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By Yasuhiro Konishi, Norizoh Saitoh

"We have developed new recycling technologies, based upon an eco-friendly biotechnology, in order to extract precious and rare metals sourced from post-consumer products. Recently we have been focusing on the metal ion-reducing bacteria, Shewanella algae and Shewanella oneidensis, which are able to reduce and deposit the precious metal ions (gold (III), platinum (IV), palladium (II), and rhodium (Ill)) into metal nanoparticles at room temperature within 120 min. When targeting the leachates from printed circuit boards, the Shewanella bacteria were able to allow selective reduction and deposition of gold (III) ions under acidic conditions in the presence of heavy metal ions, proposing a new bio-recovery system for gold. We also found that the Shewanella bacteria can separate and concentrate soluble rare metal ions (dysprosium (III), indium (Ill), and gallium (Ill)) from dilute solutions. Using this biomass adsorbent, the effectiveness of system for the novel recovery of indium from the leachate of used LCD (liquid crystal display) panels has been demonstrated.IntroductionMany high-tech manufacturing industries are highly dependent upon the use of critical raw materials that are the rare metals (e.g. rare earth elements/indium) and precious metals (e.g. gold/platinum group metals). There are now serious global concerns over the short term and long term availability of critical raw materials for high-tech manufacturing. This highlights the paramount importance of sustainable component reuse and material recycling technologies for recovery of critical raw materials. We believe that the most important domestic source of precious metals is through more recycling, and this will require more research and further development for the recycling of precious and rare metals. In general, chemical/thermal recycling is deemed to be the most appropriate means to extract the precious and rare metals from postconsumer products. However, there are issues related to the heavy use of toxic and hazardous chemicals, and the release of toxic emissions.Biological recovery methods provide an attractive alternative strategy and use microorganisms to separate and concentrate soluble precious and rare metals from dilute solutions into microbial cells via biosorption [1-3] and biomineralization [ 4, 5]. Biological systems generally operate at ambient temperature and near-neutral pH. Consequently, microbial recovery of metals would be an environmentally friendly method for recycling precious and rare metals from end-of-use products."

Jan 1, 2014

By M. E. Myers

An experimental program is being carried out to determine the thermodynamic characteristics of zinc solubilization in high-temperature iron and iron-carbon alloys. Two versions of an isopiestic technique are being used, with zinc at a lower temperature being equilibrated with pure iron foils or molten iron-carbon alloys at a higher one. The lower temperature sets the partial pressure of zinc vapor, and thus the activity relative to a given reference state. Initial results show Henrian behavior for dilute zinc solutions in austenite and a molten 4.6% C alloy, with unit-pressure solubilities in pure Fe that closely match the predictions of Wriedt.

Jan 1, 1992

By M. Tangstad, H. Mølnäs, J. D. Steenkamp

"Temperature affects several aspects of pyrometallurgical systems, including thermodynamics and reaction kinetics. Reliability of temperature measurements in laboratory and plant applications is thus important from process, safety and financial perspectives. This case study briefly introduces different techniques utilized for temperature validation, and demonstrates temperature validation on laboratory scale utilizing the wire-bridge method. Pt/Ptl3Rh thermocouple hot junctions were constructed by mechanically connecting thermocouple wires through a pure metal bridge consisting of copper, gold, nickel or palladium wire. When heating the wire-bridge thermocouple alongside a regular Pt/Ptl3Rh thermocouple, temperature offsets were quantified as the wirebridge thermocouple short-circuited at the melting points of the pure metals. At the melting points of gold (1064°C) and palladium (1555°C), average measured temperature offsets were -2.1°C ± 2.3°C and 0.2°C ± 0.4°C, respectively. Results from the copper and nickel wire-bridges were inconclusive. The paper concludes with a discussion on the potential industrial applications of the technique.IntroductionThermocouples are probably the simplest of all temperature sensors, but are widely utilized due to simplicity, versatility and ability to handle a variety of experimental conditions and industrial applications. Additionally, thermocouples are often the only option in research laboratories requiring high temperature measurements, and a high level of reliability is usually required from thermodynamic, kinetic as well as safety points of view.The study presented here originated from a test program where the compatibility between different types of carbon-based refractory materials and industrial slag produced in silicomanganese furnaces were investigated on a laboratory scale utilizing the static crucible test[l]. Due to the nature of the silicomanganese production process, the compatibility tests were to be conducted at 1600CC[2]. Details of the experimental set-up utilized for the compatibility tests are discussed in the Experimental Set-up and Method Statement section later in this paper."

