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By Evan O. Jones

Processes involving distillation under reduced pressure were developed at the Pacific Northwest Laboratory several years ago to recover spent acid solutions generated during the manufacture of nuclear fuel for the N-Reactor at the Hanford site. Following construction and testing of a pilot-plant, the technology was licensed to Viatec Recovery Systems, Inc. for commercialization. The technology developed included specialized distillation and rectification of volatile acids, removal of water and/or volatile acid from sulfuric acid, and precipitation of salts. A key feature of the Waste Acid Detoxification and Reclamation (WADR) technology is the development and use of advanced thermoplastic and fluoropolymer materials of construction in all critical process equipment. The technology was then expanded to include crystallization to recover metal salts for possible reuse. Economic and environmental advantages of the procedures include recovery of acids for reuse, simplification or elimination of the disposal of waste solutions, and possible recovery of metals. Industries expected to benefit from such applications include galvanizing, electroplating, sand leaching and any where metals are cleaned in acid solutions. Currently a modular system has been assembled for recovery of several different spent acid solutions.

Jan 1, 1995

By Louis J. Cabri

The ion microprobe (dynamic SIMS technique) is a very sensitive instrument for the quantitative determination of trace concentrations of precious metals (often at the ppb level) occurring in common sulfide minerals, either chemically-bound or as discrete particles too small for resolution by SEM. The technique involves sputtering a 250 x 250 Jim area of the grains to a depth of about one ILm and analysing the secondary ions emitted from a circular central region in the sputter crater with a 62.5 I'm diameter. The combination of quantitative mineral-specific sub-ppm analyses together with depth-profiling and the ability to produce secondary ion maps of trace precious metals makes this a very powerful technique in quantifying the precious metal distribution in refractory and other sulfide ores and process products. The technique is particularly well-established for analysis of gold-and platinum-bearing ores and process products.

Jan 1, 1996

By Hsin H. Huang

Equilibrium calculational software programs can be effectively utilized to model the importance of activity or concentration, solubility, temperature, solution pH, solution potential, and ligand complexation on extraction and recovery processes. Illustrative examples using the calculational program ST ABCAL for the creation of diagrams such as EwpH, activity or concentration-pH, and activity or concentration-EH are presented to demonstrate the fundamental characteristics of real hydrometallurgical mercury dissolution and recovery processes. An industrial application will include leaching of mercury from K 106 mercury sulfide waste and solution purification by iron cementation.

Jan 1, 2003

By Hiroaki Kawamura, Takeshi Yoshikawa, Kazuki Morita, Yutaka Yanaba

"To develop an alternative metallurgical process for phosphorus removal in the production of solar-grade silicon (SOG-Si), slag treatment of metallurgical-grade silicon (MG-Si) was conducted, followed by acid leaching. Phosphorus-doped silicon alloy or MG-Si containing certain amounts of phosphorus and calcium was reacted at 1723 K and 1773 K with CaO--CaF2 of several compositions. Phosphorus removal from the molten silicon into the slag phase was confirmed by reduction to phosphide ions, P3-, and phosphate ions, P3-. These ions were separately determined using a wet chemical analysis method developed by ourselves. The highest phosphorus distribution ratio obtained was 2. 7 after reaction for 18 h with 17.5 mass% CaO--CaF2 slag. We then conducted acid leaching of the silicon and achieved removal of a large fraction (over 90 % ) of the phosphorus, which was much higher than that obtained by ordinary oxidizing slag treatment.IntroductionIn recent years, the production of solar cells has been increasing rapidly. Because of this, the demand for solar-grade silicon (SOG-Si) has also been growing rapidly. The development of lower-cost mass production processes is therefore needed to provide silicon feedstock. Phosphorus is one of the impurities in metallurgical-grade silicon (MG-Si). Because of its large segregation coefficient (kp = 0.35) [l ], it is difficult to remove phosphorus using a solidification refining process. Vacuum melting is considered to be a promising method for removing phosphorous from MG-Si [2], but the issues of high cost and large energy consumption have still to be resolved.Slag treatment is often used to remove impurity elements by oxidizing reactions during general oxidation refining processes. For example, phosphorus in molten steel is removed into a slag phase as phosphate ions, PO4 3-l-, by the following reaction:"

