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By Mahmoud A. Rabah

"In this work, metal values were prepared from used beverage cans. The cans are made of aluminum and minor alloying metals and printed with a multi-color printing ink. A method has been investigated to remove the printed coating using organic solvents or by sand blasting technique in a rotating drum. Metal values of the cleaned cans are prepared applying combined hydro and pyrometallurgical treatments. Factors affecting the efficiency of the suggested method have been studied.The results show that the extent of removal of the printing coating is successfully performed with recyclable methyl ethyl ketone I dimethyl formarnide mixture. With sand blasting, it proceeds regularly with the inner diameter, the rotation speed of the drum, the size of the sand grains and temperature. The removed coating is stripped with the same solvent. Metal alloy(s) are prepared in two ways. In the first way, the cans are pressed into solid blocks using hydraulic press before melting at temperatures up to 1000°C using borax-sodium chloride salt mixture as a flux. The quality of the metal obtained is a function of the salt and temperature. The slag so formed was leached with mineral acid solutions. In the second way, the used beverage cans are directly dissolved in mineral acids whereby different metal values are selectively precipitated. The undissolved part is fused with sodium carbonate at 800°C and processed in the same manner. Results were explained in the light of the thermodynamic properties of the species involved."

Jan 1, 2000

By Kazuyuki Kakegawa

"Sintered body of lead zirconate titanate (PZT) was prepared through the spark plasma sintering (SPS) technique. When the mixture of raw materials was calcined at 800°C and sintered at 900°C for 10 min. with SPS technique, the sintered body had almost theoretical density but was a mixture of lead titanate (PT) and PZT. When a calcining temperature of 1100°C was employed, sintered body had a single PZT phase but a lower density. High dielectric constant was obtained for a sample calcined at 800°C, sintered with SPS tecbriique and fired again in the air at 1100°C.IntroductionSpark plasma sintering (SPS) is a recently developed technique for sintering metals and ceramics1. The scheme of SPS is shown in Fig. 1. Sample is put in a graphite die in a vacuum chamber. It is pressed and pulse voltage is applied. The electric current heats the die. It is said that the pulse causes a spark-plasma between particles in the sample. Because of the spark- plasma, sample can be sintered at temperatures lower than that in the ordinary sintering by several hundred degrees of Celsius. The sintering period is also very short2Low sintering temperature and short sintering period in SPS technique cause low reaction rate. It is both disadvantage and advantage. In some cases, the reaction cannot be completed under the SPS conditions. If a mixture of several compositions having different properties can be sintered without a compositional change by the diffusion during the sintering, combination of properties, and therefore a design of property will be possible3. The low reaction rate of SPS may enable such combination."

Jan 1, 2000

By M. A. Barakat

Large amounts of zinc ash and flue dust containing more than 80 % zinc are accumulated during galvanization processes at the surface of molten zinc bath and in the chimney respectively. Pyrometallurgical recovery of zinc from both of the ash and dust samples has been carried out. The ash was sieved with the help of an industrial sieve shaker provided with mesh sieve having a pore size 0.9 mm. The oversize fraction cut (+ 0.9 mm) was melted at 550 °C under ambient conditions. The produced ingot (1) was analyzed whereas the coarse fraction of the produced slag (+ 0.9 mm) was treated as the coarse ash or added to it. The dust was enriched with suitable fluxing salt prior to heat treatment at 600 °C for 1 h. The produced ingot (2) was analyzed whereas the resulting slag was mixed with the fines of the ash and treated by hydrometallurgical processing to prepare valuable salts of zinc. Parameters affecting recovery processes such as time, temperature and flux percentage were studied. Results obtained revealed that the two prepared ingots (1&2) were successfully recovered with recovery efficiency amounts to =85 %. The obtained samples meet the standard specifications with relatively low price. Also in the light of the strict environmental regulations of pollution control, reuse of these wastes materials will help in keeping the environment clean.

