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By Gustavo Díaz, Miguel A. García, Carlos Frías

"Under the auspices of the Commission of the European Union, a consortium composed of six European organi~ations has conducted a project to scale up the PLACID electrowinning cell to industrial size within the Placid process development. This paper is concerning the results and achievement of the industrial cell prototype after more than 1,000 hours operating time and about 10,000 Kg electrolytic lead production. In general, results have been very satisfactory, demonstrating the ability ofthe PLACID electrowinning cell to produce top quality electrolytic lead (> 99.99 %) with high current efficiency and low energy consumption.IntroductionThis paper is concerning the development of an industrial size PLACID electrowinning cell within the PLACID process development. This project began on January 1993 and was finished on April 1996.Lead metal production and manufacturing industries produce large amounts of dusts and also lead bearing slags. Spent lead-acid battery recycling also produces lead oxides from the battery pastes rather similar to those mentioned above. Those lead secondary materials are hazardous and difficult to handle by usual procedures.Existing processes to treat-lead oxides may inflict considerable damage on the environment, incur high operating costs and have limitations to produce top quality lead.The main aim of this project has been to develop a novel hydrometallurgical process able to deal with different lead bearing materials, mainly lead oxide secondaries: lead-acid battery pastes, lead fumes, furnace slags, oxide residues, etc., producing ""four nines"" pure lead in an efficient manner with a benign influence on the environment; it is called the PLACID process."

Jan 1, 1997

By Yimin Ruan

"An inverse design method is developed to obtain the optimal cooling conditions for the continuous quenching of precipitation hardenable sheet alloys to achieve the required yield strength. The yield strength of a precipitation hardenable alloy is obtained by allowing solute to enter into solid solution at a proper temperature and rapidly cooling the alloy to retain the solute in the solid solution. An aging process may be needed for the alloy to develop the final mechanical properties.The objective of the design is to optimize the quenching process so that the required yield strength can be achieved. With the inverse design method, the required yield strength is specified and the sheet thermal profile at the exit of the quenching chamber can also be specified. The conjugate gradient method is used to optimize the cooling boundary condition during quenching. The adjoint system is developed to compute the gradient of the objective functional. An aluminum sheet quenching problem is presented to demonstrate feasibility of the inverse design method.IntroductionQuenching is a critical step in metal production to achieve desired material properties, such as yield strength, hardness, etc., for precipitation hardenable alloys. In most cases, rapid quenching from the solution heat treatment temperature is necessary to obtain the required material properties, but rapid quenching may cause other problems such as excessive distortions of the quenched materials.In a solution heat treatment, the alloy is heated to a suitable temperature, held at that temperature to allow the soluble alloying elements to enter into the solid solution, and cooled rapidly (quenching) to retain the alloy elements in the solid solution. An aging process, which controls precipitation of fine particles at room (natural aging) or elevated temperatures (artificial aging), is generally followed after the quenching process to develop the final mechanical properties of the heat treated alloys."

Jan 1, 1998

By H. K. Fouad, L. A. Guirguis

The starting mill strip solution· for this study· is an ammonium uranyl tricarbonate solution of pH 8.2 containing 20g uranium/liter, after a DEPA/TOPO extraction process from sulfuric acid leaching liquor. To the first portion of the concentrated acidified strip solution, hydrofuoric acid is added at 95°C in reduced condition to obtain uranium tetrafluoride. The second portion of the uranyl carbonate strip is subjected to a precipitation step by admixing 0.3 volume of non-solvent precipitating agent such as acetone per volume of uranium. ·Uranium oxide (U30 8) is obtained from this precipitate by calcination for half an hour at 800°C in air. The third portion of the strip solution is neutralized to a pH 6.5 with sulfuric acid to precipitate iron and other contaminants. The solution is further acidified to a pH 1.85 with continuous air bubbling to remove CO2, followed by H2Ch precipitation at pH 3.5 to obtain uranyl peroxide. The latter is reduced by stannous chloride to obtain uranium trioxide dihydrate UO3. 2H20. Identifications, characterization· and purity of these products are carried out by complete chemical analyses, Scanning electron microscope study, tap density determination, X-ray diffraction and infrared spectroscopic investigations. The achieved results agreed well with that of the published data for these nuclear grade purity products.