Jan 1, 2013

By Satoshi Yamashita, Noboru Masuko

"Newly prepared bipolar membrane is promising to become a key material of an electrolyser for a production process of strong reducing solvent. This research is basic research for using bipolar membranes as electrolysers of reducing agents, Cr(II), TI(III) and V (II) on the laboratory scale. In this report, a bipolar membrane was tried with an electrolyser, reducing chromic chloride to chromous chloride. An analysis of mass balance demonstrates advantages of it over the former electrolyser equipped with an anion and/or. cation exchange membrane. The effects of current density and concentration of Cr(lll) on the reduction rate of Cr(II) and the current efficiency were examined No deterioration of the bipolar membrane resulted from the electrolytic reduction of Cr(III). IntroductionRecently, bipolar membrane that was the development subject for a long time in the industry of ion exchange membranes has met the stage of the practical application at last [l]. The expectation of the application to the hydrometallurgy field increases. We took up the manufacturing of the strong reducibility solvent as part of the application of bipolar membrane to hydrometallurgy technology. This laboratory has much experience in the electrolytic reduction of Cr (II) aqueous .solution such as chromous sulfateusing bipolar membrane were compared in theory to chromous chloride aqueous solution manufacturing of the strong reducibility solvent. The advantage of applying bipolar membrane by substituting ion exchange membrane is described, and the experimental result is reported."

Jan 1, 2000

By F. M. Nakla

Various methods of Applied Mineralogy were used for determining the nature and composition of products yielded by flotation tests for Maghara coal beneficiation. Coal samples obtained from the Sa fa mine in Northern Sinai, Egypt, were crushed, sieved, &apos;and <32 mesh size fraction was cleaned by froth flotation. Experiments were conducted to determine the effect of certain parameters on beneficiation of Maghara coal by flotation. The investigated factors included nature of frothing and/or collecting reagents, pH value of the medium, particle size distribution in the head sample, and pulp density of the coal slurry. The quality of head samples, coal concentrates, and tailing products were determined by chemical analysis, microscopic study, x-ray diffraction analysis, and occasionally by infrared (IR) absorption spectroscopy.

Jan 1, 1989

A rotating-discelectrode system was used to evaluate the electrochemical behaviour of Eu(III) during its reduction in NaCl solutions. The solution pH and NaCl concentration have a great effect on the reduction kinetics. The thermodynamic modelling study also revealed that Eu(III) exists in various forms in NaCl solutions. At a low concentration of NaCl, the predominant species is the free Eu3+. Other Eu-chloro complexes become more predominant when the NaCl concentration increases.

Jan 1, 1992

By André L. de Vegt

Soil and groundwater beneath a zinc production plant in The Netherlands are contaminated with metals and sulfate. To avoid contamination of nearby drinking water aquifers, a hydro-geological containment system and a biological treatment plant for the extracted ground water have been installed. Currently about 5000 m3/day of groundwater is extracted from a combination of 12 shallow and deep wells. Heavy metals and sulfate have to be removed from the extracted water before it can be discharged into a river. Several water treatment methods have been studied and pilot tested at the site. The preferred and selected process is based on the activity of sulfate reducing bacteria (SRB) and combines sulfate removal and heavy metal removal in one single installation. Anaerobic bacteria reduce sulfate to sulfide resulting in the precipitation of metal sulfides. Excess sulfide Is biologically converted to elemental sulfur. A full scale biological treatment system was started up in May 1992. Design, start-up, commissioning and operational experiences are reported in this paper. Concentrations of metals and sulfate in the SRB water treatment plant effluent are well within the limits set by the Dutch Authorities for discharge to surface water.

Jan 1, 1995

Designing rigging systems for complex castings has been more of an art than a science. Foundrymen have used thumb rules based on past experience to develop working designs. Of late, attempts are being made to formalize the procedure through the use of rule based expert systems, process modeling and other tools. Designing risers is one of the challenges of the rigging system design. Once the riser location have been determined, an optimization technique coupled with a casting simulation code can be used to determine the optimum riser dimensions. The main drawback of using a finite element or a finite difference based process simulation code along with the optimization routine is that the computation time involved is too large. Such an approach, thus, is unrealistic for practical situations where different options have to be explored and conclusions drawn in a short period of time. This difficulty has been avoided in the present work. The optimization scheme has been coupled with a modulus based solution routine to optimize the riser dimensions. The modulus calculations provide a good and quick estimate of the freezing time at different points in the casting. A functional, obtained from these freezing time values, is minimized by altering the dimensions of the riser until an optimum shape is obtained. Some examples have been included to illustrate the utility of this technique.

