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By Sue Xue, Carl C. Nesbitt

A project was completed which investigated the efficacy of recycling lead or lead monoxide from various fire assay wastes including crucibles, cupels and slag. The scope of the project was to determine optimal hydrometallurgical parameters so that direct separation and recovery of lead salts was economically feasible. A process was developed from the study which could use either acetic acid or nitric acid as a leachant, followed by several precipitation processes which could directly recover litharge (PbO) or other lead salts, such as lead carbonate or lead sulfate. The economics of the process is discussed. Analytical equipment such as the atomic absorption spectrophotometer and x-ray diffractometer supplied much of the information required for the study. However some novel analytical approaches using these instruments had to be developed to help in the determination of leaching kinetics and process quality control which are discussed.

Jan 1, 1999

By Kirsi M. Riihilahti

The oxidation characteristics of solid copper matte particles under simulated Kennecott-Outokumpu Flash Converting conditions are presented. The effects of feed matte grade, matte particle size, oxygen-to-matte mass ratio, oxygen content of the process gas and temperature on the particle oxidation rate, quality of conversion, particle size change and particle morphology were determined. The converting quality was highest (~68) with the 58% copper matte at 1100°C. At similar conditions, the 72% copper matte was more likely to produce copper oxides and leave unoxidized particles rather than directly produce sulfur dioxide at 1100°C, resulting in an average converting quality of 55. The quality of conversion was poorest for the 72% matte at 920°C (~45); the sulfur removal was extremely low even with a relatively high degree of oxidation. Fragmentation of the particles was significant in all cases with the 72% matte. A higher O2/matte .ratio and higher temperature, in general, resulted in increased fragmentation while oxygen enrichment had no significant effect. With the 58% matte, particle size was found to increase for the finest fractions rather than to decrease due to particle expansion.

Jan 1, 1998

By Nobuo Kikumoto

Recently, the treatment of industrial waste materials has been a serious social problem here in Japan. Filling them in ponds is now strictly prohibited due to a limited land area and incineration method is also regulated as not to generate DXN. In these conditions, Onahama Smelter has begun to treat shredder dusts (SD) of car at reverberatory furnaces to recover various metals such as copper, gold, silver and palladium without generation of DXN. The total volume of these dusts is expected more than 1 million metric tonnes a year in Japan. Onahama Smelter is now planning to treat about 20% of them in the near future by using tonnage oxygen. In this paper, the heat balance, control method of DXN and treatment of these dusts in reverberatory furnaces are described. DXN : Dioxin (The generic term of PCDD and PCDF)

Jan 1, 2000

By William Petruk

The primary requisite for a successful extractive metallurgy operation is to grind an ore fine enough to liberate the minerals so that they can be concentrated, or to expose mineral surfaces so that the minerals can be leached. The ease or difficulty of liberating or exposing the mineral grains is dependent upon the mineral textures such as grain size, crystallinity and bonding between mineral grains. In particular, mineral grains with straight grain boundaries and a weak bonding to other minerals are easily liberated and readily concentrated into high grade concentrates. In contrast mineral grains that have re-entrant boundaries and are strongly bonded to their neighbours are not easily liberated and will not produce high grade concentrates, even with regrinding. Similarly, inclusions that occur along fractures and grain boundaries can be readily exposed and leached. Whereas minute random inclusions in large grains will not be liberated or exposed unless they occur along planes of weakness.