Jan 1, 2000

Reduction of titania and ilmenite ores by Cf4-H2-Ar gas mixture was investigated in a laboratory fixed bed reactor. Titania was reduced to titanium oxycarbide in the temperature range of 12OO-1500°C. At 1400-15000C, the extent of reduction of titania to titanium oxycarbide achieved more than 85% in 90 min. Optimum conditions for titanium oxycarbide synthesis by reduction of titania include temperature in the range of 1300-1450°C, methane content 8 vol% and hydrogen content above 35 vol%. Ilmenite ore was reduced by Cf4-HrAr gas mixture to metallic iron and titanium oxycarbide. Metallic iron catalyzed methane cracking and solid carbon deposition. Titanium oxycarbide formed at temperatures as low as 950°C. The optimum temperature for reduction of ilmenite is 1200°C and the optimum methane content is 8 vol%. Increase in hydrogen content increased both rate and extent of reduction. With 5 vol% CH4-75 vol% Hr20 vol% Ar gas mixture, the reduction of ilmenite completed in 60 min. Reduction of titanium oxides to oxycarbide with following chlorination may be an efficient alternative technology for processing of titanium minerals.

Jan 1, 2001

By Thierry De Nys

A direct leaching process of sulphidic zinc-based concentrates in aqueous sulphuric acid solutions has been developed by the V.M. R & D Department. By a very accurate control of the oxidation potential of the leach solution, this process enables a separate recovery of the zinc, copper, silver, lead and sulphur of the concentrate and makes it extremely attractive for treating more complex ores. The iron, solubilized during leaching, is eliminated out of the zinc solution by means of the V.M. goethite process. Alternative flow sheets for a conventional zinc electrolysis plant are presented.

Jan 1, 1990

By D. Papazoglou

This work was undertaken to investigate the thermodynamic and kinetic feasibility of using hot sulfur dioxide bearing gases from smelting processes to selectively sulfate the nickel in nickel laterite ores for subsequent extraction in water. The environmental benefits ofthis approach, as opposed to releasing the gas to the atmosphere, and the economic benefit of directly utilizing the S02 rather than converting it to sulfuric acid are strong drivers for such a process. A thermodynamic analysis indicated that selective sulfation of the nickel could be feasible under appropriate conditions and these were explored through a series of laboratory scale experiments. Laterite samples were reacted at temperatures between 500 and 800°C with an equilibrated mixture of sulfur dioxide, oxygen and nitrogen in a fixed bed reactor. Tests were conducted on saprolitic ore from Bulong, Western Australia, limonitic ore from New Caledonia and garnieritic ore from Indonesia. Nickel extractions were highest from the limonite and relatively low from the other ores. The maximum selective extraction of nickel from the limonite in a single stage sulfation was 73%. Sulfation of other elements present in the laterites was also examined. A two-stage process was also identified which involved sulfation using a strong sulfation potential followed by weaker sulfation potential to attempt to convert ferric sulfate formed in the first stage to ferric oxide. This increased the extraction for the limonite ore to around 84% Ni, 95% Co and 2% Fe. Direct sulfation of laterite could be feasible in locations where sulfide smelting or roasting operations are relatively close to laterite deposits.

Jan 1, 2003

By D. Papazoglou

This work was undertaken to investigate the thermodynamic and kinetic feasibility of using hot sulfur dioxide bearing gases from smelting processes to selectively sulfate the nickel in nickel laterite ores for subsequent extraction in water. The environmental benefits of this approach, as opposed to releasing the gas to the atmosphere, and the economic benefit of directly utilizing the SO2 rather than converting it to sulfuric acid are strong drivers for such a process. A thermodynamic analysis indicated that selective sulfation of the nickel could be feasible under appropriate conditions and these were explored through a series of laboratory scale experiments. Laterite samples were reacted at temperatures between 500 and 800°C with an equilibrated mixture of sulfur dioxide, oxygen and nitrogen in a fixed bed reactor. Tests were conducted on saprolitic ore from Bulong, Western Australia:, limonitic ore from New Caledonia and gamieritic ore from Indonesia. Nickel extractions were highest from the limonite and relatively low from the other ores. The maximum selective extraction of nickel from the limonite in a single stage sulfation was 73%. Sulfation of other elements present in the laterites was also examined. A two-stage process was also identified which involved sulfation using a strong sulfation potenrial followed by weaker sulfation potential to attempt to convert ferric sulfate formed in the first stage to ferric oxide. This increased the extraction for the limonite ore to around 84% Ni, 95% Co and 2% Fe. Direct sulfation of laterite could be feasible in locations where sulfide smelting or roasting operations are relatively close to laterite deposits.