Jan 1, 2000

By N. Menad

. Electronic wastes are heterogeneous mixture, with mainly copper, aluminium and steel attached to or mixed with various types of plastics and ceramics. In general, small amounts of precious metals are incorporated in this mixture. Today, these components constitute an environmentally problematic fraction in disposal. Their physico-chemical characteristics have been investigated through chemical, x-ray diffraction, infrared spectroscopy, scanning electron microscopy and thermal analysis.

Jan 1, 2000

By S. Ferlay

"The main purpose of the ZIMA VAL project (Label EUREKA EU1367 and LIFE ENV/F/000278) is to demonstrate industrial scale recovery and recycling of the main components of used dry batteries (zinc, manganese dioxide, mercury, and stainless steel) into high added value products. The originality of the ZIMA VAL process resides in:1- the use of hydrometallurgy2- alkaline treatment implementation (highly selective) for zinc and mercury3- electrochemical recovery of high quality products.4- the recycling of all the battery components (zinc, mercury, manganese dioxide, stainless steel) ·5- low operating and investment costs.The process consists of physical classification, mechanical dismantling, hydrometallurgy and electrochemistry. The purpose of the demonstration plant in FALAISE (Calvados - France) is to define the technical and technological parameters of an industrial unit for the treatment of 2400 tonnes per year of used batteries."

Jan 1, 2000

By R. Menge, N. Basin, M. Sibony, J. Lecadet, S. Schmidt

In 1996, Metaleurop replaced its conventional sintering and blast furnace lead smelting activity in Nordenham, Germany by Sirosmelt/Ausmelt technology. Following some alterations to the process and the equipment, the bath smelting plant reached its design capacity for the treatment of lead concentrates, lead sulphate paste from spent batteries, secondaries and internal by-products. A reliable metallurgical process has been established, and thus higher process stability has been achieved, increasing simultaneously the refractory life. Nevertheless, improvements are needed to control the process with a better automation system and reliable expert-systems, because of the intensity of the smelting process. The introduction of the Sirosmelt process for the pyrometallurgical production of lead instead of the prior conventional process has also demonstrated the following advantages: reduced emissions of heavy metals and gaseous compounds, reduction of the specific energy consumption, minimization of residues and a reduction of staff and maintenance costs. The environmental performance of the plant meets the requirements of the German regulations.

Jan 1, 2000

By Takashi Nakamura, Kenji Oosumi, Kazuhisa Fujisawa, Takayuki Kogishi

"Recycling of used aluminum beverage cans(UBCs) is one of the important issues for aluminum manufacturer presently. The direct re-melting of UBCs shows two problems. One is a reduction in molten aluminum recovery and the other is a contamination of other metals such as Ti and Fe from paints. Both problems are caused by paints coated on the surfaces of aluminum cans. Removal technique of the paints, therefore, has been required. Although roasting and shot blast techniques have been developed, both were not successful in removing the paints effectively. A swell-peeling method has been applied to remove them using a methylene chloride solution with acids and it works very well. Small laboratory scale tests have been carried out to develop the commercial process and clarify the mechanism of the swell-peeling method in the present study.When the surface area of UBC is more than 10 cm2, peeling time is independent of the surface area, about 60 seconds, because swelling phenomenon is controlled by the penetration of the liquid through the fine pits on the surface of the paint. This is good for a commercial process. Peeling takes place when the swelling force generated by methylene chloride exceeds the adhesion force between the film and the surface of aluminum, that is weakened by the coexisting acid, especially halogenated acetic acid."

Jan 1, 2000

By D. Ducharme, J. Lenz

Operation of the Kidd electrolytic zinc plant commenced in 1972 with a cellhouse capacity of 105,000 tonnes of zinc cathode. The original cellhouse layout consisted of 42 parallel rows for a total of 588 cells. As leaching capacity increased, the cellhouse was expanded to 630 cells. Zinc cathode was manually stripped from plant start-up until the development of a mobile automated stripping system in 1994. Machine development continued until a second unit was placed in production in 1996, from which point, 60 % of the cellhouse was being stripped with the automated system. The final phase of the project was implemented in 1999 with the commissioning of two more automated strippers. This paper describes the implementation of the automated stripping system and its impact on cellhouse productivity.

