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By Arpad E. Tonna

Recycling of materials from lithium-oxyhalide batteries is a complex task, since the dismantling of batteries is associated with many hazards. The electrolyte and the lithium anode metal are extremely reactive in the presence of water or water vapor. Therefore, the dismantling process is a complex task. In this process, the lithium battery is electrically discharged, then frozen in liquid argon, and cut into small size pieces. These are fed into an incinerator, where the unreacted portion of lithium metal, thionyl chloride, plastic separators and carbon paste are decomposed and burned to gaseous products. The aluminum, iron (steel) and nickel pieces are recovered as saleable scrap metals. The off-gases are scrubbed with an alkaline sodium carbonate containing solution. The clean gases are released to the environment. The particulate mater recovered from the scrub-suspension would be available as additive to the cement industry . The recycling of battery decomposition products improves the economic viability of the disposal processes. Work is in progress to develop safe handling, processing and recycling large size lithium batteries.

Jan 1, 1995

By Guiqing Zhang, Liansheng Xiao, Zuoying Cao, Li Zeng

A new process of direct solvent extraction of nickel from sulfuric acid leach solutions of low grade and complicated nickel resources using a novel extractant HBL110 was proposed. The basic performance of new organic system was investigated and the continuous pilot plant and the industrial test were conducted. The results indicated that the extractant of HBL110 can be used to directly extract nickel selectively over iron, aluminum, manganese, magnesium, calcium and chromium from sulfuric acid leach solutions. The loaded organic solution can be easily stripped using dilute H2SO4 solutions. Both kinetics of extraction and stripping of nickel were fast. The continuous pilot plant test with the sulfuric acid leach solution of laterite containing 6.22g/L Ni2+, 14.1g/L Fe3+, 0.73g/L Fe2+, 33.9g/L Mg2+, 1.58g/L Al3+, 0.495g/L Ca2+, 0.97g/L Mn2+ and 0.5g/L Cr3+ as feed in mixer-settlers showed that the process had run stably with 98% recovery of nickel. The concentration of nickel in strip liquors reached as high as 50 g/L while the removals of Fe3+, Fe2+, Mg2+, Al3+, Ca2+, Mn2+ and Cr3+ were 98.5%, 91.5%, 99.95%, 99.8%, 99.1%, 98.6% and 99.5%, respectively. The industrial test with the sulfuric acid leach solution of electroplating sludge containing 11.5g/L Ni2+, 2.68g/L Fe3+, 7.54g/L Cr3+, 0.61g/L Mg2+, 2.09g/L Al3+, 0.68g/L Ca2+, 0.022g/L Mn2+ and 0.154g/L SiO2 as feed in mixer-settlers also showed that the process had operated successfully with 99.5% recovery of nickel. The concentration of nickel in strip liquors reached 42.7 g/L while the removals of Fe3+, Cr3+, Mg2+, Al3+, Ca2+, Mn2+ and SiO2 were 99.2%, 99.77%, 99.73%, 99.56%, 99.57%, 98.51% and 98.75%, respectively. The new process exhibited big advantages of short flow sheet, high recovery of nickel, high removal of impurities, low chemical reagent consumption and low cost. Application of this process in industry is expected to make important impact on the extraction of nickel from sulfuric acid leach solutions and to deliver good environmental and economical benefits.

Jan 1, 2016

By Marcos Aurélio S. Costa, Nilton F. Nagem, Andreia B. Henriques, Herman S. Mansur, Alexandra A. P. Mansur, Antonio E. C. Peres, Valeria G. Silva

The superfine material generated in the Bayer process was used in one innovatively way as a precursor to geopolymerization techniques because of the presence of Gibbsite. Gibbsite can play a role in system adjustment because of the SiO2/Al2O3 ratio. Furthermore in the geopolymeric system it was studied the influenceof the additives such as kaolin, metakaolin and sodium trisilicate in an alkaline media. Others conditions to form the geopolymer were also evaluated such as solid/liquid ratio, SiO2/Al2O3 ratio and total alkaline. The raw materials and geopolymeric products were characterized by several techniques e.g. XRD, DSC, FTIR and SEM. Through the FTIR technique it was observed an increase in intensity and bandwidth in the region centered at 1010 cm-1, which is related to the asymmetric vibration Si(Al)-O, this is an indicating of the possible geopolymer formation This broadening of the band promotes a relative disappearance (overlapping) peaks at 965 and 935 cm-1 associated with raw material (ESPDust).