Jan 1, 1995

By Bingchen Chen, Zhitong Sui, Junwei Ma

"In the blast furnace slag, titanium disseminated in various mineral phases Titanium could be concentrated mainly in perovskite, which could be selectively precipitated and grown by optimizing the operation factors like the slag composition, temperature of heat treatment and additive agents. This study aims at establishing the titanium slag mineralogy and its distribution in the treated slag and the as-received slag, as well as the methods of perovskite separation. After heat treatment, the grain size was grown from 5 - 20µm to 80 - 200µm, the distribution of Ti02 in perovskite was increased from 48% to 81 %, the morphology was changed from snow-shaped grain to coarsening dendrites or equiaxed crystals. A concentrate were produced by gravity separation analyzing 35.25% Ti02 with a recovery of 68.28% and a tailing analyzing 9.53% Ti02 , and a possibility of flotation upgrading was discussed. I INTRODUCTION CHINA is rich in mineral resources of titanium, 92.4% of which is vanadium-titanium bearing magnetite. About 53% titanium were in iron concentrate after mineral processing, by which the blast furnace slag containing about 25% TiO2 were produced[11 • The content of TiO2 in such slag is too low to separate titanium dioxide, and it is also too high to produce slag cement[21. It has been accumulated to 50 million tons so far, which is still increasing at a rate of 3 million tons per year, and results in a waste of titanium resources and pollution of environment. Due to the dispersed distribution of titanium component in various mineral phases, very fine grain(<10µm) and complex interfacial combination, it is very difficult to recovery titanium component from the slag by traditional separating technique. In this paper, a novel technique to recovery titanium from the waste slags was proposed [3H4l, on which three continuous processes were involved: selective concentrating, selective growing and selective separating. Perovskite was designed as a titanium-rich phase, in which the most titanium was concentrated promptly, then perovskite could be selectively grown and coarsened by optimizing the heat treatment and the appropriate additives [ 5l[6l. The grain size of perovskite phase was larger than 80 µm, and the crystals appeared as coarsening dendrites or equiaxial grains like lump."

Jan 1, 2000

By Gary R. Adams

Coating thickness control is typically difficult with touch-up solders for galvanized steel, and corrosion properties and abrasion resistance are sometimes poor. This paper reports on progress in ILZRO-sponsored research to develop an improved touch-up solder. Encouraging results were achieved in torch soldering trials with zinc-tin based alloys. Mouldability and coating thickness control were achieved over a practical working temperature range in which the solders consisted of a viscous mixture of solid primary zinc phase particles in a liquid zinc-tin eutectic matrix The mouldability was dependent on the microstructure of the starting material, and optimum structures could be obtained through control of casting solidification rates and/or by the addition of small amounts of copper. Hardness and preliminary corrosion test results showed potentially good mechanical and corrosion behaviour. The absence of toxic materials ensures environmental friendliness. Comprehensive performance testing is continuing on selected experimental zinc-tin-copper touch-up solders.

Jan 1, 1992

By D. J. Droppert

This paper describes the precipitation-production of crystalline scorodite (FeAs04.2H20) from arsenic-rich sulphate-based metallurgical solutions at ambient pressure (95°C). Arsenic is precipitated by means of a controlled precipitation technique in which the supersaturation of the solution is carefully controlled. By controlling the supersaturation in the presence of seed material. the formation of amorphous ferric arsenate is prevented. Scorodite is known to be the most stable As(V) compound and is therefore preferred as host mineral for arsenic immobilization. The effect of the following parameters on the preCipitation behaviour and kinetics of scorodite are discussed: Type of base seed concentration initial [As]. sulphate concentration. neutralization rate. seed recycling and method of Fe(ll!) addition to Fe-deficient arsenic solutions.

Jan 1, 1996

By Ann M. Hagni

The mineralogical, chemical, microtextural, and particle size character of electric arc furnace (EAF) dusts are being studied by reflected light microscopy, scanning electron microscope-energy dispersive spectroscopic analysis (SEM-EDS) and electron probe microanalysis (EPMA). The dusts consist predominantly of metallic iron, iron oxide, and calcium-iron-manganese silicate phases, together with smaller amounts of iron-manganese-zinc-calcium, iron-calcium-zinc-manganese, and calcium-iron-manganese silicates. The samples vary in their zinc contents. Chlorine occurs in phases containing iron, lead, zinc, manganese, and calcium. The dust particles range greatly in size from 1 to more than 300 ~m, but most particles are about 1 to 6 ~m. Larger particles. about 20-50 um across. also are present. They are predominantly spherical in shape, but some are cenospheres, and others are more angular particles, some of which are broken spheres and cenospheres. Their internal microtextures exhibit evidence of liquid immiscibility, exsolution, skeletal crystal growth, and oxidation react i on rims. Because EAF dusts have been classified by EPA as hazardous wastes, there is heightened interest in the treatment of these dusts to render them non-hazardous. The mineralogy of products of pyrometallurgical treatment of EAF dusts by flash furnace and pyrohydrolysis are currently under study.