Jan 1, 2003

By B. Mishra

Calcium and lithium gallides have been synthesized by powder metallurgy techniques in the stoichiometries that can be used as reduction alloys for the Rocky Flats Plant Salt-Scrub (SS) process. The SS process is performed to recover valuable metals from salts generated in the electrorefining and the molten salt extraction processes. Combustion synthesis has been optimized for variable heating rates up to the reaction ignition temperature and for green densities of the powder compacts in terms of the ignition temperature and the exothermic heating of the product in an effort to develop LiGa and CaGaz alloys. The problems arising from the melting point and density differences of calcium, lithium and gallium have also been studied. The SS alloy compositions were produced by mixing, pressing and sintering the metal-powders. The efficiency of the intermetallic alloy, Ca-17 wt. pct. Ga, as a reductant and the effect of gallium on salt clean- up has been discussed. Measurement of actinide recovery has been studied with cerium as the surrogate for the actinide metal. The development of an alloy for SS reduces a major contaminated waste disposal problem besides recovering the valuable reactive metal.

Jan 1, 1993

By D. Donald Downey

Pilot Testing Ion Exchange Resin (IEX) can go from very simple beaker testing to complicated column testing. Space velocities, regenerant quantities, loading capacities, ion leakage, are all terms that get accumulated together to prove or disprove a resin’s (or resins’) ability to load a single ion (or specific set of ions). Not getting all the resin’s operating parameters correct will disqualify (or at least skew) the results. Laboratory tests for capacity, moisture content, bead size, metals fouling, etc.—what does it all mean? At last count, there were over twenty-five separate ion exchange resin tests (analyses) that were available to end users. Standard testing procedures identify the resin properties but more specific procedures can be used to identify problems with equipment operation. Then, there are the costs to consider; simple cation resin testing (moisture content, total capacity and bead integrity) is in the $200/sample range. However, add to this Chatillon, Russian Ball Mill Test, HIAC particle size, metals and % regeneration test procedures and the lab work can increase to over $1000/sample. In this paper, the author will explain the “must-do” pilot and test procedures and why they are important and the key to understanding how resin performs ion exchange.

By W. L. Dalmijn

Glass recycling in the Netherlands 'has grown fr.om 10.000 to 300.000 tonnes per annum. The various advantages and problems of the glass cycle with reference to the state of the art in the Netherlands is given. Special attention is given to new technologies for the automated sorting of cullet with detection systems. In Western Europe the recycling of glass has, become a success story. Because of this, the percentage of ,glass cullet used in ,glass furnaces has increased. To meet the quality demands of the glass industry, automated sorting for the removal of stones, non-ferrous metals and other impurities ,had to be developed and incorporated in glass recycling plants. ;In Holland, Germany and other countries, the amount of glass collected has reached a level that colour-sorting becomes necessary to avoid market saturation with mixed cullet. Recently, two systems for colour-sorting have been developed and tested for the separation of bottles and culletin the size .range of 20 -50 mm. With the increased capacity of the new glass recycling plants, 120,000 -200,000 tpy, the quality systems have also to be improved and automated. These quality control systems are based on tile automated sorting technology developed earlier. for the glass recycling plants. The data obtained are automatically processed and printed. The sampling system and its relation to the theory of Gy will be described. Results of both developments in glass, recycling plants will be described.

Jan 1, 1995

By Richard S. Kunter

Artech Recovery Systems, Inc has developed a low pressure and temperature? leach process called the "Cashman Process" to extract metals from arsenical flue dusts and residues and fix the arsenic in an environmentally stable form as ferric arsenate (scorodite). The process was pilot tested at Hazen Research in an integrated plant including continuous recycle from August 1989 to October 1989 during which several tons of flue dust were processed. Based on this pilot program, the process was deemed technically feasible and produced commercially salable products. Residues from this pilot program were subjected to a long-term stability test jointly designed by PTI environmental services and the USEPA. The process, its versatility, and the nature of the products is discussed in some detail.

Jan 1, 1992

By B. Mishra

The major waste product of the alkaline extraction of alumina from bauxite [Bayer Process] is known as red-mud. Approximately, a ton of red-mud is produced for every two tons of bauxite that is mined. The red-mud produced from Jamaican bauxite is rich in hematite, alumina and titanium oxide. It has been shown that over 90 wt. pct. alumina can be recovered from red-mud by soda-ash sintering and caustic leaching. Hematite can be carbothermically reduced with a degree of metallization of over 94 pct. At this stage, the product could be charged through the tuyeres in an iron blast furnace or smelted to produce pig iron. The mineralogical characteristics of the reduced product are not amenable to magnetic separation for iron recovery. The problems associated with the use of reduced red-mud as an alternative to direct-reduced iron [DRI] has also been discussed. Special attention has been paid to lower the alkali content of the reduced material. If smelted, the concentration of titanium oxide in the slag will be significantly high justifying its recovery by an acid-leach process. This paper describes the successful efforts of iron and alumina recovery.

