in two Inco oxygen flash furnaces, The furnace matte is converted to low iron matte for further processing, and the molten converter slag is recycled to the flash furnaces. The flash furnace slag is discarded. Natural gas or coke supplies a minor proportion of the process heat requirements, thus limiting the flash furnace matte grade to the target 45% CuNiCo. Coke addition to the furnace offers a potential means of establishing a reducing barrier on the surface of the molten bath. Such a practice would be conducive to producing sulfur deficient (partially metallized) matte. At the same iron content, the iron activity of sulfur deficient matte is higher than that of regular matte. A supernatant coke barrier could, therefore, be expected to lead to higher nickel and cobalt recoveries, reduction or even elimination of magnetite furnace bottom build-up and increased sulfur elimination as S02 in the flash furnace. Preliminary experiments were conducted in a miniplant flash furnace to investigate the effect on process metallurgy of the suggested modified scheme. This paper presents the experimental results and discusses key aspects of the possible operation of the Inco flash furnace with a coke barrier separating the freeboard from the molten bath.

Jan 1, 2003

By S. P. Marsh, M. E. Glicksman

"The effect of capillarity-driven diffusion on the recalescence of mushy zones is studied in pure materials. The solid-liquid mixture is formed by rapid partial solidification of an initially undercooled melt, and the ratio of the two phases is subsequently maintained constant by an externally imposed adiabatic constraint. A novel technique has been developed that permits tracking of the kinetics of the diffusion-controlled evolution process in situ using precision temperature measurements averaged on a length scale larger than that of the microstructure.The mean ""temperature of a mushy zone is slightly below the bulk equilibrium melting point, and is related to a characteristic length scale of the microstructure through an appropriate statistical average of the GibbsThomson equation. Theoretical considerations indicate that the diffusion controlled recalescence will progress as t- l / 3, where t is time. This behavior is experimentally verified for both succinonitrile (SCN) and ethylene carbonate (ETC), which have markedly different morphologies. The kinetic rate constant is observed to increase monotonically with increasing volume fraction of solid in the two-phase mixtures, although a firm theoretical foundation for this result has not been developed.INTRODUCTIONA dispersed multiphase system seeking equilibrium will generally contain variations in the local .free energy density. These density variations arise from such factors as variations in the bulk free energies of the phases and the distribution of interfacial energies. In this study, we examine the kinetics of diffusion-controlled recalescence in 1 solid-liquid mixture of a pure substance at its melting point. This type of two-phase system is particularly convenient to analyze because of the well-characterized physical properties of pure phases (crystals and their melts) and their interfacial energies, and the absence of any solutal effects."

Jan 1, 1986

By David T. Hobbs

Large quantities of highly alkaline, radioactive, liquid wastes are stored in underground tanks throughout the Department of Energy complex. These wastes will be pretreated to separate radionuclides and the remaining decontaminated liquid wastes incorporated into solid waste forms for permanent disposal. Significant savings in disposal costs could result by recovering .the sodium as sodium hydroxide for reuse or disposal as nonradioactive waste. Recent testing demonstrated an electrochemical separation process for the recovery of sodium hydroxide from alkaline waste solutions; The separation process uses ion-selective membranes to separate sodium from the bulk of the waste constituents under an applied electrical field. The sodium is recovered as a 10-15 wt % solution of sodium hydroxide. Results of bench-sc3Ie and pilot-scale tests with simulated and radioactive waste solutions are presented.

Jan 1, 1999

By Ray D. Peterson

The hydrothermal enrichment of chalcopyrite by CuSO, occurs in the absence of oxidizing or reducing reagants. Kinetics of the enrichment process were determined under autoclave conditions in the temperature range of 398°K (125°C) to 473°K (200°C). Covellite (CuS) formed first, followed by digenite (Cu,,,S), with rejection of iron to the solution. The kinetics have been explained by a model which includes diffusion during the first stage formation of covellite followed by surface reaction rate control when digenite be. The effects of particle size, temperature, pH, and cupric and ferrous ion concentrations on the leaching kinetics were examined. Additions of ferrous ion to solution markedly increased the rate of reaction.