Jan 1, 2012

By Jorge A. S. Tenorio, Chuanwei Zhuo, Joner O. Alves, Yiannis A. Levendis

"The disposal of wastes is a serious environmental problem, since available landfill space is dwindling. Their treatment by pyrolysis or combustion has merit, and the corresponding fuel or power production is of technological interest. However, such processes need a rigid control of emissions. This work addresses the gaseous light hydrocarbons (LHCs) generated during sequential pyrolysis and partial oxidation of unserviceable tires, PET bottles, com wastes (DDGS) and sugarcane bagasse in a two-stage laminar-flow horizontal furnace, kept at 1000 °C. Gas chromatography was used to identify and quantify the components of the emitted gaseous light hydrocarbons. The results showed that the biomass residues generated the highest emissions of aliphatic hydrocarbons, whereas PET generated the most aromatic hydrocarbons. When stainless steel meshes were inserted in the exhaust flow, it was found that hydrocarbon emissions were curtailed; as such meshes catalyzed partial conversion of these carbon-bearing gases to carbonaceous nanomaterials.IntroductionLight hydrocarbons (LHCs) are volatile organic compounds, consisting of hydrogen and carbon with low molecular weight; the most common species are methane, ethane, propane, butane, etc. LHCs are valuable since they are a very important energy resource. However, uncontrolled release of light hydrocarbon gases to the atmosphere should be avoided [l, 2]. In this work, a development is presented for the evaluation of LHCs generated during the controlled pyrolysis/combustion of several wastes in a two-stage laminar-flow horizontal furnace. Samples of unserviceable tires, post-consumer PET bottles and waste residues from the bioethanol industry (DDGS and sugarcane bagasse) were burned. A catalyst system, consisting of stainless steel screens, was tested for its effects on the gaseous emissions."

Jan 1, 2011

By Antoine Allanore, Guillaume Lambotte, Bradley R. Nakanishi

Current industrial methods used for rare earth element (REE) extraction involve: 1) ore enrichment, 2) separation of rare earth oxides (REOs), 3) chlorination or hydrofluorination, and 4) individual electrowinning of REEs from a molten halide electrolyte. The complexity of REE extraction is inherited from their electronic configuration. Recently, molten oxide electrolysis (MOE) has been used to produce reactive metals directly from their oxides, e.g. titanium. As a single-step alternative to processes 3) and 4), or laboratory has investigated rare earth extraction by MOE. A key challenge is to find a molten electrolyte more stable than REOs. One possibility is to use binaries of REOs directly as a solvent. We have, therefore, developed two experimental approaches for studying molten REOs at temperatures exceeding 2200oC. The present work reports the most recent experimental results obtained with La2O3-Y2O3. Those promising results demonstrate potential for operating with molten REOs and refine the underlying materials challenge for electrodes to enable metal recovery.

Jan 1, 2015

By C. P. Broadbent

The process metallurgy of many nickel laterite smelting operations is controlled largely by the physical chemistry of the slag system. Consequently, accurate phase diagram information and physicochemical property data are essential to interpret and predict the behaviour and optimisation of the overall process. The system (SiO2 - MgO - FeO) first described by Bowen et al. between 1914 and 1935 and the system (SiO2 - MgO - FeO - Fe2O3) determined by Muan and Osborne in 1956 are of particular relevance to the study of nickel laterite smelting slags as these systems form a reasonable approximation of many industrial slags. This paper will review the literature for these (and other relevant) phase systems. In addition data available from the ternary and (quasi)ternary phase diagrams will be compared with data obtained from industrial slags. The physico-chemical properties under consideration will include; melting and crystallisation behaviour (solidus and liquidus temperatures), viscosity - temperature relationships, heat flux considerations, electrical conductivity, surface and interfacial tension.