Jan 1, 2000

By M. Olper, M. Maccagni, C. J. N. Buisman, C. E. Schultz

The key point of the CX-EWS process is the conversion of lead compounds, contained in the active mass of spent batteries, into lead sulphide. The obtained lead sulphide is leached with ferric fluoborate electrolyte to dissolve lead and oxidize the sulphur from sulphide to the elemental form. The lead-rich solution is fed into a diaphragm electrolytic cell depositing lead and regenerating ferric fluoborate. The introduction of sulphate reducing bacteria technology in the sulphidization step of the battery paste improves dramatically the economics of the CXEWS process, reducing the costs of chemicals, avoiding gypsum disposal and minimising the unit operations of the process. This paper describes in detail this technology change with reference to the economics of the process.

Jan 1, 2000

By James P. Bennett, Jasper Kwong

As concerns about the environment and the disposal of industrial wastes increase, the utilization of spent refractories from electric arc furnaces (EAF) is receiving more attention. Longer service life of refractories in an EAF can be achieved by foaming MgO saturated slag. The refractory wastes removed from a melt shop can be utilized as a part of these slags. The Albany Research Center is conducting research on recycling spent basic refractory materials as EAF slag conditioners. A good foaming slag should be a creamy, MgO saturated slag, which contains some solid particles (MgO-FeO). A computer model was developed to calculate the dual saturated slag chemistry with respect to CaO and MgO, the MgO saturated slag chemistry, and the solid content in solution. The effects of C/S ratio, AhO3 and temperature on the MgOsaturated slag as calculated by the model will be discussed.

Jan 1, 2000

By Jing Lin, Yuan Xu, Qingcai Liu, Dengfu Cheng

"Smelting reduction technology has been developed greatly in recent years. But one of the key problems for this technology is about the refractory that used as lining material in the molten bath. Investigation and test shown that corrosion rate of refractory was much higher and the corrosion mechanism was much more complexity in the molten bath of smelting reduction with iron bath than that of the blast furnace and rotary furnace technology [l-5]. The corrosion behavior and corrosion rate of Al2OrC-ZrO2 series refractory in the melt of smelting reduction with iron bath have been studied by rotary immersion and quasi-static immersion test in this paper. The major factors that affect the interaction between the melt and refractory were investigated. The test results shown that the corrosion rate of AI2O 3-C-ZrO2 series refractory decreased with the ZrO2 increasing when ZrO2 content was from 3% to 10%. Ferrous oxides content, relative moving speed between the melt and refractory and temperature of the molten bath were the important factors that affect the corrosion rate. But the ferrous oxides concentration was the most important one. The corrosion rate was increased as a linear relation with the rising of ferrous oxides content of the melt. The corrosion rate in the quasi-static immersion was much less than that of the dynamic immersion (rotary immersion) for the Al2O 3-CZrO2 series refractory in the same testing condition. The corrosion mechanism of Al2OrC-ZrO2 series refractory is: graphite oxidized in advance, then interaction between the constituents of refractory and melt taken place and deteriorate layer of refractory and new compounds were formed, the properties of refractory was changed.IntroductionSmelting reduction with iron bath is a typical technology [3, 4, 6]. The obvious features of the melt for smelting reduction technology with iron bath are much higher ferrous oxides and much more complexity melt composition and structure than that of the blast furnace technology [2, 5-8]. The properties of the melt were changed dynamicilly and constantly in reduction process. On the other hand, the behavior of the melt depends on the activity and the reduction rate of ferrous oxides in the molten bath[9]. Because of the high concentration of ferrous oxides in slag and high reduction rate in the molten bath, the corrosion behavior and corrosion mechanism of the refractory lining by melt are an important factor in development of the technology of smelting reduction with iron bath. Up to now, improving refractory quality to anti-corrosion of melt and developing high quality and long term refractory used as the lining refractory materials in the molten bath of the final reduction furnace are also the most important questions for developing smelting reduction technology."