Jan 1, 1994

By Ryosuke O. Suzuki

A new cell concept for calciothermic reduction is proposed in which the titanium dioxide instead of TiCl4 is used as the raw material for reduction, Metallic calcium is needed as the reductant of a thermochemicaily stable oxide, such as TiO2. CaCl2, is selected as the solvent of Ca and simultaneously as the solvent of CaO. The reduction system consists of a single cell where both the reduction reaction and the electrolytic reaction for recovery of reducing agent coexist in the same molten CaCl2 bath. A few mol%Ca dissolves in the melt and gives the media a strong reducing power. Sufficiently deoxidized metallic titanium deposits and forms a slightly sintered granular sponge. Both mechanisms of the halide flux deoxidation and the electrochemical deoxidation work efficiently for these fine precipitates, The reducing agent is in situ recovered by electrolysis of CaO because the molten CaCl2 he a relatively large solubility for CaO Some cell designs and modifications are proposed for industrial applications.

Jan 1, 2003

By Yuhsuke Mizukami

Crude high Cr containing steel such as tool steel, heat-resistant steel or stainless steel is produced by dissolution of high carbon ferro-chromium into molten crude steel. In the refining process, decarburization is performed at the first stage, and deoxidation is followed in the next stage. Therefore, the equilibrium relation between dissolved Cr and 0 in molten Fe-Cr alloy after decarburization is very important when yield of deoxidizer is considered for the ovemll control and optimization of the process. It is well known that the yield of deoxidizer does strongly depend on the kinds of refractories of furnace in the secondary refining process. In the present work, the equilibrium relation between dissolved Cr and O in molten Fe-Cr alloy has been measured in a Cr2O3, MgO or Al2O3 crucible at steelmaking temperature. O contents at given Fe-Cr components have been lower in order of Cr2O3, Al2O3 and MgO crucible. The present results have been discussed based on the activities of the constituents in pure solid Cr2O3, and FeO-Cr2O3, MgO Cr2O3 and (AI,Cr)2O3 solid solutions.

Jan 1, 2003

By I. A. Ibrahim, A. K. Ismail, A. A. I. Afifi

"Synthetic rutile for paints industry is conventionally produced by a combined smelting and leaching process. Smelting process is an energy intensive step and represents economic burden in view of the increasing energy costs. Egyptian ilmenite ore containing 40% TiO2 and 38% total Fe was thus directly leached with sulphuric acid to produce eventually synthetic rutile. The process-involves digestion of the ore with sulphuric acid whereby both TiO2 and Fe are dissolved. The solution was then treated with iron powder to convert Fe3+ to Fe2+ to avoid co-precipitation of iron during the hydrolysis step. After solid/liquid separation and clarification, Fe was crystallized as ferrous sulphate hydrate by chilling. The titanium pregnant liquor was concentrated by evaporation and then hydrolyzed to precipitate hydrated titanium dioxide which was then calcined to produce synthetic rutile containing 98.6 TiO2 and 0.58% Fe2O 3. The optimum conditions of all the processing stages were determined.IntroductionSynthetic rutile for paints, welding rods and other industries could be produced from ilmenite ore by sulfuric acid leaching process. This process is a batch process and nearly 80% of all TiO2 produced in the world is made by this process [1]. Figure l shows simple block flowsheet of the process. The process involves the following stages.Digestion: In this stage, ilmenite ore is treated with concentrated sulfuric acid where both iron and titanium are converted to their respective sulfates according to the following equations:"

Jan 1, 2000

By Yun Li

An innovative lead recycling process from scrap lead-acid battery paste is presented. The novelty in the process is avoiding SO2 generation and emission by using reductive sulfur-fixing technique. Iron-bearing secondary wastes produced from metallurgical industry were utilized as sulfur-fixing agent to capture sulfur in the form of FeS (s) instead of generation of SO2 (g). Na2CO3 molten salt was added to the smelting system to speed the reactions and improve valuable metals’ recovery and sulfur-fixation efficiency. Furthermore, this process can simultaneously co-treat various lead and iron-bearing wastes. At the same time, some precious metals, such as Au and Ag, contained in iron-bearing wastes can be recovered. The feasibility and reliability of this process was investigated thermodynamically and experimentally with the help of HSC 9.0 database and XRD and SEM-EDS analysis. A possible reaction mechanism and path in PbSO4–Fe2O3–Na2CO3–C smelting system was also clarified.

