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By Guangqing Zhang

The paper presents results of a systematic study of synthesis of titanium oxycarbide and its chlorination. Titanium oxycarbide was produced by carbothermal reduction of titania in hydrogen, argon and helium. Formation of titanium oxycarbide started at 1200°C in all gases. The reduction was the fastest in hydrogen. Formation of titanium oxycarbide in hydrogen was close to completion in 120 min at 1300°C, 60 min at 1400°C and less than 30 min at 1500°C. Reduction in argon and helium progressed at a similar rate and reached 90-95% after 300 min at 1400-1500°C. The chlorination of titanium oxycarbide was ignited at 150-200°C. Chlorine partial pressure and gas flow rate strongly affected the chlorination rate. Chlorination of titanium oxycarbide produced with carbon to titania molar ratio 2.5 at 235-400°C was close to 100% in 30 min.

Jan 1, 2009

By Yoichi Takeda

The CaO-FeO,-Cu20 slag has been practically applied to continuous converting of copper, and also has potential for refining of copper. Liquidus lines of the slag system and phase stability diagram for the liquid slag and the existing solid compounds under copper saturation are presented. Liquidus composition was determined by chemical analysis of slag sample saturated primary solid. The temperatures of invariant equilibria were investigated by thermal analyses. Oxygen potentials on the liquidus lines, the univariant and invariant equilibria were estimated from the relation slag composition and oxygen potential that relation was confirmed in separate experiments.

Jan 1, 2003

By Christophe Thiébaut

Keywords: Pyrochemistry, Salts Treatment, Distillation The pyrochemical purification of metal generates spent salts. When this metal is an actinide such as plutonium, the slags cannot be discarded and are thus disposed in nuclear facility. In order to handle with these slags, the decision has been taken to reduce stored quantities. The development of a pyrochemical treatment is in progress in the CEA Valduc centre. The feed salt, typically composed of various Pu and Am species contained into monovalent or divalent chloride matrix, is first oxidized to convert the actinides into oxides. Then the chlorides are separated from the actinide oxides by vacuum distillation. Temperatures higher than 750°C for monochloride salts mixture NaCl/KCl and higher than 1100°C for divalent CaCl2 base salts, are required to produce an industrial flow of vaporization. Inactive qualification of the process for NaCl/KCl base salt has been carried out with lanthanide surrogates. Then, a pilot equipment, called distillator has been designed and built for production-scale distillation of NaCl/KCl and CaCl2 oxidized plutonium salts. Industrial flows of vaporization have been obtained with this pilot equipment : about 4 g/cm²/h for NaCl/KCl at 800?900°C and 1 Pa, and more than 1,5 g/cm²/h for CaCl2 base salts between 1000?1200°C at 0.1 Pa. The last step, now in progress, is the integration of the distillator into a glove box.

Jan 1, 2005

By A. J. Rigby

Refractory linings in converters or anode furnaces used to over-oxidize the blister copper will suffer rapid deterioration, due to prolonged contact with copper oxide-rich slag. Nitrogen stirring with COP KIN porous plugs and use of SEMTECH OPC in converters and anode refining vessels can considerably reduce both refractory wear and processing times. In addition, careful control of the vessel atmosphere and the use of real-time optical process control minimize both slag volume and contact time with the vessel refractory.

Jan 1, 2005

By Y. K. Rao

Relatively pure crystalline lead sulfate (PbSO4) can be produced by chemical vapor transport from an impure source such as the lead-acid battery paste or the roast-ore-leach-residue from a hy¬drometallurgical process-route. In a closed-reactor, transport of matter is induced by a tempera¬ture-gradient and the steady-state transfer rate can be calculated using the data on the standard free energies of formation for the species present and the pertinent binary diffusion coefficients. The present work focusses on chemical vapor transport in a tubular reactor (1.4-cm inner diameter x 10-cm long) with the source- and deposition-ends held at 850°C (T,) and 750°C (Td), respectively; PbC12(g) is the 'solvent' or 'transport agent' and NiSO4(s) placed in the source-zone -serves to maintain a sufficiently high S0,-potential such that the stability of the lead sulfate species is ensured. For the purposes of analysis, the gas-phase in the reactor is assumed to consist of eight species: H2O, PbC12, SO3, SO2. O2 HO, C12, and PbC14. The reaction between C12(g) and PbSO4(s) in the high-temperature source-zone produces PbCl2, SO2, and 02; four more reaction-equilibria in the same zone yield other species. In the low-temperature deposition-zone, reaction equilibrium involving PbC12, H2O, and SO, leads to the nucleation and growth of PbSO4 crystals; three other reaction-equilibria occur in this zone. By employing the virtual equilibrium state for the end-zones and coupling it to the Stefan-Maxwell diffusion equations for each of the gas species, the respective partial pressures for these, in the source- and deposition-zones, are computed at steady-state. From these data, the molar fluxes of PbCl2. PbCl4, and so forth, are determined. Allowing for the transport-enhancing effects of thermal convection, the net transport rate of lead (or PbSO4) is duly calculated for specified initial conditions. The predicted rates show very good agreement with measured rate data reported in the literature [ V. Plies, T. Kohlmann and R. Gruehn: Z. anorg. allg. Chem, 568, 62 (1989)

