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By Larry M. Southwick

Considerable process and equipment development and analysis were conducted during design of Freeport Sulfur's laterite nickel facilities in the late 1950's. These covered ore concentration at Moa Bay, Cuba, and concentrate refining at Port Nickel, Louisiana. Both facilities utilized acid pressure leaching and product refining steps that were similar to those later used elsewhere in the laterite processing industry. Unfortunately, developments in Cuba removed the Moa Bay facilities from Freeport control. This deprived the project of a start-up that would have allowed thorough resolution of difficulties and a quicker attainment of production capacity. This meant lost opportunity to positively prove and complete the technology when optimum resources and staff were available. This paper reviews the original rationale of how design was developed via laboratory, bench scale and pilot studies by Freeport Sulfur. Some later operating problems will also be discussed. This case is unusual, but the lessons learned may be instructive in the application of difficult and complicated technologies, as well as the need to understand and retain access to the original development and design activities Keywords: Moa Bay, Freeport Sulfur, Port Nickel, acid pressure leaching, pilot plant, pachuca, Chemical Construction, pressure letdown, cobalt, titanium

Jan 1, 2004

By Peter R. Sanford

Cyanides are present as a dilute constituent of streams from a variety of metallurgical and mineral-processing operations. In addition, a cyanide concentration in excess of approximately 100ppb is toxic to aquatic life, and consequently these operations require a waste-treatment process to reduce the already dilute cyanide species by several orders of magnitude. Furthermore, the waste streams may have flowrates in excess of a million gallons per day. The paper reports on research conducted with a laboratory?scale electrochemical porous (graphite felt) electrode (anode) flow-reactor, which was conducted in conjunction with a computer-aided simulation of a mathematical model describing the intrinsic rate-phenomena associate with the electrode processes. The laboratory-scale cell, of rectilinear geometry, was found to be capable of reducing a feed-stream anolyte (KCN-KOH and supporting electrolyte of a single salt ? K2SO4) with a cyanide concentration of 10ppm, to less than 100ppb, at current efficiencies in the neighborhood of 50%. The computer simulation of the cell performance based on the mathematical model (and constraints imposed for tractability) was found to provide only for qualitative agreement.

Jan 1, 1998

This paper describes developments in ferro-nickel furnace technology, specifically improvements to cooling methods, furnace controls, and high voltage furnace operating regime. The evolution of these technologies is briefly presented, as context for describing the current state of the art that has enabled ferro-nickel furnace operation at over 75 MW and specific energy consumption of less than 400 kWh/t dry ore. Examples from existing operations are used to illustrate present best practices, and potential future trends are discussed: The paper begins with an overview of the fundamental aspects of pyrometallurgical treatment of lateritic ores that drive ferro-nickel furnace design. Furnace wall cooling methods are related to the requirements resulting from specific furnace process conditions, including slag and metal compositions, as well as arc and bath power. The benefits of high productivity and low specific energy consumption resulting from high voltage (shielded-arc) operating practice are discussed, along with the furnace controls and electrical power train that enable such operation even with captive power generation. This paper is an update of that which the authors prepared for the Infacon X ferro-alloys conference.

Jan 1, 2004

By A. Dadgar

The adsorption kinetics of AuBr4 on Dowex ® -21K ion-exchange resin were studied and found to be independent of the initial gold, bromine, and base metals concentrations. A commercially-available undivided hypochlorite generating cell was used to generate bromine from simulated mixed halide (Br-/CI-) solutions. Electrolyses were performed with solutions containing very low Br' ion concentrations. The current efficiencies were 80-90%, and Br- ion utilization was maximized. A detailed economic assessment was made considering the capital and the operating costs for a 1000 mtpd gold ore processing plant. The toxicity and discharge levels of bromide, bromine, and cyanide were compared from a detailed analysis of the published literature data. Comparing bromine vapor with hydrogen cyanide gas for a given length of exposure, the lethal concentration of bromine is about 3 times less than hydrogen cyanide. The toxicity of sodium bromide is similar to that of sodium chloride. Acute poisoning to bromides and chlorides is rare because of their low toxicities. The allowed discharge levels of Br-, Br2, and CN- in fresh water are 250, 0.1, and 0.005 mg dm-3, respectively.