Jan 1, 1991

By Steven R. Pittman, Colin McCullough, Peter Galuska

"Traditionally Continuous Fiber Aluminum Matrix Composites have been fabricated using high strength fibers and high strength matrices, often commercial alloys, with the goal of producing high strength composites. However the specific role of the choice of matrix alloy on composite properties has not been well established. One way to control composite tensile strength is to use coatings to introduce a low strength interface between fiber and matrix which tends to reduce the importance of the matrix selection, but unfortunately renders the transverse strength unacceptably low. Thus using a system with strong bonding between fiber and matrix is desirable, such as an alumina fiber / aluminum alloy matrix system. In this case the transverse strength is a strong function of the matrix strength. However the longitudinal strength then depends largely on the characteristics of the matrix. The important role of the matrix is discussed using examples of alumina fibers in various aluminum alloy matrices. The key attributes are matrix constituent phases, alloy chemistry, alloy reactivity with the fiber, and matrix strength. From the understanding developed in these systems a set of design rules may be established for selecting an optimum matrix. IntroductionAluminum matrix composites (AMC's) reinforced with continuous fibers offer very attractive property gains over AI alloys, such as strength, stiffness, and fatigue resistance. These gains are magnified when specific mechanical properties are compared which make them attractive candidates for replacing steel, nickel, titanium and aluminum alloy parts in weight critical applications (1). Many systems have been tried in the past; B/AI, C/AI, SiC/AI, Si-Ti-C-O/AI and AI203/AI. Technically B/AI was a very good system but was expensive in regard to both fiber cost and fabrication and SiC/AI and C/AI systems are still plagued with reactivity problems. The Si-Ti-C-O/AI appears to be a good strength system but with lower stiffness. Until recently, the AI203/AI was a low strength system, in part due to a lack of a high strength fiber. Recently 3M introduced a high strength AI203 fiber - Nextel™ 610, which leads to high strength composites (1,2) and may also be both low cost and also compatible with less expensive casting approaches for fabrication."

Jan 1, 1996

By Lawrence L. Brown

As part of the Federal effort to help maintain an adequate supply of fertilizer materials, the Bureau of Mines conducted research to characterize complex low-grade Michigan phosphate materials and to devise methods for recovering fertilizer-grade phosphate concentrates. The rock is from middle Precambrian sedimentary formations in the Marquette Range located in the central part of the Upper Peninsula of Michigan. Occurrence of phosphate-bearing sediments in Precambrian rocks is rare. This deposit, containing 12 to 15 pct P2O5 is believed to be the richest Precambrian phosphate deposit in the United States. Petrographic examination showed that the conglomeritic rock contains crystalline apatite both in "black pebbles" and in quartz matrix. Attrition scrubbing and sizing tests showed that there is no tendency for phosphate to concentrate in any of the sized fractions. In beneficiation tests, which included grinding to minus 325 mesh followed by phosphate mineral flotation using a fatty acid-fuel oil collector, a phosphate concentrate was obtained that had a grade of 30 pet P2O5 and a P2O5 recovery of 72 pct. This concentrate should be suitable for fertilizer manufacture.

Jan 1, 1982

By Niko Hellstén

To capture efficiently the valuable trace metals from nickel slag using electric furnace, it is important to study their distributions between the slag and metallic phases in the furnace. It is impossible to calculate accurately these distributions without experimental measurements. Therefore, in this work, selected trace metal distributions and phase equilibria between K2O containing iron-silicate slags and a metallic Ni-Fe-Cu alloy in nickel slag cleaning furnace conditions were studied. The experimental method developed and applied during the work, involved a modified quenching technique that included equilibration of the samples in semi-sealed quartz ampoules in an inert atmosphere and metallic Fe saturation. The use of the semi-sealed quartz ampoule prevents the escape of volatile elements from the sample during equilibration. Chemical compositions of the phases and the trace elements were analysed by EPMA. From the measured compositions, the trace metal distribution coefficients between the molten Ni-Fe-Cu alloy and slag were calculated.