Jan 1, 1995

By Wen-Ming Chien

Keywords: AN-KN Phase Transition, Lattice Parameters of AN-KN, X-ray Diffraction The lattice parameters of the low and high temperature phase of KNO3-rich (in NH4NO3) solid solutions have been determined by the X-ray diffraction method. The low temperature single KNO3 phase (KN II) are from 92%-100% KNO3 in NH4NO3 composition range and from room temperature to 393 K showing in X-ray diffraction patterns. The high temperature KNO3 phase (KN I) showed very broad composition range between 20% to 100% KNO3. The lattice parameters of KNO3-rich (KN II and KN I) solid solutions have been calculated at different temperature range. The volumes of orthorhombic KN II phase decrease from 0.3208(3) to 0.3195(3) nm³ at the room temperature as the compositions increase from 95% to 100% KNO3. The lattice constants of the hexagonal KN I phase show that there is no significant change in a-direction when the temperature increases. Details X-ray results and lattice expansion equations during heating will be presented.

Jan 1, 2005

By Yavuz Ali Topkaya

Rare earth ferrosilicide is a versatile alloy mainly used to control the detrimental effects of sulfur in steel and to modify graphite structures in cast iron. The aim of this study was to determine the optimum conditions to make rare earth ferrosilicon alloy using a preconcentrate produced from a bastnasite type of ore present in the Beylikahir-Eskisehir region of Turkey. This concentrate contained 23.5%REO, 41.37% CaF2, 10.69% BaSO4, 8.50% CaCO3, 4.18%Fe2O3, 2.83% Al2O3, 2.74% SiO2, 1.20% P2O5 and small amount of other oxides. The initial metallothermic reduction of this concentrate using ferrosilicon and aluminum in a graphite crucible placed in a muffle furnace gave very low recoveries due to the difficulties encountered in adjusting the slag composition, temperature and amount of additives. Therefore, two batches of rare earth oxide concentrate containing 61.1% and 81.7% cerium oxide, respectively, that were procured from a Turkish glass producer, were used to optimize with respect to temperature, duration, slag-making additives and amount of reducers. In these experiments, smelting and reduction was done in an induction furnace with graphite crucible, and, ferrosilicon and aluminum were added after melting the charge. As a result, there was no difficulty in obtaining a rare earth ferrosilicon alloy containing 35-55% RE, 5-25% Fe and 20-40% Si, with about 80% metal recovery. When the optimum conditions were applied to the preconcentrate, alloys of similar compositions were obtained with 70-80% recovery. Experiments were also done with mixtures of preconcentrate and rich concentrate, and, recoveries as high as 95% were obtained. Only in this case, to increase the recovery, mixtures had to be charged to the empty graphite crucible after heating the crucible to the required temperature.

Jan 1, 2006

By A. P. I. Popoola, D. O. Okanigbe, A. A. Adeleke

In view of the steady depletion of primary sources of copper and the increased global demand for refined copper, it becomes necessary to explore some secondary sources for possible extraction of copper. The waste copper smelter dust (CSD) is a rich secondary resource for copper as shown by the chemical composition of the South African Palabora coppers smelter plant CSD that assayed 18.02, 13.36, and 3.4 wt% copper, iron and sulphur, respectively. Studies on CSD have focused majorly on either dust characterization or treatment, while hydrometallurgical extraction without pretreatment and with pretreatment using techniques such as oxidative roasting are also considered quite attractive. The challenge of iron dissolution during the leaching stage in these processes necessitates adequate purification of the leach liquor before the extraction of the metal as nano-particles. Hence, this review examined the theories relating to the characterization and treatment of CSD for copper recovery as nanoparticles; with factors having a bearing on the treatment process such as kinetics considered with the aim of providing scientific basis for the research.