Jan 1, 1994

By Yutaka Shiraishi

Two methods were developed to measure the viscosity of the slag from the glassy to the liquid states in an ascending temperature process. The first method employs rotating parallel plates within which is placed a solid cylindrical sample in line with a sphere. The second method uses a tube which is pushed into a sample held in a rotating crucible. Both methods were tested using standard glasses, including boron trioxide and NBS standard glass #711. The main difference between these two methods is in sample preparation. Comparative measurements between two methods were performed using a sodium boro-disilicate glass containing 5%mol of alumina. The results showed good agreement in the mid-range of glassy viscosities, 105 to to7 Pa.s. In the liquid state, there were no significant differences between the two methods.

Jan 1, 2003

By Shujian Jia, Mingming Song, Gaoyang Song, Bo Song, Yuhou Yang

An innovative method is investigated to separate inclusion particles from liquid metal by super gravity. To make clear the characteristics of the inclusion separation, Al melt containing MgAl2O4 particles with diameters less than 150 μm has been treated under various super-gravity fields. The thickness of particle-accumulated layer formed at the bottom of the sample and the area fraction, number density and size of inclusions were measured. It is found that the thickness of the particle-accumulated layer decreases and the area fraction of particles at this location increases with the increase of super-gravity field. With the gravity coefficient G=500, time t=2 min, and temperature T=1023 K, it is hardly to find any solid particles in the upper and middle areas of the sample and the separation efficiency is up to 90%.

Jan 1, 2015

By Tim Robinson, Georges Houlachi, Michael Moats, Marco Ginatta, Michael Free, David Creber, Neale Neelameggham, George Holywell

"Electrolytic processing is used commercially to recover and/or refine metals such as aluminum, copper, magnesium, nickel, and zinc. There are also new and exciting opportunities to utilize electrometallurgy in the production of titanium, lead, and other metals. This paper reviews some of the main technologies that are used to produce and refine metals as well as some of the recent advances and future directions the electrometallurgy industry may implement to meet the challenges faced now as well as those that are likely to be faced in the future.IntroductionElectrolytic processing is used commercially to recover and/or refine metals that include large scale production for metals such as aluminum, copper, magnesium, nickel, and zinc as well as small scale production for metals such as gold and silver. There are also new and exciting opportunities to utilize electrometallurgy in the production of titanium, lead, and other metals. This paper will focus only on electrometallurgical processing of metals with relatively large production markets."

Jan 1, 2012

By V. Blet

Rare earth elements (REE) are regarded today as highly critical raw materials but currently lack suitable recycling processes. A combined hydro- and pyrometallurgical process aimed at REE recovery from used NdFeB permanent magnets was recently developed by the CEA. The process integrates the physico-chemical treatment of magnets, followed by a solvent extraction step for the recovery and intra-REE separation using a selective extractant. A subsequent pyrometallurgical treatment via molten chloride salt electrolysis allowed the isolation of pure Dy metal. Technical-economic assessment and life-cycle analysis were also conducted. Following this first successful demonstration, a new project aimed at the recovery of REE from end-of-life nickel-metal-hydride batteries is currently being developed in association with industrial and academic partners. The project aims at evaluating from an experimental and economic perspective different processes converging at the production of value-added products such as cermet materials for catalytic applications, purified REO concentrates, or metallic alloys.