Jan 1, 2000

By M. Shevchenko

Integrated experimental and modelling research program on the phase equilibria and development of thermodynamic databases of the lead and copper metallurgical gas/ slag-matte-metal-solids systems (PbO-“Cu2O”-FeO-Fe2O3- ZnO-CaO-SiO2) is being undertaken to support improvements in the pyrometallurgical smelting and recycling processes. This is the first systematic investigation of phase equilibria of slag systems in equilibrium with Pb metal, providing information for systems in which copper coexists in slag with lead or zinc as major components. The experimental studies involve high-temperature equilibration of synthetic samples, rapid quenching, and measurement of the compositions of equilibrium phases using electron probe X-ray microanalysis (EPMA). FactSage-based thermodynamic database development is integrated with experimental research. Initial thermodynamic assessments are used to identify priority compositions and conditions for experiments, which are planned to provide specific data to assist thermodynamic optimisation. Significant improvement in the accuracy of the phase equilibria description is achieved. Continuous database improvement and extension to include new elements are targeted. Example of industrial application is given.

By G. K. Ruhlandt, C. W. Kim

"A 3-D Finite Element Method program called ""SOLCAST"" has been developed to simulate the casting solidification process. Using the temperature recovery method to evaluate the latent heat of fusion and applying a new combination of the time integration scheme, SOLCAST reduces the computational time significantly compared to an existing commercial FEM program, and produces accurate results comparable to experimental casting results. Prediction of casting shrinkage porosity for A390 aluminum alloy will also be discussed. To make this FEM program useful for foundry engineers, this program was connected to a commercial pre- and post-processor.IntroductionBecause of recently increased competition, foundrymen must produce high quality castings more economically. Therefore, casting solidification analysis prior to casting production is an attractive way to reduce costs and development time.Although the actual casting solidification process is a very complicated phenomena, foundrymen could predict where shrinkage defects would occur based on a transient conduction heat transfer analysis that includes the liberation of latent heat. A numerical analysis is generally required to solve the heat diffusion equation with the latent heat diffusion term, because casting shapes are very complicated and pure materials are rarely used.Different numerical methods have been applied to the casting solidification analysis 1. Among them, a finite difference method 2 and a finite element method (FEM)3 are most commonly used.Each simulation method has one or more basic difficulties which are different for each method. These difficulties are:(1) Modeling casting shapes on a computer.(2) Time consuming computation.(3) Uncertain material properties."

Jan 1, 1986

By H. Senoh

For the purpose of clarifying the reason caused a drastic decrease of discharge capacity for MmNi3.6Mn0.4Al0.3Co0.7 electrode at relatively low temperatures, various factors influencing the charge-discharge processes were investigated in the temperature range of 25°C to -40°C. The charge efficiency obviously decreased at low temperatures less than 0°C due to a decrease in the rate of the charge-transfer reaction on the electrode surface. Moreover, both the rate of the hydrogen diffusion from the alloy bulk to surface and the rate of the charge-transfer reaction significantly influenced the high-rate dischargeability. The addition of Mo to MmNi3.6Mn0.4Al0.3Co0.7 alloy was found to be effective for improving the electrocatalytic activity, leading to the improvements of the charge efficiency and the high-rate dischargeability at relatively low temperatures.

Jan 1, 2002

By Yichi Lu, Haydn N. G. Wadley, Douglas T. Queheillalt

"Using a 3-D ray tracing methodology combined with laser ultrasonically measured elastic constant data near the melting point, ultrasonic propagation in cylindrical single crystal bodies containing either a convex or a concave solid-liquid interface have been simulated and used to design new sensing concepts. Ray paths, wavefronts and time-of-flight (TOF) of rays that travel from a source to an arbitrarily positioned receiver have been calculated. Experimentally measured TOF data have been collected using laser generated/detected ultrasound on model systems with independently known interface shapes. Both numerically simulated data and experimental results have shown that the solidification (interfacial) region can be identified from ultrasonic transmission TOF data. Since convex and concave solid-liquid interfaces result in distinctively different TOF data. When TOF data collected in the diametral plane are used in a nonlinear least squares algorithm, the interface curvature has been successfully reconstructed and ultrasonic velocities of both the solid and liquid obtained. The reconstruction errors were found to be less than 5%.IntroductionMany of today's single crystal semiconductors are grown by variants of a vertical Bridgman technique in which a cylindrical ampoule of a molten semiconductor is translated through a thermal gradient, resulting in directional solidification and the growth of a single crystal, Fig. 1.1 It has long been recognized that during crystal growth the velocity and the shape of the solid-liquid interface, together with the local temperature gradient, control the mechanism of solidification (i.e. planar, cellular or dendritic), the likelihood of secondary grain nucleation/ twin formation (i.e. the loss of single crystallinity), solute (dopant) segregation, dislocation generation, etc. They thus determine the crystals' resulting quality.2-4 The solidification rate and the solid-liquid interface shape are also sensitive functions of the internal temperature gradient (both axial and radial) during solidification.5•6 This in turn is governed by the heat flux distribution incident upon the ampoule, the latent heat release at the interface, and heat transport (by a combination of conduction, buoyancy and surface tension driven convection, and radiation) within the ampoule. The solid-liquid interface's instantaneous position, velocity and shape during crystal growth are therefore difficult to predict and uncontrolled during growth, especially for those semiconductor materials with low thermal conductivity (e.g. CdTe).4-6 The development of technologies to non-invasively sense the interface position and shape throughout the vertical Bridgman crystal growth process has therefore become a key step toward developing a better understanding of the growth process, for enabling sensor-based process control, and thus ultimately for improving the yield and quality of difficult to grow semiconductor materials like CdTe."

