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By Keith E. Forrester

This paper presents results of bench scale laboratory evaluation of a processes developed by FESI and Brookhaven National Laboratories for the extraction and recovery of Pb and other heavy metals from incinerator ash which was subsequently modified by FESI for the extraction and recovery of Pb from soils excavated from a FESI client scrap yard and battery breaking operation facility. The specific waste matrix presented within the paper is a battery acid contaminated surficial soil at 0" to 12" depth. The extraction method was found to be highly successful on the bench scale in generating a final post-extracted soil matrix which passed TCLP Pb regulatory limits and retained minimal Pb after aggressive extraction application. The paper findings at this time are brief, as a majority of the research results are currently being compiled and additional efforts are underway based upon initial screening findings.

Jan 1, 1995

By C. J. Beyke

Slags and/or mattes from three secondary lead producers were studied as part of an effort to develop treatment methods for these lead-bearing residues. Each company used a somewhat different production process. Company A used a reverberatory furnace followed by a blast furnace. Company B used only a blast furnace. Company C used both a reverberatory and a blast furnace, and the scrap material was desulfurized with sodium carbonate prior to smelting. The slag matrix produced from sulfur-bearing scrap consisted mainly of iron-calcium silicates; the slag from desulfurized material was similar, but also contained sodium. In all the slags most lead was present in metallic form, often alloyed with tin, antimony, arsenic, and/or iron. Slag from Company B contained the most alloying elements, often as discrete subparticles within the lead droplets. Mattes were produced at Companies A and B; predominant phases were pyrrhotite and magnetite, while lead was present in metallic form and as galena.

Jan 1, 1995

By W. Zhao

Several years ago, Reddy and Blander presented upriori model for calculating the sulfide capacity of binary silicate melts. It is modified now to apply to CaO-AlO 1.5 melts at different temperatures and compositions. Our predictions are in very good agreement with the available experimental data. From a comparison of binary calcium aluminate and calcium silicate systems, higher sulfide capacities are obtained in aluminate systems. The sulfur can be removed from hot metal more effectively by adding aluminate melts.

Jan 1, 1995

By Marc Verhaege

The effluent under investigation results from a catalic oxidation unit in which paraxylene is oxydised to terephtalic acid. The solution contains cobalt and manganese as their acetates in a concentration range of 0,4 - 1,2 g/I of cobalt and 0,8 - 2,4 g/l of manganese. Before being fed into the main waste stream treatment unit of the plant it is advisable to apply a petreatment step in which both metals are eliminated to a great extent from this effluent. Conventional treatment is done by precipitation of both metals either through pH increment with a base or by adding a suitable reagent producing insoluble species. The aim of this study was to look for a treatment (elimination of both metal species) in which no sludge or precipitate is formed.

Jan 1, 1995

The direct removal of lead ions from D2EHPA-kerosene using metallic zinc as the reducing agent was evaluated. The electrochemical process, called galvanic stripping, is a potential alternative stripping technique when standard chemical methods are not adequate. Four parameters found to be important in the rate of lead removal were studied in a factorially designed experiment. The variable evaluated included D2EHPA concentration, temperature, zinc surface area and solution agitation. Temperature and surface area were found to be the most significant, while agitation and D2EHPA concentration had less influence on the reaction. An activation energy of 22.5 Kcal/mole was calculated indicating a chemically-controlled process. The reaction was also sensitive to the concentration of oxygen in the system. The zinc required was considerably in excess of stoichiometry, possibly due to the dissolution and redeposition of lead: In general, the results were encouraging and demonstrated that lead impurities could be removed from D2EHPA using cementation type reactions.