Mar 1, 2017

By Hong Yong Sohn

Keywords: Barium sulfate, Barium sulfide, Environment, Kinetics, Pollutants, Sulfur dioxide conversion, Thermodynamics Nonferrous smelters and coal gasification processes generate sulfur dioxide streams, most of which are treated to produce sulfuric acid with the accompanying problems of market shortage and transportation difficulties. While the conversion of sulfur dioxide to elemental sulfur has many environmental advantages, no processes exist that are environmentally acceptable and economically viable. A method for converting sulfur dioxide to elemental sulfur by a cyclic process involving calcium or barium sulfide and calcium or barium sulfate without generating solid wastes has been developed. In this process, the sulfate, as the starting raw material, is reduced by a suitable reducing agent such as hydrogen to produce the sulfide, which is used to reduce sulfur dioxide producing elemental sulfur vapor and regenerating the sulfate. The latter is then reduced to reproduce the sulfide. This paper describes work on the BaS/BaSO4 system. Thermodynamic analysis and experimental results indicated that the BaS-SO2 reaction produces mainly sulfur vapor and solid barium sulfate and that the gaseous product from the BaSO4-H2 reaction is mainly water vapor. The rates of the two reactions are reasonably rapid in the temperature range 700-1050°C.

Jan 1, 2005

By Thomas Weyand, Thomas Claridge, Dale Nickels

"This paper addresses the initial results of a project to evaluate the suitability of copper mining tailings as raw material for the production of structural products using PMET’s patented technology. Preliminary testing indicated that high performance structural products were possible using these materials. A demonstration scale project produced approximately 1,500 bricks in various colors. These products fall under under ASTM C- 73 and were found to present properties suitable for severe weather applications. Although the products in this project were of typical brick dimensions, other products are possible, for example concrete block substitutes or pavers. These products from the PMET process are commercially known as Brixx. This paper will provide operational details of the production process, mineralogy and mechanical properties of the products.INTRODUCTIONPMET has developed process technology that can convert various siliceous waste materials into competent structural products. This technology is the subject of US patent # 6,068,803. In general, the process consists of mixing lime, water and the major feed stock, pressing to form a “green” shape, and curing the product in an autoclave for 6 hours with saturated steam at ~200oC. The curing process forms Tobermorite, which acts as a crystalline binder. Freeport-McMoRan approached PMET to see whether mine tailings from the Sierrita mine, containing significant amounts of clay, might be a suitable feed material for the production of structural products. “Brixx” is the commercial term used to describe the resultant structural product formed in the test work. This paper is a preliminary evaluation of a technology that is being considered by Freeport-McMoRan. This report is not an endorsement by Freeport-McMoRan of the process or products, nor is it a commitment to use this technology."

Jan 1, 2008

By Warren J. Bruckard, Mark I. Pownceby, Sazzad Ahmad, M. Akbar Rhamdhani

Rutile is the preferred feedstock for producing high-grade TiO2 pigment but due to decreasing resources, alternative materials such as ilmenite is now used to produce a synthetic rutile (SR) feedstock. This requires removal of impurities (e.g. Fe, Mg, Mn) which, for a primary ilmenite is straightforward process. Processing of weathered ilmenite however, is complex, especially when chrome-bearing impurities are present since minor chromium downgrades the SR market value as it imparts color to the final TiO2 pigment, Chrome-bearing spinels are a problem in weathered ilmenites from the Murray Basin, Australia as their physical and chemical properties overlap with ilmenite making separation difficult. In this paper, different sulfidation process routes for weathered ilmenites are analyzed for their applicability to Murray Basin deposits as a mean of remove chrome spinel impurities. Thermodynamic and experimental studies indicated that selective sulfidation of chrome-bearing spinel can be achieved under controlled pO2 and pS2 processing conditions thereby making them amenable to separation.

Jan 1, 2015

By Fang Wu

The paper designs an extraction flow for the total recovery of nickel and cobalt and removing magnesium simultaneously from the cadthodic materials of the spent hydrogen-nickel and cadmium-nickel batteries. The separation of Co, Ni and Mg though P507 extraction .The extraction equilibrium pH is 4.5~5.0, ßNi/Co is 140~180, and ß Ni/Mg is 20~25; nickel and magnesium are scrubbed in two steps, in which the equilibrium pH of nickel and magnesium scrubbing is controlled at 5.0±0.1 and 4.4±0.1 respectively. The stepwise scrubbing technique is adopted to remove 94.5% of magnesium and to recover 99.45% of nickel and 95.35% of cobalt. During the integrated extraction and precipitation process the total recovery fraction of nickel and cobalt are 99.99% and 99.95%, and the recovery fraction of magnesium is 94.02%.The recovered NiSO4 and CoSO4 solution are enriched and crystallized.