Jan 1, 1993

By Metehan Erdogan, Orhan Gökçe Göksu, Ishak Karakaya

"An experiment (mixture) design was created to optimize the process parameters of the electrochemical reduction of CaW04 to W in molten CaCl2-NaCl eutectic mixture. Temperature, applied voltage and the length of Kanthal wire winding of the CaW04 pellets were selected as the process parameters that were allowed to vary between the predetermined minimum and maximum values. The rates of the electrochemical reductions were interpreted from the variations of current and total charge vs. time graphs under different conditions. The analysis pointed out that 640°C and 2.81 V resulted in the fastest reduction. Itwas seen that the effect of Kanthal wire winding on the output current was less pronounced when compared to the other two parameters.IntroductionFFC Cambridge Process [1] has been applied to a number of metal oxides in laboratory experiments to produce metals. In nearly all of these studies, the electrolysis temperature was around 900°C, the electrolyte was pure CaCl2 or CaCl2 containing salt solutions and the anode was graphite. However, it was recently shown that the electrochemical reduction process of metal oxides in CaCl2 containing electrolytes at the mentioned high temperatures was not suitable for tungsten production [2], It was reported that as soon as WO3 contacts CaCl2, the following reaction occurs:"

Jan 1, 2012

By C. T. Philipp

Recycling of waste is much preferred over disposal. This paper discusses the Enviroscience, Inc. (ESI) process, now being commercialized by MetWool, Inc., to recycle hazardous wastes using an extractive metallurgical process which is followed by vitrification of non-reducible metal oxides. In this process, volatile and reducible metals are reclaimed as their respective oxides and elements.

Jan 1, 1995

By H. Y. Sohn

The purpose of this article is to analyze critically and quantitatively the effect of chemical equilibrium on the overall rates of fluid-solid reactions. It is shown through a mathematical analysis that a reaction with a small equilibrium constant (a positive standard free energy of reaction) is more likely to be rate-controlled by pore diffusion or mass transfer than a reaction with a large equilibrium constant. The overall reaction rate of the former also tends to be slow. Furthermore, the apparent activation energy of such a reaction approaches the standard enthalpy of reaction (Mf'), rather than the true activation energy of the chemical reaction. The Law of Additive Reaction Times developed by the author is shown to apply to equilibrium-limited fluid-solid reactions and to be useful in quantitatively analyzing the behavior of such reactions.

Jan 1, 2003

By H. Y. Sohn

The purpose of this article is to analyze critically and quantitatively the effect of chemical equilibrium on the overall rates of fluid-solid reactions. It is shown through a mathematical analysis that a reaction with a small equilibrium constant (a positive standard free energy of reaction) is more likely to be rate-controlled by pore diffusion or mass transfer than a reaction with a large equilibrium constant. The overall reaction rate of the former also tends to be slow. Furthermore, the apparent activation energy of such a reaction approaches the standard enthalpy of reaction (M-f'), rather than the true activation energy of the chemical reaction. The Law of Additive Reaction Times developed by the author is shown to apply to equilibrium-limited fluid-solid reactions and to be useful in quantitatively analyzing the behavior of such reactions.

Jan 1, 2003

By Leiv Kolbeinsen, Vincent Canaguier, Ingeborg-Helene Svenum

The syntheses of stoichiometric iron chromite and chromites with chosen impurity content have been developed using the induction skull melting technique. The aim for this synthetic material is to obtain pure samples to study the carburization by methane-hydrogen gas mixtures. For each synthesis, the parameters influencing the skull melting experiment have been considered. The product phases have been analyzed using X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Energy-Dispersive X-ray Spectroscopy (EDS) and X-ray Photoelectron Spectroscopy (XPS). The synthetic material was subsequently pelletized and sintered in argon. The use of excess iron was found to improve the quality of the final product as well as to help the melting. The difference in magnesium content between first and last solids formed seem to indicate a segregation phenomenon, while no evidence could support a similar trend for aluminum substitution in chromite.