By Ibrahim Yusufoglu, Ahmet Orkun Kalpakli, Cem Kahruman, Sedat Ilhan

"The effects of oxalic acid concentration, temperature, stirring rate and particle size on the dissolution rate of synthetically prepared calcium molybdate were investigated. Dissolution of calcium molybdate in oxalic acid solutions takes place as a series - parallel type reaction. In the first reaction step, which proceeds according to the ""Langmuir - Hinshelwood Mechanism"", calcium aqua oxalato molybdate is formed as a complex chelate intermediate product. In the second reaction step, molybdic acid is formed during the slow hydrolysis of calcium aqua oxalato molybdate, and it reacts rapidly with oxalic acid to form the polymeric hydrogen oxalate dimolybdate chelate as an end product. Activation energies were calculated as 41.4 and 49.9 kJ mol-1 for the first and zero order reactions. The fractional conversion versus time relationship can be given by the following equation.IntroductionMolybdenum is used widely in electric-electronic, metal working, aerospace and aeronautic, nuclear, glass and petrochemical industries because of its high melting temperature and resistance against chemical effects. However, the largest molybdenum consumers are the iron-steel and super alloy industries where molybdenum is used as an alloying element. Industrially important molybdenum minerals are limited to molybdenite (M0S2), powellite (CaMo04) and wulfenite (PbMo04), which are considered as primary molybdenum resources. Secondary molybdenum resources are spent catalysts and scrap [1-4].Molybdenum has been produced by pyrometallurgical processes in the past. Since it is possible to process low grade molybdenum ores and industrial wastes by hydrometallurgical processes, which are more environmentally friendly than pyrometallurgical processes, the importance of the use of hydrometallurgical processes has increased in the molybdenum production industry."

Jan 1, 2012

By W. R. McDonald

The U.S. Bureau of Mines investigated treatment of gold and silver refractory ores and concentrates that respond poorly to conventional cyanidation techniques due to the complex mineralogy of the ore. Three types of ores were investigated: gold locked placer sands, gold locked in sulfides, and gold that is robbed from the pregnant cyanide solutions by minerals in the ore. Ore treatment included grinding, flotation, cyanidation, air oxidation, pressure oxidation, hypochlorite oxidation, roasting, and carbon in leach.

Jan 1, 1991

By A. K. Kyllo

A study has been carried out on the dusts from Hudson Bay Mining and Smelting&apos;s Flin Flon copper smelter. The aim of the work was to determine the mechanisms of dust formation and the deportment of the various constituents. The work concentrated on the copper converters, but the electrostatic precipitators and baghouse also clean the reverberatory furnace off gas, so some mixing will have occurred. The dust composition was found to vary with distance from the furnace, and to be made up of three major components: solidified droplets, unreacted flux, and condensed particles. The solidified droplets were formed from material ejected from the converter during blowing, while the flux was blown out of the converters immediately after charging. The condensed particles contained the majority of the lead and zinc, as well as the volatile impurities. There was also a significant soluble content of the dusts, increasing with distance from the furnace. The condensed material may be separated from the remainder by a simple washing and sizing technique.

Jan 1, 1996

By Roger Altman

The solubility of copper in primary spinel crystals encountered in reverberatory slag samples has been determined by electron microprobe analysis. These spinels, which ranged in composition from 22% A12O3 to pure magnetite, contained small quantities of dissolved copper (0-0.4%). Based on literature data it was estimated that the solubility limit of copper in solid magnetite is no greater than about 1% at 1200°C and about 2% at 1250°C. However, it was found that practically every spinel crystal examined contained significant amounts of matte inclusions. Further examination of converter slag revealed large quantities of irregularly shaped precipitated magnetite crystals which contained a large proportion of copper inclusions. Additional experimentation showed that the total copper content in reverberatory slag samples was greater than the sum of the estimated en- trained plus dissolved matte in the slag. This difference is believed to be significant and is due to the presence of matte inclusions in the spinel crystals. In the present reverberatory slag samples these inclusions accounted for about 1/2 of the amount of sulfide directly entrained in the slag.

Jan 1, 1976

By Steve Lloyd, Ryan J. Foy, Brandon Steinborn, Jerome P. Downey

Research was performed to evaluate copper and silver extraction from samples of bornite flotation concentrate. Sulfation roasting experiments were performed in a rotary tube furnace, a fluidized bed reactor, and a static bed muffle furnace. Roasting was plagued with rapid, lowtemperature calcine sintering, apparently related to the presence of organic matter in the concentrate. Calcine entered a weak acid leaching process to remove copper, and silver was extracted from the weak acid leach residue in a ferric chloride and hydrochloric acid solution. Copper extraction efficiencies in excess of 90% were attained in the weak acid leach while 90% silver extraction was achieved in the ferric chloride leach, along with copper and lead extractions as high as 93% and 99% respectively. The two-stage leaching process resulted in overall extraction efficiencies of 99% copper and 90% silver.