Jan 1, 2009

Sm-Co alloy is a kind of magnetic material with high power and has been applied in modern industry widely. In this study, the wet chemical co-precipitation was developed for synthesis of the Sm-Co alloy oxide precursor. The thermodynamic analysis of the studied system was done to clarify the solution behavior theoretically based on the thermodynamic equilibrium and simultaneous equilibrium. Then, the experiments were done to address the various effects on the wet chemical process, including solution pH, reactant concentration, dispersant, reaction temperature and time, etc. It is found that by precise control of the process, the Sm-Co alloy oxide precursor was synthesized with fine crystallization and special size & size distribution.

Jan 1, 2005

By Li Chen

A new process, i.e. Ball milling--Neural leaching--Oxidation calcinations--Chloridizing distillation--Hydrolysis, was designed to recover germanium from the vacuum furnace slag produced in Shaoguan smelter. The suitable process and operational parameters were determined for the practical production.

Jan 1, 2005

By M. A. Barakat

"Adsorption of heavy metal ions specifically, Cu(II), Zn(II), Mn(II), and Cr(VI) from aqueous solution on synthetic 4A Zeolite was evaluated. The 4A zeolite was synthesized previously by dehydroxylation of low grade Kalabsha Kaolin at 800 °C, and reacted hydrothermally with 2-4 M NaOH solution at 100 °C for 2h. The adsorption capacity of the metal ions were found to be strongly dependent on pH and initial metal ion concentration. At the optimium conditions the adsorption capacity decreased in the order Cu(II) > Zn(II) > Mn(II) > Cr(VI) ions. Almost complete adsorption was achieved for both of Cu(II) and Zn(II) ions at pH > 6, while the adsorption capacity for both Mn(II) and Cr(VI) was 96, and 55.3 % at pH 11 and pH 3, respectively. The results also showed that the grain size of the 4A zeolite has a little effect on the adsorption capacity. The experimental data was compared with two adsorption isotherms, Langmuir and Freundlich isotheroms. The results showed a good agreement of the Langmuir plots with the experimental data.1. IntroductionSeveral industrial wastewater streams may contain heavy metals such as Cr, Cu, Pb, Zn, Co, Ni, Mn, etc. including the waste liquids generated by metal finishing or the mineral processing industries. Heavy metals are considered hazardous pollutants due to their toxicity, even at low concentration, and nonbiodegradability. Increasing level of heavy metals in natural water bodies poses a serious threat to all living species including humans. It is, therefore, essential to reduce the heavy metal concentration in effluents/wastewater before it is discharged into the water bodies [1]."

Jan 1, 2008

By Zhigang Liang

Investigation into the mixing of 150t ladle furnace by two-nozzle jetting was performed by a water model simulation of 1:4. The effects of nozzle arrangements including separation angle, radial position and asymmetry as well as tracer adding position on the mixing time were studied. The most favorable mixing is achieved when the two nozzles are symmetrically arranged at half radii in the ladle, with 45o separation angle. The empirical relationship between the mixing time and stirring power intensity has been established for two-nozzle jetting based on the present experimental results. In addition, the swelling above bath surface is also investigated with two-nozzle jetting.

Jan 1, 2009

By Junji Shibata

Keywords: Synergistic effect, Solvent extraction, Nickel ion, extractant mixture Waste solution from the Ni non-electric plating process contains 4.0 kg/m3 Ni (II), 0.1 kg/m3 Fe (III), 0.01 kg/m3 Zn (II), 48 kg/m3 SO42-, 98 kg/m3 HPO32- and 31 kg/m3 lactic acid as a typical composition. Solvent extraction, cementation, ion exchange resin and precipitation methods may be used for the treatment of this kind of solution. In this study, solvent extraction of Ni (II) is investigated by using two kinds of extractants in order to clarify the relationship between extraction equilibrium (static synergistic effect) and extraction rate (dynamic synergistic effect) for several extractant mixtures. The static synergistic effect does not take place significantly for the extractant mixtures of acidic extractants and neutral organphosphorous compounds, while a large static synergistic effect is confirmed when the extractant mixtures of acidic extractants and nitrogen-containing compounds are used. Nickel ions can be extracted in the wide pH range of 3.0-8.0 without any pH adjustment by using the several extractant mixtures. At the same time, the extraction rate remarkably increases by using the extractant mixtures of acidic extractants and nitrogen-containing compounds.