Jan 1, 1992

Cospidie (3CaO*2SiO2*CaFe2) is one of the most important compounds crystallized in mold flux films during casting in the continuous casting process of steel, The primary crystallization field of cuspidine has been experimentally developed in the CaO-SiO2-CaF2-SiF4 system. The cuspidine-NaF binary and cuspidine-CaF2-NaF ternary systems have been also experimentally determined to study effects of addition of NaF on the primary field of cuspidine. In order to discuss its thermodynamic stability the standard Gibbs energy of formation of cuspidine has been deterimed by an electromotive force methods using CaF2 as solid electrolyte and a transpiration method as follows: ^fG° (cuspidine) /kjmol-1 = 5198 + 0.825T (+12) (1313<T/K<1329): EMF method ^fG° (cuspidine) /kjmol-1 = 5178 + 0.813T (+8) (1221<T/K<1469): Transpiration method The chemical potential diagram and constituent activities for the CaO-SiO2-CaF2 System have been evaluated based on the obtained thermodynamic data.

Jan 1, 2003

By R. L. Nyirenda

One of the problems with ammoniacal-ammonium carbonate leaching of EAF carbon steelmaking flue dust is that zinc present in spinel phases is not leached. This paper presents results of test work in which prior to leaching, EAF dust was reduced with CO containing gas to decompose the spinels into zinc oxide and iron bearing phases, mainly metallic iron and wustite. From such reduction products, the amount of zinc leached increases but the iron co-leached becomes extensive. The effect of various leaching parameters such as liquor concentration and redox potential on zinc and iron dissolution has been investigated. Supplementary experiments utilizing pure zinc oxide and pure iron phases were also carried out. Results show that the co-dissolution of iron from severely reduced EAF dust cannot be prevented. This is because the wustite phase contains zinc which can only be leached when iron also dissolves. Further, the zinc bearing wustite phase is not totally soluble so that the residue cannot be made zinc free. In the absence of air, dissolution of metallic iron hardly occurred, though in leaching experiments of a long duration its transformation to a spinel structure was observed.

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

By C. R. Palmer

The Bureau of Mines investigated the use of ion-exchange technology for the recovery of precious metals from cyanide leach and spent electrolytic solutions. This research included adsorption of gold and silver on both weak-and strong-base anion-exchange resins. The effects of nickel, mercury. and iron on precious metal loading of strong-base resins were also determined. Due to the nonselectlvity of strong-base resins, selective elution also was investigated. Both commercially available and experimental weak-base anion-exchange resins were tested. None of the commercial weak-base resins tested were suitable for a caustic-cyanide system owing to their low recovery of precious metals at pH 10 or above; however, three experimental resins have possible application. Continuous tests conducted with mill cyanide solution in a multicompartmented ion-exchange column using strong-base anion-exchange resins adsorbed nearly 100 pct of the precious metals as well as the iron and nickel. During the elution of this loaded resin the iron was first removed with NaCI plus NaOH; then nickel with dilute H2S04 or HCl; finally gold and silver with thiourea in dilute HCl.

Jan 1, 1988

By Torn H. Okabe

A fundamental study was conducted with the purpose of establishing an environmentally sound recovery process for recycling of valuable metals, by combining scraps containing such metals. As an example, direct extraction and recovery of neodymium (Nd) in magnet scraps was investigated by utilizing liquid metal as an extraction medium. It was found that liquid magnesium (Mg) is a suitable extraction medium and can extract Nd from iron alloys with high efficiency at around I 100 K. The newly developed extraction apparatus for Nd is a mechanically simple and static device without moving parts, where the Mg extraction medium circulates due to differences in the temperature inside the reaction vessel. This developed device can simultaneously accomplish continuous extraction of metal Nd from scraps, re-extraction of Mg from Mg-Nd alloy and the eventual recovery of pure Mg. As a result, metal Nd with 98 % purity was directly recovered from magnet scraps under certain conditions. It was also shown that the extraction agent Mg could be reused. The results of this investigation show the possibility of establishing a new process for the direct extraction of Nd in pure metal form without oxidization.