Jan 1, 2000

By Bradford C. Wesstrom

The extraction of metals from Copper Refinery Slimes may involve many different processes. This paper describes the use of pressure leaching for decopperizing of copper refinery slimes at the El Paso Refinery. Process equipment will be described, along with the process chemistry, unit operations and unit processes associated with the decopperizing process. Copper contained in the raw slimes ranges from 15-35%. After autoclaving less than 1 % copper remains.

Jan 1, 2000

By Corby G. Anderson

Today, with a stringent economic and environmental climate prevailing in the copper business, there is increased interest in evaluating new processing alternatives for production. Hydrometallurgical pressure oxidation of copper concentrates is one of the more viable approaches and several technological candidates have emerged. Of these, an overlooked but, ironically the first industrially proven methodology, utilized nitrogen species catalyzation in the oxidizing pressure leach system to produce copper via SX!EW. Given its many inherent process advantages, this may prove to be a feasible process alternative for the future. In this paper, the history of the system and its application to chalcopyrite concentrates will be outlined. In particular, a novel methodology for effective recovery of precious metals from chalcopyrite concentrates will be discussed. Finally, the perceived economics of this unique industrially proven process will be delineated.

Jan 1, 2000

By U. Kammer

The reduction of the lead content in the separator fraction produced during the mechanical processing of spent lead-acid batteries is an important environmental and economical issues. The reduction of lead down to less than 1 percent is very difficult using hydroseparators that are common in battery recycling facilities. Very promising results were achieved performing experiments on a test rig using a new technology in battery treatment: a discharge-type jigging unit. The materials is fed onto the jigging bed and transported through the machine. Due to the intensive movement of the feed, an additional washing effect is also obtained in addition to separation of the lead and plastic fractions. The knowledge gained from this development work at UVR-FIA GmbH in Freiberg, Germany, led to a patent application. This paper focuses on the results of the development work and the start-up and one year's operation of the industrial-scale application at Harz-Metall GmbH in Goslar, Gennany.

Jan 1, 2000

By O. Kitamura, H. Kubota

The Harima Works started its ISP operation in 1966 and been expanding its production capacity from 3,000 tonne Zn/month and 1,500 tonne Pb/month to 7,500 tonne Zn/month and 2,500 tonne Pb/month. It is not only treating zinc, lead and bulk concentrates but also secondary materials like Waelz kiln oxide from the Shisaka Works of Sumitomo Metal Mining, waste treatment sludges, industrial wastes and others. Its final products cover Prime Western Grade (PWG) zinc, Special High Grade (SHG) zinc, continuous galvanizing grade zinc, electrolytic lead, cadmium, indium, thallium and sulfuric acid. This paper briefly describes the smelter's historical and present operations. The key data for the current impurity control management and for the distribution of impurities such as copper, iron and arsenic are presented.