Jan 1, 2005

By Z. Sun

Magnetic fields have been used for inclusions removal from melt and preparation of materials with gradient compositions. Fundamental in these applications is that the induced magnetic forces on the particles/melt can enhance migration and change the interaction behavior. In the present paper, migration and interaction behavior of electrical-insulating particles in a conductive melt under strong magnetic field are theoretically analyzed. It is found that the migration can be considerably enhanced for micrometer sized particles by applying a strong magnetic field. In addition, two forces are involved in the interaction between two particles: the interparticle magnetic dipole-dipole attractive force due to magnetization and the repulsive force induced by flow of the melt. This theoretical analysis renders a better understanding of recent experimental results. Additionally, a new method by using strong magnetic field can be proposed to control the particle size distribution for the preparation of metal-matrix composites.

Jan 1, 2009

By Jin Qiu

Experiments were performed to determine the extent of minor element elimination that occurred when mixtures of copper smelter dust and copper concentrate, were calcined under vacuum. Almost complete removal of the As, Sb, Bi and Pb occurred due to the conversion of the minor element compounds of these elements into their highly volatile sulphides by reaction with sulphur from the concentrate. Heat and mass balance calculations of the slag-blow in a copper converter found that ~30 tonnes of the vacuum calcine could be used to produce 100 tonnes of copper as white metal. The use of dirty concentrate as the sulphidizing agent in the vacuum calcination means that the minor element treatment capacity of the smelter complex could be increased by 60 %. Also the productivity of the converters may be increased by up to 8 % due to the supply of copper values and oxygen in the calcined mixture.

Jan 1, 2005

By Ryo Sasai, Takeshi Itakura, Haruki Imaizumi, Hideaki Itoh

"Emission of industrial wastewater containing harmful oxoanions is one of the serious problems on account of its toxicity and the environmental pollution, especially caused by boric, phosphinic, arsenic and antimonic species. In this study, we developed a novel treatment technique of such polluted-water by hydrothermal mineralization. The treatment is “Geomimetic” method for precipitating oxoanions in aqueous media as natural ore resources by using hydrothermal treatment with calcium salts mineralizer. The treatment made it possible not only to detoxify the polluted-water, but also to recover the calcium minerals such as Ca2B2O5·H2O, Ca5(AsO4)3(OH), etc. Concentration of each ion in treated-water was lower than that of effluent standard in Japan. Moreover, the residual concentration of each ion was independent of the initial concentration, but it depends only on the solubility of the formed mineral under hydrothermal condition. Therefore, the hydrothermal treatment could be recommended as one of the treatment techniques of polluted-water.IntroductionVarious oxoanions such as boron and arsenic oxo-anions have high toxicity against human health and the environment. They are important resources, however, for plating or advanced material manufacturing industries[1-3], from which the wastewater containing these oxoanions is generated every day. An appropriate treatment is often required for industrial wastewaters to attain national effluent standards of Japan (NESJ, B: 10 mg/dm3, As: 0.1 mg/dm3). On the other hand, there is no production of arsenic and boric resources in Japan, and they are expected to be recycled. Therefore, the establishment of a system for the removal and recycling of arsenic and boron from wastewaters is of global significance.Several methods to remove them from aqueous media have been already reported by using adsorption[4], electro-coagulation[5], membrane separation[6-8] and biological techniques[9]. However, these methods have the following problems because of their stability in water. (1) Removal yield is low, especially for tri-valent arsenite ion (AsIIIO3 3-) and borate ion. (2) The applicable concentration range is narrow. In addition, the used adsorbents or collected residues after treatments are sill hazardous wastes, so that they must be treated by a proper method. But, it is very difficult to convert them to recyclable resources at most industrial plants. These problems are caused by the difficulty to recover these oxoanions as stable solid precipitates with low solubility in water. The establishment of recycling system of these hazardous compounds will be one of the world-important issues, especially, in Japan, which is poor in natural resources. On the other hand, compounds that contain high arsenic concentrations and are insoluble in water, are often found in natural minerals, for example, as haidinglite (Ca(AsO3OH)·(H2O) or Johnbaumite (Ca5(AsO4)3(OH)). This fact suggests that nature has an ability to produce insoluble As-bearing minerals. Similar phenomena can be found in case of boron, antimony, etc."

Jan 1, 2008