Jan 1, 2015

By N. Kanari

One of the criteria to define the market value of chromite concentrate is its chromium to iron ratio. Changing this ratio for a definite chromite mineral is impossible by physical processing. This study investigated the possibility of increasing this ratio through the carbochlorination and the oxychlorination of chromite concentrates. Experiments are carried out up to 1000 °C. The characteristics of samples and reaction products are determined by SEM, XRD and chemical analysis. The carbochlorination of a chromite concentrate at about 600 °C leads to the . selective partial elimination of iron allowing a higher Cr/Fe ratio of the treated concentrate. Selective extraction of iron could also be achieved at about 950 °C by oxychlorination. In this case, a part of chromium contained in the concentrate is recovered as chromium oxychloride. The obtained residue had high content of Cr, Mg and A1 oxides. Such material has probably better chemical and thermal properties that may. be useful for foundary and refractory applications. Two flow-sheets for the beneficiation of the chromite concentrates using carho- and oxychlorination are suggested.

Jan 1, 1997

By Mikiya Tanaka

This paper outlines our attempt to establish a recycle process of nickel in the spent baths and waste rinse water of electroless nickel plating plants using solvent extraction and solvent-impregnated support, Solvent extraction studies of nickel from actual spent baths revealed that (i) nickel is efficiently extracted by a hydroxyoxime extractant such as LIX84I at a pH greater than 6 and is readily stripped with sulfuric acid, and (ii) the mixtures of LIX63 and acidic organophosphorus extractants (D2ERP A, PC88A, and Cyanex 272) enhanee the nickel extraction efficiency to a sufficient degree without pH adjustment, but at the same time, reduce the stripping efficiency. The application of acidic organophosphorus extractants to selectively remove impurity metal ions (iron and zinc) from a real spent bath before extracting nickel lead to the finding that PC88A and Cyanex 272 effectively remove iron and zinc without pH adjustment leaving nickel in the raffinate. The removal of nickel from the waste rinse water was also studied. Solvent-impregnated supports with a macroporous resin and oil sorbents made of natural kapok fiber and synthetic fiber as supports were applied using D2EHPA and LIX860 as the extractants. During the batch operation, nickel is removed with a high efficiency without pH adjustment. During the column operation, however, the effective removal is hindered by (i) the dissolution of the nickel-D2EHPA complex into the aqueous phase in the high loading region, and (ii) the slow removal rate of the LIX860-impregnated support.

Jan 1, 2003

By John M. Gaines

Lead concentrates from the Viburnum Trend in Southeast Missouri are sintered, prior to smelting, to bind the particles together, homogenize the feed, and reduce the sulfur content. About 20% of the sinter at some plants is classified as bad sinter. A total of 130 samples of good and bad sinters were studied by reflected light microscopy, scanning electron microscopy-energy dispersive analysis, and electron microprobe analysis to characterize their differences in mineralogy and textures. Good sinters consist predominantly of hardysonite, franklinite, lead silicate matrix, and large crystals of calcium-magnesium-iron silicate, together with minor amounts of lead oxides, lead-zinc silicate, metallic lead, specular hematite, magnetite, lead-iron-bearing zincite, and zinc-lead-magnesium-bearing wustite in a tightly intergrown mesh of crystals and with an evenly distributed porosity of about 15-20%. Bad sinters contain larger amounts of lead silicate matrix, galena, metallic lead, and lead oxides, but smaller amounts of hardysonite, franklinite, and calcium-magnesium-iron silicate, lack intimate intergrowth of the phases, and have lower (0-5%) and unevenly distributed porosity.

Jan 1, 1992

By C. Koopman

During the production of phosphoric acid from phosphate ore and sulfuric acid, large amounts of calcium sulfate are formed, in which impurities from the feedstock are incorporated. To use the calcium sulfate in, for example, the building industry, a lower concentration of impurities is desired. Mercury, copper, lead, and cadmium were extracted from clear industrial recrystallization acid (0.8-3.9 mol/kg H3PO4, 0.2-0:5 mol/kg H2SO4) by supported solvent extraction with the extracting agent Cyanex 302 in kerosene in a transverse flow hollow fiber module. The permeability for the mercury ion was 1.4.10-6 m/s, whereas that for the copper ion was calculated to be 1.5.10 m/s. Cadmium, lead, and copper were extracted during the recrystallization of calcium sulfate hemihydrate to dihydrate, an existing step within the ,phosphoric acid production process, by solvent extraction with the same extracting agent. The concentrations of cadmium and zinc in the newly formed calcium sulfate were proven to be decreased. Unfortunately, concentrations of mercury and lead were too low for analysis.

Jan 1, 1999