"Hematite pellets were electro-deoxidized to iron in molten sodium hydroxide to produce iron containing about 10-wt % oxygen. The anodic reaction was the evolution of oxygen on an inert nickel anode. Before the electrochemical reaction, there is a reaction between sodium hydroxide and ferric oxide to form sodium ferrite and, in order to compensate for the reduction in sodium oxide content, 1 wt % sodium oxide is added to the melt. In a laboratory cell, the cell voltage was 1.7 V with a current density of 5000 A m-2, a current efficiency of 90% and an energy consumption of 2.8 kWh kg-1.Introduction The iron and steel industry contributes about 2.3 bn tonnes/annum of the carbon dioxide to the atmosphere, which is about 10% of the total, and some believe that, in order to prevent a catastrophic rise in the earth’s temperature, carbon dioxide emissions must be reduced by 50% come 2050. However, by 2050, it is likely that the iron and steel industry would have grown significantly so that the production may have risen to 2 or 3 bn tonnes/year so in order to meet the 50 % reduction on today’s figure, the carbon dioxide may have to be reduced to 25% or less, which is a very demanding requirement. There are probably three ways of reducing the carbon dioxide output:1. By capture and sequestration, but this may be technically very demanding.2. Reduction using hydrogen in place of carbon."

Jan 1, 2009

By Z. Zhang, Cuihuan Huang, Zongshu Zou, Nan Wang, Xueqian Xin

"Vitrification is considered as an attractive procedure for municipal solid waste incineration ash, which can realize the volume reduction and innocent treatment of incineration ash, as well as reuse of bottom ash. The main oxide components of molten ash slag are CaO, Al2O3, SiO2, Fe2O3, MgO, and Na2O, accounting for more than 90% of the total mass. The phase relations and thermodynamic properties of the CaO-Al2O3-SiO2-FeOx-MgO-Na2O oxide system is highly required, and is of great scientific significance for optimization of vitrification processing and sustainable resource utilization of melting slag. A study on the equilibria phase relations of CaO-SiO2-MgO-FeOx system was done by using CALPHAD method based on FactSage in this paper. The modeling parameters for the thermodynamic properties of liquid phase in CaO-SiO2-MgO-FeOx system were established and the equilibrium phase relations of MgO-SiO2-FeOx and CaO-SiO2-FeOx-MgO systems were calculated for different temperatures and oxygen partial pressures.IntroductionThe main oxide components of vitrified bottom ash slag are CaO, Al2O3, SiO2, Fe2O3, MgO, and Na2O, accounting for more than 90% of the bottom ash by weight [1]. During slag processing and modification, the knowledge of thermodynamic properties and liquidus temperature in the related slag system is highly required [2-5], which is not yet available. Through literature survey [6-9], it is clear that the systematic information on the concerned complex slag system is scarce. Most binary subsystems except FeOx-Na2O have been investigated well. Among ternary subsystems, few phase relations of the Na2O-MgO-SiO2 ternary system are available. For the phase relations of the system Na2O-MgO-Al2O3, all the studies are focused on the Al2O3-rich region. Investigation on the CaO-Al2O3-FeOx system is limited to Fe2O3-containing system with relatively higher oxygen potential. Most quaternary systems are not studied well except the CaO-MgO-Al2O3-SiO2 system, mainly due to their metallurgical importance. Figure 1 demonstrates the research status of the vitrified bottom ash slag with almost zero effort [10]. The effort here is defined based on the published literature by considering the number of publications, the investigated composition ranges, and the research details. So far the engineers in the field have to make assumptions of the thermodynamic properties of the simplified oxide system, without taking into consideration the interactions of the different oxide components, which hinders the development of the slag valorization and utilization. In order to provide thermodynamic properties for the application of the vitrified bottom ash, the six-component oxide system (CaO-MgO-Al2O3-SiO2-FeOx-Na2O) will be investigated through both experimental approach and computer modeling."

Jan 1, 2011

By Patrick R. Taylor

This investigation studied the inflight calcination kinetics of nuclear waste simulant using a thermal plasma reactor. A series of experiments were performed to determine the conversion of insoluble aluminum compounds to the soluble compounds and the decomposition of complex organic and nitrite compounds present in the simulant waste. Thermodynamic calculations based on free energy minimization were performed to establish a theoretical basis for this investigation. A kinetic model to describe the conversion of gibsite to sodium aluminate has been proposed. The products of the calcination were characterized using XRD, Gas Chromatography, and chemical analysis by ICP. The results of this investigation indicated 85% gibsite conversion to sodium aluminate, 90% of nitrate decomposition, 52% TOC decomposition and 90% conversion of chromium to soluble compounds. A process is identified for inflight calcination of wastes. Key words: Plasma, waste, simulant, calcination