Jan 1, 2000

By Masahiro Yoshimura, Sergiy Korablov

"Hydi-othermal corrosion ofTiN, TlAlN and CrN PVD films (3 µm thick) deposited on SUS-304 substrate was studied in 100MPa water in 20-950°C temperature range up , to 750h. The beginning temperature of their reaction was determined as 200°c for TiN and TiAlN and 500°C for CrN films, which are quite low in comparison with that of air oxidation of those powders. Very thin oxide scales. of TinO; n-I homologous series phases were formed above 300°C. TiO2 anatare. is observed for TIN and TiAlN films at 400°C. The· feature of hydrothermal corrosion of CrN films seems to be CrNxOy phase formation.Distinguishable weight changes were observed at higher temperature than 700°C for TiN, 750°C for· TiAlN and 800°C for CrN respectively. Hydrothermal corrosion kinetics .was constructed to calculate the activation energy of hydrothermal corrosions. On the base of obtained data, hydrothermal corrosion resistance was as follows: TiN – TiAlN - CrN. Facetted oxide crystals were formed at higher temperature than 500°C for TiN, TiAlN and 850°C forCrN.IntroductionThe metallic nitride (TiN; TiAlN, CrN) PVD films have high hardness, strength and wear resistance. Therefore these films are widely used in industry for wear resistij.nce application such as cutting tools and die molds. Their performances depend on not only the mechanical properties but also corrosion resistance of coated films. High temperature oxidation of metalliq nitride and nitride films was well studied [1-5]. However there are no reliable data concerning the .corrosion resistance of coated nitride materials. In high-temperature and high-pressure water. There are a few reports on hydrothermal corrosion of nitride films [6,7]. The increase of corrosion resistance of CVD films was observed in following succession TiC - TiCNO - TiCN - TiN at 300-680°C temperature interval and I 00 MPa pressure water according to data of the first report. Kawana et al. [7] have reported about excellent corrosion resistance of CrN films under 290°C and 8, 6 MPa water during I 000 h in the circulating type experimental loop. The films thickness was about 7-10 µm in both cases. However it remains unclear the chemical state of the surface species and especially in-depth distribution, oxide scale thickness and its growth, and defects formation in the oxide film."

Jan 1, 2000

By Hiroshi Ono

"By newly developed ICP method, trace amounts of As(III), As(V) .,Sb(III) and Sb(V) were precisely determined within accuracy of sub ng/ml. As(III) and Sb(III) were separated from As(V) and Sb(V) by extracting into ·xylene as diethyldithiocarbamate complexes using diethylammonium diethyldithiocarbamate (DDDC), and then back-extracted into nitric acid for a quantitative determiruition by ICP-AES equipped with hydridegeneration system The recoveries of As(III) and Sb(III) were satisfactory throughout the extraction with 0.04mol/l DDDC in xylene from lmol/l hydrochloric acid solution and the back-extraction with 7 mol/l nitric acid. As(V) and Sb(V) were reduced to As(III) and Sb(III) by ascorbic acid and potassium iodide, and their quantities were determined as mentioned above. The detection limits were found to be 0.58ng/ml for As(III), 0.63ng/ml for Sb(III) using 50ml of a sample. The proposed method was applied to analysis of the real sample.Introduction In drain, arsenic(AS) concentration is prescribed below 0.lmg/l, so As must be removed. As is existed at .the form of As(III) or As(V) in solution. For t1Jeir difference of chemic;µ property, it is not easy to remove As in solution. So it is an urgent necessity to develop for determining concentration of As(III) and As(V). Antimony( Sb) has resemblance .chemical property to As. So Sb was experimented the same as As.The separation and determination of As(III) and As(V) have been carried out using several methods, such as ICP after copreclpitating separation, HPLC, direct hydride generation atomic absorption. However these methods have some problems. One of main problems is that HPLC and direct hydride generation atomic absorption methods are influenced by coexisting elements."

Jan 1, 2000

By Mitsuhiro Ohtaki, Tetsuzo Arakawa, Fujio Murata

Refining of Zn from aluminum scrap melt by some vacuum distillation processes was studied to promote aluminum scrap recycling. Effects of distillation conditions, such as melt temperature, vacuum pressure and holding time, on Zn distillation behavior were investigated theoretically and experimentally by 0.3kg/ch scale vacuum resistance furnace. Three methods to increase the surface-area/volume ratio of liquid metal, such as gas atomizing, mechanical atomizing and mechanical stirring, were tested to increase the Zn distillation rate in 5kg/ch scale vacuum resistance-furnace. It was easy to lower the remaining Zn content to less than 0.1 wt% within one minute by mechanical stirring method. A water-model simulation experiment indicated that a significant agitation of the melt by stirring would be effective to increase the distillation rate. Continuous agitation vacuum distillation process (CA VP) has been designed and the pilot plant is now in construction.