By Akira Yazawa

To realize highly efficient process in extractive metallurgy, continuous operation nearly in equilibrium is preferable, but most metallurgical processes consist of plural steps with different chemical potentials. Traditional two-step process of sintering followed by reduction is continuous in each step, but is heterogeneous reaction system far from equilibrium, and the chemical potentials are varied considerably along the distance the charge travels in a reactor. This route will become old-fasioned in next century due to the various inherent problems caused especially by sintering process. To establish reasonable new smelting processes, the important tasks of the metallurgists are how to introduce feed and reacting gas in the reactor, and also how to overcome the difference in chemical potential in the reactor system. Based on the ways to solve theses tasks, recent proposals of new smelting process for copper and lead are classified and discussed with the help of sulfur-oxygen potential diagram. On such potential diagram, each equilibrium step in continuous smelting is expressed at a fixed point, and two reactors with different chemical potentials must be connected by continuous molten flow through launder or partition wall. In the latter case, the reactor is apparently single, but some technical problems must be overcome. While, in a batch smelting like converter, potential variation is successively realized along a path on chemical potential diagram with the time elapsed. To establish immediate equilibrium, continuous steady flow of reactants into well mixed reactor is indispensable. In modern smelting process, the ore is mostly supplied in the form of powder which have huge surface area and fluid character, and consequently injection process must be very attractive. Several examples are discussed for both of copper and lead smelting, and promising future technologies are suggested.

Jan 1, 1988

By Lenny Winkel

With the aim to develop a solar-driven process for the extraction of copper from sulfide concentrates research on the decomposition of copper sulfides under inert atmospheres has been initiated. Thermogravimetric measurements on chalcocite,(Cu2S) revealed that copper is formed already at 1823 K. Chalcopyrite (CuFeS2) also disintegrates at this temperature, although at a lower rate. Copper and iron have been identified in the solid residue. The results confirm the feasibility of copper extraction by direct decomposition of sulfides under atmospheric pressure. The decomposition under inert atmosphere prevents generation of SO2, it also alters the behavior of volatile impurities during decomposition of copper sulfide concentrates. Chemical equilibrium calculations for chalcopyrite contaminated with enargite (Cu3AsS4) have shown that the absence of an oxidic slag allows for a complete evaporation of arsenic and subsequent separation from intermediate sulfides. The need to better assess the potential of direct sulfide decomposition has prompted the development of an experimental setup for studying the decomposition reactions. The experiment has been devised such that data on the decomposition kinetics and on impurity removal can be obtained at temperatures up to 2500 K.

Jan 1, 2003

By Christina V. White

An experimental study was undertaken to investigate the feasibility of utilizing vapor transport for the treatment of heavy metal contaminated smelter soils. The focus of this project was to develop process chemistries that would make incineration a viable process for the treatment these soils. The experimentation concentrated on the elimination of arsenic, cadmium, and lead, and was performed in a laboramry scale rotary kiln setup. Three soil samples from non¬ferrous smelter sites, which contained various concentrations of contaminants, were utilized in the experimentation. Three chemistries were investigated for the volatilization of the heavy metals: Chloridizing volatilization, ferric chloride vapor complex formation, and the use of oxygen potential control. The samples were analyzed for residual heavy metals so that the extractions could be determined. However, the ultimate test was the leachability of the residual arsenic, cadmium, and lead, as determined by the TCLP test. The results firmly establish that incineration is a feasible process for the treatment of metal contaminated soils. It was found that no one process chemistry is suitable for all different soil samples. A two-step process consisting of a reducing step followed by a hydro-chlorination step was required to make Soil Sample-B pass the TCLP tests for all three heavy metals. Soil Sample-A passed the TCLP tests for arsenic, cadmium, and lead using a hydro-chlorination process at a minimum temperature of 700°C. In addition to passing the TCLP mm for Soil Sample-A and Soil Sample-B, 70 to 80 percent removal of the impurities was accomplished. This demonstrates that the leachability of the impurities was decreased primarily due to the removal of a large fraction of the contaminants, Soil Sample-C possessed very high levels of cadmium and lead and only moderate extractions of the impurities were generated from this soil. The arsenic TCLP test was passed at 500'C using a process gas containing ferric chloride and at temperatures of 700°C and above using chlorination of hydro-chlorination.