Jan 1, 1996

By Charles I. Richman

Aquispirillum magnetotacticum (AM) is gram-negative hetrotrophic bacteria that belongs to a class ,of magnetotactic bacteria that have an ecological niche in marine marches and fresh water swamp sediments. Thiobacillus Ferrooxidans (TF) is a Gram-negative, acidophillic chemoliths that may have similar chemical conditions within the cytoplasmic membrane as Aquaspirillum M. to support growth of Magnetosomes. Magnetosomes are cellular bodies that accumulate under slightly aerobic conditions. Magnetotactic motion occurs in an external magnetic field and depends on the medium viscosity. The Atomic Force Microscope equipped with a magnetic tip shows the presence of Magnetosomes in these bacteria strains. The size, shape of magnetosomes in AM and TF strains are characterized.

Jan 1, 1998

By Katsukiyo Marukawa, Manabu Iguchi, Sigeta Hara, Shinichiro Yokoya, Sigeo Takagi

"A numerical analysis and water model study of the mold region of a continuous casting apparatus was performed with a novel injection concept using swirling flow in the pouring tube, to control the heat and mass transfer in the continuous casting mold.As a result, the following results were found:1) By changing swirl strength, it is easy to control the flow pattern as well as the direction of the flow.2) Uniform velocity distribution can be obtained within a very short distance from the outlet of the nozzle.3) Heat and mass transfer near the meniscus can be remarkably activated compared with a conventional straight type immersion nozzle without swirl.4) Swirl helps the superheat in the melt dissipate.S) Penetration depth of nozzle outlet flow is decreased remarkably by the application of swirling.6) For the case without swirl, the peak of the flow moves near the mold-wall with flowing down from the outlet of the nozzle due to the Coanda-effect. On the other hand, peak of the flow moves near the mold axis with flowing down from the nozzle-outlet within considerable short distance, namely axi-symmetric velocity distribution can be obtained within very short distance from the nozzle-outlet.Those findings mentioned above are very useful to control the flow pattern in the billet and bloom continuous casters."

Jan 1, 2001

By Hwa-Soo Park, J. K. Yoon, Hoseok Nam

In a thin slab casting process, control of fluid flow in mold is particularly difficult due to the high casting speed and large aspect ratio of the mold and the understanding of the fluid flow motion as well as heat transfer in mold is regarded as the most important information because the melt delivery is directly related to the problems of shell growth nonuniformity, surface turbulence and mold powder entrapment. A mathematical model has been developed for the coupled analysis of fluid flow, heat transfer and solidification in funnel type mold using finite volume method based on a body fitted coordinate and the characteristics of the transport phenomena in the mold of thin slab caster were analyzed by numerical simulation. As a result of simulation, the basic flow pattern is characterized as four large recirculations and two small eddies near the narrow faces of mold, which is somewhat different from that of parallel type mold or other conventional slab caster. The heat transfer model accurately predicted the mold positions susceptible to cracking as a result of thermal stress and the predicted shell thickness shows good agreements with the measured shell thickness on breakout products. We also investigated the influences of some operation parameters such as casting speed, nozzle type, submerging depth and mold material on fluid flow, heat transfer and distribution of solidifying shell and various information for the determination of optimal operating conditions were obtained.

Jan 1, 2000

By Gabriel Riveros

Fire refining of copper consists of two stages copper oxidation and copper reduction. Very frequently the capacity of the anode furnace is determined by the rate of copper reduction. The analysis of factors affecting the rate of the oxygen reduction from a liquid copper with solid carbon or injected hydrocarbons pointed out the role of the mass transfer in a liquid copper in final stage of the reduction. Experimental results of copper reduction with graphite and injected natural gas in laboratory- scale crucibles showed two stages of the reduction process with a sharp change of the controlling mechanism. The estimated dynamic surface area of gas bubbles based on the measured bubble frequency and the gas flowrate allowed for the detennination of the reaction constant as a degree of the partial pre-combustion of the air/natural gas mix. The variation of the used reductant as a function of the oxygen concentration and temperature has been evaluated based on the detennined kinetic model. The intensification of copper reduction in fire refining has been discusses on the basis of obtained kinetic data and analysis of various factors detennining the time of reduction.

Jan 1, 2003