Jan 1, 2000

By Shoji Taniguchi, Lifeng Zhang

"In this paper, firstly the 3D single-phase turbulent steady fluid flow in a vessel with four baffles stirred by a single impeller is mathematically simulated. Turbulence is modeled by using the standard k - e model. Sliding-grid method is used to model the impeller. The flow domain is divided into two cylindrical, the inner one rotates at the same speed as the impeller, and the outer one is fixed with the baffles. Results indicate that the high-speed zone is near the paddles, and larger stirring speed generates larger fluid flow velocity. The calculated stirring intensity data are used to analyze the experimental results. Secondly the effects, such as filter pore size, gas flow rate and NaCl concentration, on bubble size are studied by experiment. For the particle removal rate by bubble flotation in this vessel, first order kinetics is adopted. The effects of initial number of the particles, gas flow rate, particle and bubble size, stirring speed and surface condition, on the removal rate constant are discussed, and an empirical equation is derived by experimental data. At last, a simple model is developed to study the particle attachment probability on bubble surface under turbulent flow conditions. IntroductionIt is well known that inclusions have a bad effect on steel quality. Trying to remove inclusions from liquid steel as many as possible is one of the main objects for the metallurgical workers. Lots of ways are developed to remove inclusions from liquid steel. Gas injection is an effective one. This technique is used to achieve homogeneity in the temperature and metal composition and to assist in the removal of second phase and dissolved impurities from molten steel. Gas injection is commonly applied to the secondary metallurgy processes and continuous casting, for example the ladle argon gas treatment, RH vacuum degassing, and the gas injection in the Submerged Entry Nozzles (SEN) of continuous casting mold, etc. The development of these processes focuses on achieving two conditions: fine bubbles and good mixing. Fine bubbles provide a large gas/liquid interfacial area and a high attachment probability to inclusions, and good mixing enhances the efficiency of impurity transfer."

Jan 1, 2000

By Fabiola Alvarez, Ana E. Bote, Daniel Pasquevich

"The oxidation of aluminum and its alloys was extensively studied for improving the corrosion resistance in structural materials having high specific strengths. But this reaction involves the formation of a very thin barrier layer on the metallic pieces. Furthermore, the ·recent development of the directed melt oxidation process for producing metal-ceramic; composites has renewed the interest in the study of interaction between gases and metals. Oxidation experiments in the presence of different chlorine partial pressures and at different temperatures were performed in ·a thermogravimetric balance, and microstructures were analyzed by electronic microscopy and X-ray diffraction. The oxy-chlorination kinetics was determined and the oxide formed W(IS amorphous at temperatures below 600 °C and crystalline .at higher temperatures. The appropriate experimental conditions for the fastest completed oxidation was further determined.IntroductionThe use of fine powders for the manufacture of ceramic components has significant advantages. They include excellent sinterability; low sintering temperature and better microstructure leading to improved mechanical properties. The conventional method of producing fine oxide powders involves controlled precipitation and pirolysis of suitable salts. The main limitation of the high temperature decomposition route is the evolution of environmentally unacceptable and corrosive gases. Controlled precipitation of hydroxides from solutions of salts, followed by thermal treatment involves large volumes of solutions and the calcination step that can induce grain growth (1).Direct oxidation of aluminum metal for producing alumina powder requires high temperatures for the direct oxidation of molten Al alloys by a vapor phase oxidant process (2, 3) or high technological process like thermal plasma reactor ( 4).Oxidation of high purity aluminum (5, 6) below the melting temperature· is initially characterized by a nearly linear reaction rate, followed by a rate which decreases rapidly with further weight gain. However, the oxidation rate of an aluminummagnesium alloy is much faster and it does not conform to any common oxidation law, but it is nearly parabolic at temperatures between 200 and 400 °C, an nearly linear· above 400 °C."

Jan 1, 2000