Jan 1, 2003

By Torn H. Okabe

A fundamental study was conducted with the purpose of establishing an environmentally sound recovery process for recycling of valuable metals, by combining scraps containing such metals. As an example, direct extraction and recovery of neodymium (Nd) in magnet scraps was investigated by utilizing liquid metal as an extraction medium. It was found that liquid magnesium (Mg) is a suitable extraction medium and can extract Nd from iron alloys with high efficiency at around 1100 K. The newly developed extraction apparatus for Nd is a mechanically simple and static device without moving parts, where the Mg extraction medium circulates due to differences in the temperature inside the reaction vessel. This developed device can simultaneously accomplish continuous extraction of metal Nd from scraps, re-extraction of Mg from Mg-Nd alloy and the eventual recovery of pure Mg. As a result, metal Nd with 98 % purity was directly recovered from magnet scraps under certain conditions. It was also shown that the extraction agent Mg could be reused. The results of this investigation show the possibility of establishing a new process for the direct extraction of Nd in pure metal form without oxidization.

Jan 1, 2003

By Z. Jing, L. Qihou, C. Jun, L. Hui, Z. Yumeng

Three phases of Bi2O3 were first synthesized by extraction-stripping precipitation and post decomposition from BiCl3 leaching solution. The as-prepared Bi2O3 were characterized by X-ray powder diffraction (XRD), Fourier transform infrared spectra (FT-IR), scanning and transmission electron microscopy (SEM, TEM), UV-vis diffuse reflectance spectroscopy (UV-vis DRS), Brunauer-Emmett-Teller (BET) and X-ray photoelectron spectroscopy (XPS). The photocatalytic performances of the oxides were investigated by decomposing rhodamine B (RB) under visible irradiation. It shows that the Bi2O3 with different crystal structures and morphology were obtained under different decomposition temperature. The band gaps of as-prepared samples were 2.36, 2.41, and 2.78 eV for b-Bi2O3, a-Bi2O3, and d-Bi2O3, respectively, and the photocatalytic activities followed the order: b-Bi2O3 > a-Bi2O3 > d-Bi2O3, which was in good accordance with the photoluminescence spectra measurement results. The b-Bi2O3 exhibited the best photocatalytic performance which can effectively degrade 99.23% RB within 240 min.

Mar 1, 2018

By Enrui Dai, Weibing Chen, Bin Yang, Wenhui Ma, Haisheng Fang, Hui Wang

LiMn0.8Fe0.2PO4/C composite was prepared by an improved solid-state method and the effect of calcination temperature on properties of the obtained materials was investigated. The results showed that increasing calcination temperature from 600 to 700 oC improved the performance of the LiMn0.8Fe0.2PO4/C due to enhanced crystallinity and increased conductivity, but further increase in calcination temperature to 800 oC led to degraded performance due to particle growth and decrease in porosity. Therefore, the LiMn0.8Fe0.2PO4/C composite prepared at 700 oC exhibited the best electrochemical performance, and could deliver a high capacity of 152 mAh g−1 at 0.1 C, 147 mAh g−1 at 1 C and 114 mAh g−1 at 10 C. In addition, the performance of the LiMn0.8Fe0.2PO4/C and LiMn0.8Fe0.19Mg0.01PO4/C was compared when they were obtained at the optimum calcination temperature.