Jan 1, 1995

By C. Flores

A novel process using solid metals for the direct reduction of more noble metal ions from solvent extraction organics has been developed. Base metals recovery has been the principal focus of investigations to date but feasibility tests have now also been made on galvanically stripping selected precious metals. In this study gold (III) was loaded from an aqueous HAuCI4 .3H20 solution into a mixed organic 40 vol.% TBP, 10 vol. % D2EHPA in kerosene. The direct precipitation of metallic gold from the loaded organic phase using zinc powder and iron, aluminum and copper slabs at 70 °C was successfully demonstrated. The gold reduction rates were relatively fast even though the conductivity of the organic solutions is very low. The reaction rates were studied as a function of the variables zinc particulate size, oxygen and nitrogen atmosphere, water content in the organic phase, organic ratios and temperature. The gold morphology was usually powdery or dendritic in nature but continuous films were obtained in some instances. Activation energies were calculated and possible reaction mechanisms are discussed. In general, the results obtained were very promising and showed that gold can be successfully cemented from selected organic solvents by galvanic stripping using less noble solid metal reductants.

Jan 1, 1995

By Y. Ikeda

Typical electric appliances were dismantled into component pieces to study the recyclability of these discarded goods. Types and weight ratios of these component materials were investigated and characterized. The results showed that if they are dismantled properly, these goods could be classified into several groups of similar materials and/or structures, namely those consisting of single materials, metal-plastic combinations, metal-metal combinations and complex combinations of many different materials. By separating each combination into recyclable materials and isolating hazardous materials, it was found that the final waste for disposal could be reduced and the recycling efficiency could be improved markedly as compared to the conventional shredding method. The metal-metal combinations account for 60% by weight of the total metal contents in electric appliances, and therefore, it becomes important to segregate these metals. For the complex combinations, a process consisting of pyrolytic decomposition of plastic contaminants followed by smelting of the residue is proposed. It is anticipated that nearly zero-emission recycling of electric appliances will be achieved by applying this treatment process.

Jan 1, 1995

By Gus Van Weert

This paper describes the results of autoclave testwork where ferric nitrate was hydrolysed in the presence of certain cations and anions and the resulting hematite analyzed for foreign constituents. For the cations Zn++, Ni++, Cu++, and AI+++, selectivity factors of over 107 were found. Magnesium gave 3.106. These factors are calculated as Me/Fe in solution over Me/Fe in the hematite; Me representing the metal in ion added. As-a result of the testwork at Delft University of Technology, BUDELCO (the Netherlands electrolytic zinc producer) ran a series of ferric nitrate hydrolysis tests in the presence of 10 additional trace elements. Impurity levels were prejudiced on Me2 EPHA extraction of iron from their zinc circuit, followed by HNO3 stripping. Good selectivity against base metals was confirmed, but trace elements forming anions (As. Sb) and sulphate were incorporated in the hematite. These BUDELCO results are also presented.

Jan 1, 1995

By . Menad Gaballah I

Three samples of solid wastes generated by the non ferrous metallurgy were characterized. These residues contain up to 42 % of valuable metal compounds ( Cu, Pb and Zn ) and 23 %of toxic compounds t As, Hg, Cd and Se ). These sample were subjected to thermal treatments between 200 DC and 800 °C in controlled oxidizing. reducing and chlorinating atmospheres. Up to 99 % of As, Cd, Hg and Se were eliminated from these industrial wastes. Cu, Pb, and Zn compounds were concentrated in the treatments' residues of these samples. A Global Decontamination Factor' GDF ' was defined to measure the efficiency of the elimination of toxic elements and the recovery of valuable elements for a specific sample submitted to a given treatment. It seems that the thermal treatment in a reducing atmosphere was the most efficient in decontaminating these solids and the concentration of valuable elements. a.

Jan 1, 1995

By G. L. Watt

Fine sized titanium diboride (TiB2) powders have been synthesized in a thermal plasma reactor. Precursor for the synthesis were rutile, boron oxide, and methane. The effect of plasma gas type, precursor ratio, and input power on the synthesis was studied. The produced powders were characterized by X-ray diffraction and chemical analysis. The purified powders were CIP'd, HIP'd, sintered and characterized for porosity, hardness, and microstructure and the results compared with a commercially available TiB2 powder sample.