Jan 1, 1996

By Kazuyoshi Shimakage, Shinji Hirai, Kenji Wada

"An amorphous zirconium oxide coating was prepared by the sol-gel process using zirconium tetra-n-butoxide on the surface of aluminum to improve the corrosion resistance to salt, acid and alkaline attacks. The coating films formed on the smooth aluminum substrates under UV-irradiation indicated an excellent corrosion resistance for salt, acid and alkaline attack tests. For example, the corroded area of coating film in salt attack test for 3600ks in the order of sol-gel coating· film< chromate film <boehmite film, and the sol-gel coating film had the best corrosion resistance. The coating film prepared on the coarse aluminum substrate by a boiling treatment after heat treatment at 573K also had greater corrosion resistance, and a water-avid surface appeared a contact angle of approximately 3°.IntroductionAs given in a previous paper1; a composite film consisting of a porous layer of anodically grown aluminum oxide filled with amorphous zirconium oxide and an amorphous zirconium oxide coating layer deposited thereon via the sol-gel process utilizing the dip-coating technique, was prepared to improve the alkaline corrosion resistance of aluminum. The alkaline corrosion resistance of these composite films was increased in the range of 24 to 50 times those of conventional anodic oxide films anodized in sulfuric acid. As a result, it was proved that heat treatment at 573K after dip-coating was an important process to .remove organic component from gel film and to accelerate the densification of coating layer. Furthermore, the effect of ultraviolet (UV) irradiation at ambient temperature on the densification of coating layer was also examined to lower the heat-treatment temperature2.Then, a sol-gel film prepared by UV irradiation at ambient temperature indicated that alkaline corrosion resistance of aluminum was superior in the range of 2.4 times to 2. 6 times that of the conventional composite film heated at 573K."

Jan 1, 2000

By Eugene Jak

Copper sulphide processing technologies face increasing pressures associated with decreasing concentrate grade leading to increasing thermal inefficiency and lower productivity. Impurity concentrations are on average increasing, creating potential environmental risk and additional treatment costs. In copper flash smelters dust, partially oxidised materials and fume formed from the condensation of volatile impurities, are routinely recycled to the feed. In the converting stage the heat balance is maintained by charging anode reverts and other inert materials. In both cases, the thermal energy available from sulphide oxidation is not fully utilised or optimised. The productivities of both smelter and converter stages can be potentially increased through the addition of a high copper, low iron, low impurity precipitated copper product. Calculations are carried out for fayalite smelter and calcium ferrite converter slags using an optimised FactSage thermodynamic database. The potential for significant increases in smelter and converter productivities using existing technologies are predicted.

By Yuuki Yoshida

Electrolytic manganese dioxide, EMD, is the positive electrode material of primary batteries and the raw material of LMC used as the positive mass of lithium ion batteries and is currently produced by anodic deposition on and harvesting from a titanium anode in acidic manganese sulfate solutions prepared by dissolving high purity of manganese sulfate into sulfuric acid solutions. This paper presents an alternative method of EMD production using a novel anode, Mn2O3 coated titanium, at lower operating temperature than the current process to explore a possibility of manganese recovery from zinc electrowinning solutions. The Mn2O3/ Ti anode prepared by thermal decomposition of a precursor solution containing Mn (II) showed the anodic deposition of MnO2 by constant current electrolysis and the current efficiency was 95% in maximum, while the current efficiency and the crystallographic structure of deposited MnO2 depended on the current density, the electrolysis time, the bath temperature, and the concentration of Mn(II). The deposited MnO2 was successfully harvested from the anode and the recovery rate was 98%.