Jan 1, 2015

By C. A. Nogueira, F. Margarido

"A research work has being carried out annmg at evaluating the possibility of treating simultaneously several electrochemical systems of spent batteries using the same process, in order to overcome the high costs and difficulties of selective collection and sorting. Zn-Mn02 systems, representing more than 75% of portable battery market, shall be treated in dedicated processes. The treatment assessment using a single hydrometallurgical process of the other major systems (NiCd, NiMH and Li-ion), having Ni and Co as main metals, was the aim of the research work here reported. Sulfuric acid leaching was demonstrated to be adequate for dissolving more than 90% of the metals of interest contained in batteries. The subsequent separation of metals by solvent extraction, using organophosphorous extractants like DEHPA and Cyanex 272, allowed the production of pure solutions of rare earths, cadmium/manganese, cobalt, nickel and lithium, enabling their further recovering.IntroductionRecycling is the best approach for end-of-life management of spent batteries mainly by environmental reasons but also motivated by resources conservation and, in some cases, by economic profits. Most relevant electrochemical systems of portable cells are Zn-Mn02 (ZMB, alkaline and saline), nickel-cadmium (NiCd), nickel-metal hydride (NiMH) and lithium-ion (LIB). These batteries are collected, sorted and usually treated separately, applying for pyrometallurgical or hydrometallurgical technologies, the former being the most common.Several processes have been developed and some of them industrially applied, as described in some available review papers [l, 2]. In Europe for ZMB systems the oldest processes are Batrec [3] and Citron [4]. Although having differences in details, both are based on pyrometallurgical recovery of zinc by distillation, in metallic or oxide forms, being manganese retained in the slag together with iron. Hydrometallurgical alternatives are also available, like Zincex [5] and Recupyl [ 6] processes, both using sulfuric acid solutions as leachant. The application of the existing technologies to battery recycling, instead of using dedicated processes, is other alternative already tested, being the Waeltz furnace or the Imperial Smelting some examples."

Jan 1, 2012

By Åke Saudström

An EAF dust sample generated in a scrap based steel mill was treated by a combination of hydro- and pyrometallurgial techniques. The EAF dust contained mainly ferritic spinels forming solid solution phases according to the general chemical formula (MnxZnyFe1-x-y)Fe2O4 and other oxide phases such as ZuO. CaO and Ca2Fe2O5. The EAF dust was first treated by hydrochloric acid leaching at p8=3 which dissolved 63% of the zinc. The pyrometallurgical treatment of the leaching residue was studied using an induction heating system to simulate some important operations of EAF smelting of the residue in combination with steelmaking. The leaching residue was mixed with carbon powder to obtain a mixture with 52.1% ZnFe2O4 and 175% carbon. The mixture, scrap, and slag former were charged together in a crucible and heated to attain a melt temperature around 1650°C. The effects of different amounts of mixture on the zinc balance and iron recovery were examined. Based on the test results, suggestions are made for the EAF recycling procedure of the leaching residue.

Jan 1, 2003

By Nobuo Takahashi

Effective solvent extraction media have been investigated for purification of rare earths. At first, a quaternary ammonium compound was studied. The counter anions of rare earths and organic dielectric substances were tested to improve separation factors,. And second, crown ethers were selected for extractant. Several diluents of crown-adducts were tested to improve solubility and distribution coefficient as well as the counter anions of rare earths. Especially, in the presence of strong reducing agents, highly selective extraction of europium from other rare earths was observed. The third extactnts were ß -diketones. Presence of organic dielectric substances was very effective to improve separation factors. Though those. three groups of extractants were suitable for mutual separation of light rare earths, alkyl esters of alkyl-phosphonic acids were suitable for mutual separation of heavy rare earths because of their high separation factors. To keep proper pH value was necessary for acidic extractants, so control method of the solution pH was studied with high molecule insoluble amines or salts of those.