Jan 1, 1995

By M. S. Lee

A cold model study on the effects of various operating conditions on the dispersed-phase holdup in a liquid-liquid emulsion generated by bottom gas injection has been performed using water and kerosene. Dimensional analysis was used to correlate the holdup with the operating conditions and the sampling locations. The holdup increased with gas velocity, and decreased with axial and radial distances. The radial distribution of holdup follows a Gaussian function. The holdup increased with increasing ratio of the heavy phase to light phase volumes and decreased with the total height of the heavy phase. The combined effects of various operating conditions can be represented by the Froude number. The variation of the holdup within the plume was correlated by a single equation involving a set of dimensionless numbers.

Jan 1, 1995

By Masafumi Maeda

Our aim in this project was to develop a new copper refining technology utilizing pyrometallurgical treatment and a raw materials preparation technique. In the recycling process; raw material is not an idealized concentrate of copper sulfide but is composed of various types of scrap, industrial wastes such as sludge, ash and slag, and municipal wastes. Since we cannot expect oxidation heat in this process as in sulfide smelting, organic materials are viewed as an alternative energy source. Quality of the copper produced is targeted as 99.99% and an intermediate grade will also be marketable. To benefit the plant, rare metals and other nonferrous metals will also be recovered The overall system is described in this paper, specific topics outlined and preliminary research presented. Current Japanese technology for recycling copper based materials is briefly reviewed.

Jan 1, 1995

By J. Y. Hwang

Microwave heating is an attractive alternative to conventional heating methods because heat is generated directly within the microwave absorbing materials. It has potential to be utilized for selective heating and removal of specified components from a materials mixture. This investigation was undertaken to explore the potential of selective heating and burning of binders for foundry sand reclamation. Selected raw materials and binders used in foundry operations were tested to determine their receptivity to microwave heating. Time needed to reach 600°C and/or the maximum temperature achieved for samples irradiated by microwaves for twenty minutes under 800 W microwave power are reported. The microwave heating characteristics of the selected materials are summarized and discussed. The interactions between microwaves and the raw materials used in a foundry. such as silica sand. chromite sand and bentonite (clay) binder were studied. The results showed that chromite sand coupled well with microwave energy at ambient temperature while silica sand did not. This was expected because the major component of chromite sand. iron chromite (FeCr2O4). is a good microwave absorber. while quartz, which is the major component of silica sand, is a microwave transparent material at ambient temperature. Bentonite absorbs microwaves well because it contains a hydroxyl functional group and water molecules in its structure. It was found that the structure of bentonite was changed through microwave irradiation. Microwave heating characteristics of silica sand mixed with different amounts of bentonite binders were investigated. The presence of bentonite in the mixture improved the microwave heating of silica sand significantly. and bentonite was deactivated by the microwave processing.

Jan 1, 1995

By Maria K. Kojo

The interaction between various slags and a nickel concentrate containing pyrite, pentlandite, and violarite were investigated by submerging concentrate pellets in molten slags. The slags were contained in MgO-A12O3 spinel crucibles. The slag oxidizes the iron sulfides in the concentrate, resulting in a nickel matte. The amount of S02 gas formed during reaction was measured to determine the oxidation reactivity of the slags. The experimental variables included temperature, the ferric/ferrous ratio of slag, and other slag properties such as the FeO/SiO2 ratio and the MgO and NiO contents. The reactivity of the slag depended in a complex manner on its oxidizing power, viscosity, and interfacial tension. The slag composition for the greatest reactivity was determined to be Fe3+/Fe2+ = 0.3, Fe/SiO2 = 1.3, and % MgO = 2. This slag, however, caused substantial foaming. Increasing the MgO content to 10% or replacing it by 5% MgO + 8% NiO eliminated at a slight decrease in reactivity. The implications of the findings from this work in the bath smelting of nickel sulfide concentrates are discussed.