Jan 1, 1997

By H. Y. Sohn

The ignition and combustion of chalcopyrite particles under suspension-smelting conditions, in which the particle-particle interaction is neglected, has been analyzed by considering the intrinsic kinetics of oxidation and heat and mass transfer between the particle and its surroundings. Reasonable agreement has been obtained between the calculated results and experimental results from a laminar-flow furnace reported in the literature. This computation- al procedure has further been applied to flash-smelting conditions. Under suspension-smelting conditions (Sh = Nu = 2), chalcopyrite particles ignite at around 960 K. The effects of various parameters, such as oxygen concentration, particle size, and gas temperature, have also been evaluated. Comparison between calculated results in this work and experimental observations indicates that SO is the important gaseous product that forms at the surface of the particle.

Jan 1, 1993

By Jefferson Caponero

The tire is an expressive component of Municipal Solid Waste, manly when its occupied volume is considered. Its treatment by pyrolysis stands for a list of advantages, such as: landfill releasing and a production of a high quality fuel. The exploitation of new natural resources is becoming more difficult each day, basically due to the environmental damages caused by this type of activity. This work presents a study on the thermal behaviour of Brazilian tires using thermogravimetric analysis and differential thermal analysis, in order to optimise the pyrolysis process of tires. Samples of I to 2 mm were investigated at atmospheres of nitrogen, argon, oxygen and mixtures of these gases at temperatures up to 1273K, under heating rates between 1 to 50 Klmin . The results showed that the behaviour of each sample is related to both the atmosphere composition and the heating rate.

Jan 1, 2001

By Xuan Cheng

The electrochemistry of sulfide mineral flotation is reviewed with particular emphasis on galvanic interaction among minerals and grinding media, and its relevance to flotation of complex sulfide ores is discussed. Surface alteration due to galvanic interactions among chalcopyrite, pyrrhotite and mild steel is analyzed in terms of voltammetric and chronoamperometric studies on individual minerals and through galvanic current measurements in 2- and 3- electrode combinations. The results are related to laboratory flotation behaviors of chalcopyrite-pyrrhotite mixtures simulating copper-nickel bearing Duluth gabbro.

Jan 1, 1993

By T. T. Chen

Gold in the Twin Creeks ore is primarily associated with arsenian pyrite. During pressure oxidation, the sulphides are solubilized, but part of the dissolved iron reprecipitates as jarosite and as an iron sulphate-arsenate-phosphate phase. The pressure oxidation products are subjected to cyanide leaching. The cyanide leach residues consist of quartz, gypsum, bassanite, anhydrite, small amounts of jarosite, an iron-sulphate-arsenate-phosphate phase, as well as trace amounts of orthoclase, rutile, pyrite, hematite and monazite; all these particles are dispersed in a fine grained matrix of illite-muscovite. The autoclave leach residues contain a small amount of carbonaceous matter. Many gold grains are detected on the surfaces of the carbon particles, and these gold particles are not leached during cyanidation. The gold particles are typically 0.1-0.2/Lm in size and commonly are embedded in the carbon surface or are coated with a K-AI-Si-S-O phase on the surface of the carbon. The gold grains are consistently associated with elevated CI contents (50-300 ppm Cl). The poor gold cyanide leach recoveries, which initially occurred in the Twin Creek developmental circuit under certain operating conditions, are attributed to the presence of chloride in the feed. This results in the formation of soluble gold chlorocomplexes in the autolcave and the subsequent sequestering of the gold on the surfaces of the carbon particles.

Jan 1, 2000