Jan 1, 1995

By Kimio Itagaki, Makoto Ohtsuka, Kouki Chiba, Minoru Matsumoto

"The properties of Ni-Mn-Ga films such as chemical composition, crystal structure, microstructure and transformation temperature were investigated with respect to sputtering conditions in the present study. The Ni-Mn-Ga films were deposited on a polyvinyl alcohol substrate with a radio-frequency magnetron sputtering apparatus using the NisoMn2sGa2s and Nis2Mn:«1Ga24 targets. After separating from the substrates, the films were annealed at the temperature between 873 and 1273 K for 3.6 ks. The chemical composition of the films depended on the radiofrequency generating power, however, there was no dependence on the heat treatment temperature. Each deposited film had a columnar grain structure. After heat treatment, the width of columnar grains widened and then became indistinct with increasing heat treatment temperature. The Heusler type cubic crystal structure of the fi4n with heat treatment at 1073 K changed to the tetragonal one through the martensitic structural transformation during cooling. The martensitic structural transformation temperature increased with increasing nickel content of films, while the Curie temperature decreased. The film obtained at 200 W using the Nis2Mn24Ga24 target after heat treatment at 1073 K showed one-way shape memory effect through the reverse martensitic structural transformation during heating.IntroductionThe ternary intermetallic compound NiiMnGa has a Heusler-type crystal structure and is an intelligent material, which has a shape memory effect and a ferromagnetic property. The martensitic structural transformation occurs within the ferromagnetic temperature region. The cubic crystal structure of L21 at high temperature changes to a tetragonal one through the martehsitic structural transformation during cooling. The films of this compound can be applied for an actuator of micro-machines."

Jan 1, 2000

By Xuerong Wen

The oxidation behavior of TiAl3 intermetallics was investigated as a hnction of time at 1273K in pure dry oxygen. The oxidation experiments were carried out using TGA method. The oxidation scales were analyzed using SEM, EDS and X-ray diffraction methods. The structures of oxides formed at the different oxidation times were analyzed. The mechanism of oxidation of TiAl3 intermetallics was discussed.

Jan 1, 1998

By Guo Chen, Xuefeng Liao, Tu Hu, Shengzhou Zhang, Hongying Xia, Jinhui Peng, Libo Zhang

Pine nut shell is as raw material for preparation of high surface area activated carbon (HSAAC) by microwave induced KOH activation. The effects of microwave power, activation duration and KOH/C mass rate (R) on the iodine adsorption capability and activated carbon yield were investigated. Additionally the surface characteristics of HSAAC were characterized by nitrogen adsorption isotherms and SEM. The operating variables were optimized utilizing the response surface methodology and were identified microwave power 738W, activation duration 17 min, and R 4, corresponding to a yield of 46.28 % and an iodine number of 2154 mg/g. The key pore structure parameters of HSAAC such as the Brunauer–Emmett–Teller (BET) surface area and total pore volume were estimated to be 3819 m2/g and 2.09 mL/g, respectively. The findings strongly support the feasibility of microwave heating for preparation of HSAAC from spent pine nut shell by microwave induced KOH activation.