Mar 1, 2017

By C. Kathryn Sole

The close proximity of cobalt and nickel on the Periodic Table and their frequent occurrence together in nature means that their separation in primary hydrometallurgical flowsheets is not only often necessary, but requires the use of innovative chemistry to achieve high selectivity. Today, increasingly stringent demands for the high-purity cobalt and nickel salts required for battery applications in consumer electronics, electric vehicles, and solar applications are again challenging the state of the art. The evolution of cobalt–nickel separations is traced from the basic precipitation technologies employed in 1960s, through commissioning of the first cobalt solvent-extraction plant in South Africa in 1974, to the commercialisation of organophosphinic-acid extractants (which provided a step-change improvement in selectivity) and their eventual widespread use in the 1980s and ’90s. This was followed later by their sulphur analogue, which enabled different possibilities for laterite processing in the new millennium. Separations in chloride media, which take advantage of the different speciation chemistries, and nickel extraction by oximes in ammoniacal systems are also discussed. More recently, chelating and solvent-impregnated resins have added further dimensions to the possibilities for flowsheet design and enabled higher purity products to be attained from both primary and secondary sources. Selected case studies and flowsheets are described.

By E. Dendy Sloan

An overview of hydrate properties is given, with emphasis on unusual deviations from ice, the most common solid water form. Reliable sample preparation and reproduction of in situ hydrates provide the foundation for all hydrate science and engineering. Relations are given to connect the three domains in the title: (1) micro-scopic properties measured with Raman, NMR, and diffraction spectroscopy, (2) meso-scopic properties measured with single crystals, and (3) macro-scopic properties measured with pressures, temperatures, volumes, etc. A principal illustration relates micro-scopic and macro-scopic domains. Experiments provides the basis for improving statistical thermodynamics model for these compounds. To date, this model is one of the most commonly used industrial statistical thermodynamics applications, based upon the classical model of van der Waals and Platteeuw (1959). Microscopic measurements and simulations indicate model assumption improvements, resulting in the next generation of the statistical thermodynamics for improved macroscopic property prediction.

Jan 1, 2002

By T. Wang, R. G. Reddy

"A new eutectic of LiNO3-NaNO3-KNO3 ternary system was calculated by using thermodynamic modeling and the eutectic temperature was predicted to be 389.15K. The melting point was determined using Differential Scanning Calorimetry (DSC). On repeated measurements, it was found that the melting point of the eutectic composition showed excellent reproducibility with the predicted value. The heat capacity was also measured using DSC and the data as function of temperature were fit to polynomial functions. Subsequently, the thermodynamic properties such as enthalpy, entropy and Gibbs energies of this novel ternary eutectic salt mixture were deduced as function of temperature.IntroductionIn these days, the provision of the large amount of energy required in the peak period relies more and more on the parabolic trough solar power plant and it works by utilizing the thermal transfer fluid. Consequently, the development of inoovative thermal transfer fluid with higher energy storage density is paramount to lower the expense for generating energy [1-4]."

Jan 1, 2013

By Qian Li, Honggui Han, Jun Wang, Shichao Yu, Chunxiao Zhao, Maoxing Hong, Rui Liao, Xingxing Wang

In this study, bioleaching experiments, synchrotron X-ray Diffraction (SR-XRD), X-ray absorption near edge structure (XANES) and X-ray Photoelectron Spectroscopy (XPS) were conducted to investigate the intermediates and surface species of bornite leached by mesophilic mixed bacteria of Leptospirillum ferriphilum, Acidithiobacillus caldus and Sulfobacillus thermosulfidooxidans. CuS, Cu9Fe9S16 and S8 were the main intermediate species during bornite bioleaching by mesophilic mixed bacteria, and CuFeS2 was also detected. The surface species of S2− and S2 2− would be polymerized to Sn 2− during bioleaching. The formation of element sulfur and the increase of its content were confirmed by the fitted results of XPS spectra. The presence of polysulfide and element sulfur did not inhibit the bornite bioleaching. The formations of CuS and CuFeS2 were confirmed by the results of Cu K-edge XANES spectra.