Jan 1, 1995

By Benjamin Vidales

Copper in concentrations above 0.5 weight percent in iron and steel causes hot shortness. This tendency is intensified in the presence of dissolved tin above 0.05 weight percent in the alloy. The understanding of the mechanism of removal of copper from molten iron and steel is of industrial importance. In this investigation, we present the experimental results of the removal of copper from molten iron using sulphide flux in the temperature range 1000°-1500°C. The solution thermodynamic properties of binary sulphide melts have been estimated by using the relevant phase diagrams and the behaviour of copper sulphide in these melts is discussed. The kinetics and thermodynamics of the removal reaction are also explained and, the experimental results are also reported showing the equilibrium distribution of copper and sulphur in molten iron.

Jan 1, 1995

By N. Kanarin

A thermodynamic study is reported on the chlorination of Fe(1-x.)O, Fe2O3, Cr2O3, MgO, Mg2SiO4 with chlorine in the presence or the absence of reducing atmospheres. The reactivities of these compounds as well as that of Mg3Si2O5(OH)4 using Cl2+N2, Cl2+air, and Cl2+CO gas mixtures were studied by non isothermal thermogravimetric analysis between 20 and 1000 °C. The same solids were chlorinated in a horizontal experimental set, during two hours between 350 and 1000 °C, in reducing and oxidizing atmospheres: The chlorination products were examined by XRD and SEM, and possible reaction paths were examined. Results indicate that the carbochlorination of these solids was better than their chlorination; Furthermore, the carbochlorination was performed at lower temperatures than those of the chlorination. Finally, the reaction extent was higher in the case of carbo-chlorination of these compounds. Based on these results, a process was suggested for the selective recovery of chromium compounds from the chromite concentrate.

Jan 1, 1995

By James P. Bennett

The U.S. Bureau of Mines, Tuscaloosa Research Center, is conducting a review of the usage of different types of refractories, the current industrial practices to recycle/dispose of spent refractories, and the concerns associated with these practices. This information will serve as the technical basis for initiating a research program to recycle or find alternate uses for spent refractory materials. Approximately 1.6 million metric tons of clay based and 1.2 million metric tons of non-clay based refractory materials were manufactured in the United States in 1992 alone, representing a value of almost 2 billion dollars. Landfill has been and remains the disposal means of choice. Issues such as environmental regulations, concerns over landfill disposal, future liability, and product stewardship programs have brought about increased emphasis for recycling or alternate material use. Information on refractory consumption and the issues associated with recycling or disposing of used materials will be discussed, including current recycling practices.

Jan 1, 1995

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 Michael Meyer

In the past shredder fluff was discarded in landfills, but shrinking landfill space and the partly hazardous content of the fluff as well as its caloric value, all resulted in efforts to turn this waste problem into a an energy resource. In order to produce a fuel, the inorganic compounds have to be removed. Extensive analyses and particle size measurements were made on fluff from various shredder. For optimal separation all particles are reduced to a uniform, relatively small size. In a subsequent combined - screening and air classification - process, successful separation into organic and inorganic fractions is achieved. The inorganic fraction is treated in a heavy media or an eddy-current separator to recover the valuable metals, while the organic fraction is now suitable for thermal processing, such as fluidized bed gasification and using the resulting carbon as a chemical reagent.

Jan 1, 1995

By R. P. King

The essential features of an image analysis system for the measurement of mineral liberation are described. Good procedures for image acquisition and image processing prior to image analysis are defined. The basic stereological methods for the measurement of volume fraction, surface area per unit volume, particle size distribution and liberation spectra are given. The appropriate methods for fractal correction when measuring perimeters of irregular features and for frame correction when measuring linear intercepts are developed. Practically useful and accurate procedures for the stereological correction of particle size and liberation distribution methods are given.

Jan 1, 1995