Jan 1, 2016

By M. Wu, A. Kharicha, A. Ludwig

"The droplet formation during melting of a 400 mm diameter electrode is simulated with a multiphase-MHD approach. The computational model includes a layer of slag and a layer of liquid steel. A VOF approach is used for the interface tracking and a potential formulation is used for the electric and the magnetic field. The Lorentz force and the Joule heating are recalculated at each time step in function of the phase distribution. The first results provided by this model are presented.IntroductionThe Electro-Slag-Remelting (ESR) process is an advanced technology for the production of components of e.g. high quality steels [ 1-9]. An alternating current (Figure 1) is passed from a conventionally melted and cast solid electrode through a layer of molten slag to the baseplate. Because of the electrical resistivity of the slag, Joule heating is generated and the slag transfers this energy to ingot and mould surfaces and to the melting electrode tip. The molten metal produced in the form of droplets passes through the slag and feeds a liquid pool from where directional solidification takes place. The slag and the ingot are contained in a water cooled copper mould. As also the baseplate is water cooled, a heat flow regime is imposed that gives controlled solidification, and this results in improved structure characteristics of ESR ingots.This process involves two liquids, a liquid metal and a liquid slag. Each liquid is subject to a phase change due to melting and/or solidification. From a fluid dynamic point of view, the ESR process is clearly a multiphase process, with free interfaces (slag/pool, gas/slag), and with a mixed area (slag and falling steel droplets) [ 10-15].Physically, the development of the heat and mass transfer at the slag/droplet interface is important for the final ingot quality, composition and cleanliness. Visual observations of the droplet formation just under the electrode being melted is almost impossible. Due to the presence of high temperatures, opacity of the materials, and the presence of the mould it is not possible to directly observe the behaviour the slag/pool interface. Although usually assumed flat [1-9], a previous work [10] using a Volume of fluid (VOF) model has shown that the interface shape between a layer of slag and steel layer in a cylindrical cavity is highly coupled with the distribution of the electric current. A full scale simulation of the ESR process using a VOF model has shown that the shape of the pool interface is likely to be non flat."

Jan 1, 2011

By B. Q. Li, Y. Shu, K Lynn

"This paper discusses the effects of magnetic field and internal radiation on the melt flow and solidification morphology during solidification processing of oxide crystals for optoelectronic and remote sensing applications. The numerical solution of the integral differential equation characterizing the internal radiation and the magnetohydrodynamic equations describing the magnetic and transport phenomena is obtained by applying the combined discontinuous and continuous finite element method. The results show that both internal radiation and an externally applied magnetic field can have important effects on the melt flow and solidification behavior during the melt processing of oxide materials.IntroductionOptical single crystals are widely used in optical and electronic devices. These crystals are often grown from high temperature oxide melts under strictly controlled conditions. As in the well-known single crystal growth processes for semiconductor wafers, thermal gradient in the melt is a major contributing fuctor to the oxide melt pool. Unlike the semiconductor single crystal growth processes, however, the oxide melt is semitransparent and internal thermal radiation plays an important role in redistributing the thermal energy in the melt pool. Our recent experience with pilot-scale plant measurements also shows that the oxide melt is electrically conducting, although its electrical conductivity is considered much lower than the liquid metal or semiconductor melt.The fact that the oxide melt is absorbing and emitting in the thermal radiation frequency range makes it difficult to study the thermal energy transport in the melt pool. This is because thermal radiation is governed by a hyperbolic differential equation, which is different from those describing the transport processes in liquids. Also, our understanding of how thermal radiation interacts with other transport mechanisms such as convection and conduction is rather limited at point in time, in particular in high temperature oxide melts for optical single crystal processing."

Jan 1, 2004

By Merete Tangstad, Fei Li

This paper studies the quartz and carbon black pellets at elevated temperature with varying temperature and gas atmosphere. High-purity quartz and commercial ultra-pure carbon black was mixed (carbon content wt.15%), and then pelletized into particles of 1-3mm in diameter. The stoichiometric analysis of the pellet during heating is studied in thermogravimetric analysis (TGA) furnace at different temperature in CO and Ar atmosphere. The microstructure, phase changes and element content of sample before/after heating is characterized by X-ray diffraction, scanning electron microscope, X-ray fluorescence and LECO analyzer. The reaction process can be divided into two stages. Higher temperature and argon atmosphere are the positive parameters for SiC formation.