Mar 1, 2018

By Rollie E. Dutton, David A. Stubbs

"A sensor has been developed and tested that is capable of emitting and receiving ultrasonic energy at temperatures exceeding 900°C and pressures above 150 MPa. The sensor works with standard ultrasonic pulser-receivers and has demonstrated the capability of measuring workpiece deformation during hot isostatic pressing (HIP). Details of the sensor design, performance, and coupling of the ultrasound to the workpiece are described. Ultrasonic data acquired by the sensor, in situ, during HIP runs and at elevated temperatures in air are presented.INTRODUCTIONHigh temperature structural components, such as structural castings for jet engines, nickel-base superalloy turbine blades, and ceramic and metal matrix composites made from powders are often densified by hot isostatic pressing (HIP). For powder consolidification, the HIP process involves sealing the powder (and reinforcing fibers for composites) within an evacuated ""Can"" made of a material that softens at high temperatures. A hydrostatic pressure is then applied by pressurizing the inside of the HIP vessel with argon gas (up to 140 MPa). The hydrostatic pressure densities the powder through the elimination of the porosity between the powder particles.This paper presents details of the development and preliminary testing of an ultrasonic displacement sensor that can be used to monitor materials processing, in situ, at temperatures and pressures significantly higher than current ultrasonic displacement sensors. The target processing environment for this sensor is that typically found in a hot isostatic pressure (HIP) vessel, i.e., temperatures exceeding 1000°C and pressures above 138 MP a."

Jan 1, 1997

By Shengli Wu, Mingyin Kou, Laixin Wang, Xinliang Liu, Zhennan Qi, Yujue Wang

Softening and melting experiments were conducted on four kinds of imported lump ores named A-D, under different temperature intervals within the self-developed visualization high temperature furnace. By calculating the reduction and shrinking degree under different intervals, softening and melting indexes were determined. These ores all expanded firstly followed by shrinkage with the temperature increasing. The difference of lump ore’s own characteristic led to different softening and melting behavior. The results showed that the looser the structure was, the better the reducibility will be. The compact structure and good reducibility led to high expansion rate. The beginning softening temperature declined and the ending softening temperature increased because of high porosity, which resulted in wide softening temperature interval. The charging ratio of lump ore A should be improved. Lump ore B should be distributed in the center of the blast furnace. Lump ores C and D should be used less.

Jan 1, 2016

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 L. Evrard, S. Brouwer, E. Bosly, E. Boydens

"A partial desulfurization roasting process has been tested on a typical copper-zinc sulfide concentrate in a Nichols Herreshoff monohearth pilot furnace whereby the su!fµr is partially removed and iron is to a certain degree preferentially oxidized. The phase changes that occur in the particles during selective roasting at 650°C and 800°C over a range of residence times were investigated by the use of chemical analysis, optical microscopy, X-ray diffraction and electron microprobe analyses. The purpose of this work was to get an insight into the mineral assemblages formed by controlled oxidation roasting and to evaluate if this non traditional approach could be afterwards used to recover zinc, copper and iron by a physical separation method. IntroductionThere has been considerable interest over the years in improving extraction and processing procedures for recovering non ferrous metals especially from polymetallic ores containing copper, lead, zinc and iron sulfides with very fine intergrown phases. Complex sulfide ores, which represent considerable reserves and resources in copper, lead and zinc, as well as precious metals and sulfur, are difficult to treat by conventional physical processes, leading to impure concentrates at low metal recovery. Some methods that can be used to treat such ores were described by G. Barbery (1). Various metallurgical routes generally combining pyro- and hydrometallurgical methods have been explored to develop new processes to recover the metals from zinc-bearing sulfidic ores and concentrates (2, 3, 4). The feasibility of partitioning complex sulfide minerals to simpler phases in order to improve selective extraction of mineral constituents has also been investigated (5)."

Jan 1, 1999

By E. Fregeau-Wu

The major obstacle in recycling steelmaking slags to the blast furnace is their phosphorus content. Removal of the phosphorus, which is primarily associated with the silicate and phosphate phases, would allow for greater recycle of these slags for their iron, manganese, and lime contents. Calculations show that separation of the silicates from the oxide phases would remove nearly 90% of the phosphorus from the slag. The variable grain size of the as-received slag made liberation by fine grinding difficult. Therefore, slow-cooling experiments were undertaken to improve the grain size distribution. The grain size distributions were determined using in-situ image analysis. The samples were ground to their apparent liberation size and high gradient magnetic separation was used to separate the magnetic oxides from the nonmagnetic silicates and phosphates. Liberation analysis and modeling was performed on selected separation products for discussion of benefication characteristics.

Jan 1, 1995