By Lv Guozhi, Niu Liping, Liu Yan, Zhao Qiuyue, He Jicheng, Zhang Ting’an, Dou Zhihe

"This paper proposed a new method of Mg and Cl2 circulating for titanium sponge production by direct pyrolysis and thermal reduction process. Effects of pyrolysis temperature, pyrolysis time and partial pressure of oxygen on pyrolysis efficiency were researched, and the crystallite structural transformation of MgO productions at different pyrolysis temperature and time were analyzed by XRD. The experimental results indicates that the pyrolysis temperature and time effects the pyrolysis efficiency obviously, and the reasonable pyrolysis conditions by using MgCl2 in molten state are as follows: the pyrolysis temperature is 1100?, pyrolysis time is 60min and the partial pressure of oxygen is 100%, the pyrolysis efficiency get above 95% at this conditions. The dynamic analysis of molten magnesium chloride pyrolysis reaction shows that, as a chemical reaction process control, the response of the apparent activation energy Ea=70.4 kJ/mol.IntroductionTitanium is a young metal, it is applied in industrial until the Second World War. It is 160 years from the discovery of titanium to the industrial production of ductility titanium by magnesium reduction method in the United States in 1948. As a new kind of metal, titanium and titanium material are better than the traditional metal materials in mechanical properties, heat resistance and thermal conductivity. Titanium is a kind of landmark structure and function material, which is called “space metal”, “Marine metal”, “Intelligent metal” [1-3]. Although the study of new methods of titanium melting get more at present, Kroll method and Hunter method are really applied to industrial production methods for titanium smelting, and Hunter method is already discontinued because of costs at present. The core technology in Kroll method of sponge titanium production process can be ome down to two circulation, namely the cycle of magnesium and chlorine in preparation-process of titanium sponge. In the traditional Kroll method, the cycle is realized through magnesium chloride which is produced by the electrolytic magnesium reduction process in hot molten state. But because investment of equipment for electrolysis method is too high, this method has not been used by most titanium sponge production enterprise in China. At present most titanium sponge production enterprise in China produce titanium sponge by the outsourcing of titanium tetrachloride, but the main disadvantage of this method is that the by-product of magnesium chloride is difficult to deal with."

Jan 1, 2012

By James B. Pfeiffer

TETRA Technologies, Inc., has applied its HDS? metals precipitation system to control a mine drainage problem. The effluent from the mine contains primarily zinc, manganese and iron, plus varying small amounts of cadmium, copper and lead. The flow from the mine averages 350 gpm, and varies considerably depending on season and weather conditions. The plant was designed to treat 1000 gpm of the water and generate a dense sludge suitable for recycling. The HDS? system contains a number of reactors, followed by post filtration and meets stringent metals discharge criteria as specified by New Source Performance Standards.

Jan 1, 1994

By Saskia Duyvesteyn

Ion flotation is a technique applicable to the removal of metal ions from dilute solutions, using ionic surfactants.- While there are a number of physical and chemical parameters that influence the ion flotation process, this paper focuses on two of the important chemical ones, namely frother concentration and ionic strength. The effect of several frothers, including ethanol, iso-propanol and MIBC at concentrations ranging from 0% to 0.4%, was studied for the model Cd-dodecylsulfate and Cu-dodecylsulfate systems. The ionic strength, as well as the effect of monovalent and multivalent counter ions, was also studied in the range of 1@3 - 1 M, at constant pH. The results are discussed in terms of applicability to a range of effluents from minerals and materials processing operations.

Jan 1, 1994

By S. P. Mathew

The ISASMELT Lead Process is a continuous two stage process for the production of crude lead from concentrate. It is based on the use of a top entry submerged Sirosmelt lance to produce turbulent baths in which high intensity smelting or reduction reactions can occur. The process involves oxidizing the concentrates in the first stage to produce a high lead slag. This slag is tapped continuously and transferred down a launder to a second furnace where it is reduced with coal. Crude lead and discard slag are tapped continuously from this furnace through a single taphole and separated in a conventional forehearth. Process and engineering design work for a commercial scale Lead ISASKELT plant designed to produce 60000 tpa crude lead has been completed. This plant is planned to be operational in 1991.

Jan 1, 1990