Jan 1, 2016

By Rodney J. Ishak

The reduction of Mn3O4 to MnO has been investigated in a thermobalance apparatus. The charge was composed of manganese ore (decomposed by heating/calcination or pre-reduction to mainly Mn304) and coke. The material was charged to a crucible, which was suspended in the balance. CO-gas was distributed through a grid in the bottom of the crucible. Two sizes of ores were used; 2.4-4.8 mm and 6.7-9.5 mm. Coke particles were in the size range 4.8-6.7 mm. Experiments were conducted in the 900-1100°C temperature range. The composition of the product gas was monitored continuously. External mass transport between bulk gas and particle surface does not seem to limit the rate of reduction. Assuming that both diffusion through product layer and chemical reaction at the interface between MnO and Mn304 are rate controlling, the data was tried both in a shrinking core model and in a grain model using regression. The grain model gives the best physical description of the process, because the reactant is in fact a porous medium. With this model the effective diffusivity was calculated to be in the 1.5-6.10-5 m2/s range. The pore size was mainly between 0.1 and 10 um.

Jan 1, 2003

By Jewel Gomes

Produced water (PW) is salty water trapped in the reservoir rock and brought up along with oil or gas during production. It subsists under high pressures and temperatures, and usually contains hydrocarbons and metals. Therefore, it must be treated before being discharged to surface water. Different techniques are being used to treat PW through phase separations, system control and design, and chemical treatments. In this paper, we discuss our experimental results on treating PW through electrocoagulation (EC). The performance of EC was investigated for the reduction of chemical oxygen demand (COD) and metal ions. Effects of different electrodes, residence time, current density, and pH were also studied to optimize the treatment conditions. Different kinds of cleansing agents, such as lime and borax were used to break the buffering effect encountered during treatment. FTIR, SEM/EDS, and XRD were used to characterize the EC-floc and thus to elucidate removal mechanisms.

Jan 1, 2009

By K. S. Izbakhanov

The Chimkent Lead Plant was constructed in 1934 and since that time has undergone many revisions. In 1975 the slag fuming operation was changed from pulverized coal to natural gas fuel. In 1981 the slag fuming furnace water jacket system was converted to evaporative cooling with high pressure steam production. The impact of these changes and the method of their application are described.

Jan 1, 1990

By Shengli Wu, Laixin Wang, Minyin Kou, Xinliang Liu, Weidong Zhuang, Yujue Wang

COREX process has obvious advantages in environment protection but still has some disadvantages, for example, it has a higher sulfur content of hot metal than blast furnace. In this paper, the thermodynamics and dynamics of desulfurization have been investigated to obtain the main operation parameters related to the mass fraction of sulfur in the hot metal. In addition, statistical analyses have been carried out to study the relationship between operating parameters and sulfur content of COREX hot metal based on actual plant data. It has been found that the mass fraction of sulfur in hot metal is significantly influenced by the C content in hot metal, MgO/Al2O3 in slag, the concentration of MgO in slag, the temperature of hot metal and binary basicity (R2).A linear model has been developed and subsequently used for reducing the mass fraction of sulfur in hot metal, improve the quality of hot metal and contribute to low carbon ironmaking.