Jan 1, 2015

By Dong Joon Min, Joo Hyun Park, Mi Sun Choi, Jae Hong Shin

Sublimation of ZrCl4 is important for the production of nuclear grade metallic Zr in Kroll’s process. The sublimation kinetics of ZrCl4 was investigated by TGA under both isothermal and non-isothermal conditions. The sublimation rate of ZrCl4 increased with increasing temperature under isothermal conditions. ZrCl4 sublimation was confirmed to be a zero-order process under isothermal conditions, whereas it was first-order kinetics under non-isothermal conditions. The activation energy of ZrCl4 sublimation under isothermal conditions was 21.7 kJ/mol. The activation energy for non-isothermal sublimation was 101.4 kJ/mol and 108.1 kJ/mol with the Kissinger method and Flynn- Wall-Ozawa method, respectively. These non-isothermal activation energies were very close to the heat of sublimation (103.3 kJ/mol). Sublimation occurs by two elementary steps: surface reaction and desorption. Therefore, the overall activation energy of ZrCl4 sublimation is 104.8(±3.4) kJ/mol. The activation energy of the surface reaction and desorption steps are proposed to be 83.1 kJ/mol and 21.7 kJ/mol, respectively.

Jan 1, 2014

The generation of acid mine water is? due to the oxidation and weathering of sulfide bearing tailings and overburdens. Ferrite precipitation prooess has been applied to treat acid mine water. The conventional ferrite preC1pitatlon requires air oxidation at high temperature, or long aging time or addition of magnetite powder ,as promoter. In this investigation, a modified ferrite, precipitation process is developed by which magnetic ferrite can be produced at an ambient temperature. Acid mine waters from Berkeley Pit (Montana, U. S. A.) and from Noranda Tailings (Quebec, Canada) were used. The co precipitation of heavy metals from these two acid mine waters is studied as a function of FeIM molar ratio, oxidation time and settling rate under applied magnetic field. The investigation indicates that the modified ferrite co precipitation can remove substantially all of the, dissolved metal ions from acid mine water. The ferrite product obtained after precipitation&apos; is characterized by XRD, SEM, BET and saturation magnetization. The results show that spinel ferrite, precipitation can be achieved at room temperature and the saturation magnetization of ferrite product from,acid mine water is comparable to that of pure ferrites.

Jan 1, 1995

By Bing Li, Miao Shen, Qiang Wang, Yuqi Chen

Electrochemical methods including cyclic voltammograms, square wave voltammograms, chronopotentiometry are applied to characterize the reduction potentials of Na+ and Li+ ions in LiCl-KCl melts. According to theoretical calculation, the reduction potential for Na+ is slightly more negative than Li+ in NaCl-LiCl-KCl melts at 450℃. However, by electrochemical measurements, the reduction potential of Na+ is slightly more positive than Li+ in the above melt and the potential difference between Na+ and Li+ reaches 0.16-0.2V on an inert W electrode in 1.0-2.0 wt% NaCl-LiCl-KCl melts. An active Pb electrode is used to improve the removal rate of Na+ from LiCl-KCl melts. The reduction potentials for both Na+ ions and Li+ ions on a Pb electrode shift to more positive values and the reduction currents become larger. After 6h electrolysis on a Pb electrode at -3.0V, the practical removal efficiency of Na+ ions reaches 90.12% and the reduced products contain metallic Na and Li with a Na/Li mass ratio of 4.25/1.

Jan 1, 2015

By Petr Dvorak, Jana Selucka, Hong Vu, Petra Starkova, Tomas Frydl

Waste, generated during high pressure leaching of lateritic nickel ores, contains about 50% of iron in form of magnetite but high chromium content ( *3%) does not allow its extensive utilization as the raw material for pig iron production in blast furnace. The chromium removal from the waste was carried out by two methods: (1) oxidative alkali roasting with NaOH and/or Na2CO3, followed by water leaching and (2) oxidative leaching in KOH sub-molten salts solutions. The results show that about 90.1% of Cr was removed when the waste was roasted at 900 °C for 3 h with 33.1 wt% of NaOH. The removal of 88.2% of Cr was achieved if the waste was roasted at 900 °C for 3 h with 40 wt% of Na2CO3. The sodium content in the water-leached residues was reduced from 5% to about 0.5% by reaction with CaO in aqueous solutions at 80 °C for 2 h. About 70% of Cr was removed if the waste was leached at 190 °C in 73 wt% KOH for 8 h.