Jan 1, 2016

By Wang Jia, Chai Li-yuan, Zhang Jin-Long, Peng Bing, Zhang Qiang

"Electrolytic manganese dioxide (EMD) residue was mixed with shale and fly ash as the main materials to make solidification/sintering brick for the utilization of the residue from EMD production. The effects of sintering temperature, sintering time, solid waste content and cooling process on its mechanical properties and toxic elements solidification were investigated according to compressive strength and leaching toxicity. The results showed that the calcined residue had capability of solidifying toxic metals and exhibited perfect strength after treated in the optimal parameters of EMD residue below 50%, temperature at 1000-1100°C, time3-5h, and semi-quenched at 600°C1 InstructionSolid clay-brick holds the leading position among building materials for a very long time in China. The traditional technique of making clay-brick has the drawbacks of backward process, simple facilities and single product. Since Chinese Reform and Opening-up, urban-rural construction and real estate have been booming with the rapidly development of national economy and science technology. The problems of ruining fertile land, environment contamination and high energy consumption in the traditional technique of clay-brick making have not been solved yet. On the other hand, more than 7 billion tons of industrial wastes are accumulated over years which occupies over 6.7 million hectares filed and causes serious environmental problems[1-31. Strategy present in ""The Chinese Agenda of the 21st Century"" required the production of wall materials less energy conservation, land saving and waste recycling.Coal gangue[4-9l, fly ash[I0- 13l, sludge from waste water treatment and tailings of gypsum, pyrite, copper mine, high silicon containing iron, asbestos and ects [l4-lSJ are the solid wastes used for brick making around the world. There are two kinds of process for brick making, high temperature sintering and low temperature steam curing[19•201. Although the technology of two brick making made great progress and got widely application in construction field, no precedent for preparing sintering-bricks with EMD residue as materials occurred in China because of its complicated processing technics and lack of sufficient practical experience to guarantee the bricks' quality.In this study, EMD residue was mixed with shale and fly ash as the main materials to make solidification/sintering brick. The effects of sintering temperature, sintering time, solid waste content and cooling process on its mechanical properties and toxic elements solidification were investigated according to compressive strength and leaching toxicity."

Jan 1, 2011

By S. Mondon

Hibi Smelter which is a Copper Smelter lining a blast furnace, produces 2,700 metric tons of anode copper per month. Generally, in a copper refinery, arsenic and antimony are considerably troublesome impurities. With regard to the elimination of antimony, Hibi Smelter has two handicaps described as follows. (1) Smelting under the slightly oxidizing atmosphere in the blast furnace. (2) Recycling the converter slag to the blast furnace after cooling. Therefore antimony and arsenic, mainly antimony, elimination tests, in which the alkaline flux was injected through the two tuyeres in the blowing stage, were carried out in the rotary anode furnace. Antimony and arsenic were respectively removed more than 90 96 from the molten copper, and their high eliminations are discussed by application of the transitory and permanent reaction model with the flux injection, which was presented by T. Lehner.

Jan 1, 1983

By M. A. Gimenes

The utilization of chlorination in extractive metallurgy and advanced ceramics areas has been widely investigated as a preparative route in order to obtain intermetallic compounds, which are used as precursors in the development of new materials and process. The major processes of decomposition of rare-earth ores use sulfuric acid and sodium hydroxide at high temperatures, however there is not much work concerning chlorination. In this work, a systematic study of the reaction between xenotime (REPO4), chlorine and carbon has been performed. Particular emphasis was on kinetic studies to establish optimized conditions for the reaction. The kinetics of chlorination of xenotime raw material by rare-earth elements/compounds has been studied over a temperature range from 600°C to 950°C. The influence on the rate of conversion of xenotime to RECl3 on temperature, partial pressure of chlorine, carbon content, and particle size were investigated. A global rate equation that includes these parameters has been developed. The results show that the process follows the unreacted core-shrinking model with a formation of a porous product layer. The powder X ray-diffraction technique corroborated this model showing clearly the patterns related to the formation of yttrium oxychloride (YOCl), indicating that the reaction mechanism involves the presence ofan intermediate step before the formation of lanthanide chloride.

Jan 1, 2000

By ZhiLong ZHAO, Lin Lin, Zhancheng Guo, Jingtao GAO, Huiqing Tang

Grain sticking often occurs in the fluidized bed reduction of f ine iron ore, which is closely related to the precipitation morphology of metallic iron on the surface of ore particles. In this work, simulating the gas-solid reduction process of iron ore, in situ observations were carried out to investigate effects of doping mineral oxides on the precipitation morphology evolution of metallic iron during reduction of iron oxides with CO. Results indicate that the precipitation morphology of metallic iron is related to the quantity of doped mineral oxides. The minimum mole fraction of doped oxide ( xyOA N ) that can inhibit the growth of iron whiskers is related to its cation radius ( Ax r ), extranuclear electronic layers ( Ax n ) and valence electrons ( Ax q ). Their relation can be expressed as:

Jan 1, 2016