Mar 1, 2017

By Lawrence L. Brown

As part of the Federal effort to help maintain an adequate supply of fertilizer materials, the Bureau of Mines conducted research to characterize complex low-grade Michigan phosphate materials and to devise methods for recovering fertilizer-grade phosphate concentrates. The rock is from middle Precambrian sedimentary formations in the Marquette Range located in the central part of the Upper Peninsula of Michigan. Occurrence of phosphate-bearing sediments in Precambrian rocks is rare. This deposit, containing 12 to 15 pct P2O5 is believed to be the richest Precambrian phosphate deposit in the United States. Petrographic examination showed that the conglomeritic rock contains crystalline apatite both in "black pebbles" and in quartz matrix. Attrition scrubbing and sizing tests showed that there is no tendency for phosphate to concentrate in any of the sized fractions. In beneficiation tests, which included grinding to minus 325 mesh followed by phosphate mineral flotation using a fatty acid-fuel oil collector, a phosphate concentrate was obtained that had a grade of 30 pet P2O5 and a P2O5 recovery of 72 pct. This concentrate should be suitable for fertilizer manufacture.

Jan 1, 1982

By Joel F. Flurnerfelt

Molten Al and Al alloys containing si, Mn, Ti, and y have been lanced with nitrogen-bearing gases. These lancing experiments provided the means for observing what phases form during exposure to nitrogen-bearing gases for finite periods of time, <2 minutes, at high temperatures, >1290oC. The experiments were conducted in sn induction heated drop tube furnace apparatus. The overall premise of these experiments was to select those Al alloys and gas compositions that show promise of forming secondary dispersoid phases, particularly AIN, in the Al matrix. The alloys selected will be atomized using gas atomization reaction synthesis (GARS) using the most favorable conditions. In this case, the chosen Al alloy will be atomized with a nitrogen-bearing gas, such that the Al and gaseous nitrogen species react to form a dispersoid phase within each powder particle. The powder particles that result from this "aggressive" GARS-process would be essentially Al metal-matrix composites within a uniform distribution of dispersoids. To date, only high-purity Al has been atomized using a mild GARS reaction. This work is funded by the Materials Science Division of DOE-BES under contract number W-7405-Eng-82.

Jan 1, 1996

By M. Huang

A conductivity-based sensor for on-line measurement of free acid was recently built. This sensor is suitable for high ionic strength solutions and its corrosion-free operation is based on induction currents. It has been tested against literature data and measurements made using a previous developed contact-type conductivity cell, with an average difference within 1%. The electrical conductivities of H2SO4?H2O, H2SO4?MgSO4?H2O and NaCl?Laterite-H2Osolutions at temperatures up to 250 °C were discussed. It was found that the solution conductivity depends on various factors, such as the electrolyte concentrations, the type of electrolytes, temperature and the amount of dispersions. A semi-empirical model was developed to account for all the factors discussed. This model was further tested on actual process solutions from the hydrometallurgy of nickel where sulphuric acid solutions containing a variety of metal sulphates and solids. The average difference between the estimated acid concentration from this model and the one from titration was generally less than 5%, which is excellent for industrial applications.

Jan 1, 2006

By Hector M. Henao

To provide thermodynamic data for converting nickel matte to liquid nickel at high temperature, an experimental study was conducted on the phase equilibrium between the Ni-S alloy and the FeOX-SiO2, FeOx-CaO, and CaO-A12O3 base slag in a magnesia crucible and the CaO-Al2O3-MgO slag in an alumina crucible. All experiments were carried out at 1773 K under controlled pso2 of 0.1 atm and po2 in a range between 5x10- and 10-5 atm by using CO-CO2-SO2 gas mixtures. The dissolution of nickel in the slag was found to be minimum for the CaO-Al203¬-MgO slag with a molar ratio of NCaO/NA1203=1.7. The solubility of nickel in this slag at p02 of 6x10 atm (just before the precipitation of solid NiO) was 4 mass%. This result suggests that a CaO-A12O3 base slag could be used in converting Ni-S melt to nickel while minimizing nickel losses to the slag.

Jan 1, 2002