The disintegration of agglomerates of solid charge used in a nickel flash furnace has been investigated. The in-flight agglomerate size of solid charge with different characteristics has been measured using turbulent conditions similar to a full-scale flash furnace. Plant observations indicated that under certain conditions solid charge was able to pass through the furnace shaft unreacted. The motivation for this work was to improve the understanding and the modelling of a flash furnace. A review of the literature revealed that the disintegration of agglomerates of solid charge is very important to the performance of a flash furnace, however, there has been no detailed study of the factors governing the disintegration of in-flight agglomerates of solid charge.A laboratory-scale experimental rig was constructed to non-intrusively measure the in-flight agglomerate size distribution of solid charge and to visualise the powder injection process, while using turbulent conditions similar to a flash furnace. A high-speed video technique and a laser diffraction technique were used to measure the wide range of in-flight agglomerate sizes present during powder injection. A range of variables including the particle size, turbulence level, packing density, particle shape, solid concentration, and moisture content were investigated.

The disintegration of agglomerates of solid charge used in a nickel flash furnace has been investigated. The in-flight agglomerate size of solid charge with different characteristics has been measured using turbulent conditions similar to a full-scale flash furnace. Plant observations indicated that under certain conditions solid charge was able to pass through the furnace shaft unreacted. The motivation for this work was to improve the understanding and the modelling of a flash furnace. A review of the literature revealed that the disintegration of agglomerates of solid charge is very important to the performance of a flash furnace, however, there has been no detailed study of the factors governing the disintegration of in-flight agglomerates of solid charge.A laboratory-scale experimental rig was constructed to non-intrusively measure the in-flight agglomerate size distribution of solid charge and to visualise the powder injection process, while using turbulent conditions similar to a flash furnace. A high-speed video technique and a laser diffraction technique were used to measure the wide range of in-flight agglomerate sizes present during powder injection. A range of variables including the particle size, turbulence level, packing density, particle shape, solid concentration, and moisture content were investigated.

The sulphation and sulphate decomposition occurring during the oxidation of nickel concentrates were studied by thermal analysis. Samples of industrial nickel concentrates were heated in inert gas to temperatures between 400°C and 850°C and oxidized isothermally in air or in a 4%O2-96%N2 mixture. During isothermal oxidation of the concentrates, SO2 evolved from the roasting reactions led to partial formation of metal sulphates. Following the oxidation and sulphation of the sample, the decomposition of the formed sulphates was studied. This was completed either by heating the sulphated sample to 950°C to thermally decompose the sulphates, or by lowering the partial pressure of oxygen while holding the sample at the isothermal oxidation temperature. The sulphation of the sample was found to follow the parabolic rate law, implying diffusion as the rate controlling-step. The thermal decomposition of the sulphates occurred at a near constant rate, implying zero-order kinetics.

The sulphation and sulphate decomposition occurring during the oxidation of nickel concentrates were studied by thermal analysis. Samples of industrial nickel concentrates were heated in inert gas to temperatures between 400°C and 850°C and oxidized isothermally in air or in a 4%O2-96%N2 mixture. During isothermal oxidation of the concentrates, SO2 evolved from the roasting reactions led to partial formation of metal sulphates. Following the oxidation and sulphation of the sample, the decomposition of the formed sulphates was studied. This was completed either by heating the sulphated sample to 950°C to thermally decompose the sulphates, or by lowering the partial pressure of oxygen while holding the sample at the isothermal oxidation temperature. The sulphation of the sample was found to follow the parabolic rate law, implying diffusion as the rate controlling-step. The thermal decomposition of the sulphates occurred at a near constant rate, implying zero-order kinetics.

Selective oxidation and sulfation roasting of nickel concentrate followed by leaching was investigated as a novel route for nickel production. In the oxidation roasting stage, the iron species in the nickel concentrate was preferentially oxidized to form iron oxides, leaving non-ferrous metals (Ni, Cu, Co) as sulfides. The roasted product was then sulfation roasted to convert the sulfides of the latter metals into water-soluble sulfates. The sulfates were then leached into solution for further recovery and separation from iron oxides. The oxidation of nickel concentrate was firstly studied by means of thermogravimetric and differential thermal analysis over a wide temperature range. A reaction scheme was deduced, in which preferential oxidation of iron sulfide species occurred over a wide temperature range up to about 700 ºC, forming a Ni1-xS core with iron oxide shell. A batch fluidized bed roaster was then constructed to study the oxidation and sulfation roasting of nickel sulfide concentrate. Oxidation roasting tests were carried out at temperatures between 650 °C and 775 °C. It was found that low temperatures (e.g. 650 °C) are favorable for the preferential oxidation of iron sulfide species while minimizing the formation of nickeliferous oxides, i.e. trevorite and NiO. Several parameters were varied in the sulfation roasting experiments, including the sulfation gas flowrate, sulfation roasting temperature, the addition of Na2SO4, sulfation roasting time, and the oxidation roasting temperature. Under optimized conditions of sulfation gas composition (95% air, 5% SO2), temperature (700 °C), Na2SO4 addition (10 wt%) and time (150 min), the conversions to sulfates were 79% Ni, 91% Cu, and 91% Co. Only 5% Fe forms water-soluble sulfate. The residue from the leaching of calcine in water contained 49% Fe and 10% Ni, which is a suitable feedstock for the production of ferronickel alloys. Therefore, further studies were also conducted to evaluate the reduction behavior of the residue with CO, H2 and graphite.

Non-oxidative acid leaching of pyrrhotite from Kevitsa’s Ni-concentrate and methods to recover by-products, have been investigated. Selective dissolution of pyrrhotite (Fe1-xS, 0<x<0.25) can enrich the content of the valuable metals, such as Ni and Co, in the final concentrate and will reduce the amount of Fe and S sent to the smelters. The pyrometallurgical smelting of leached concentrate will thus give less formation of smelter by-products in form of slag and SO2. The leaching was studied through an experimental design plan with parameter settings of  38.8% to 57.8% H2SO4 and temperatures from 60 to 100°C. The best results were obtained in experiments carried out at the lower experimental range. Leaching at 60°C with an initial acid concentration of 38.8% H2SO4 was found sufficient to selectively dissolve most of the pyrrhotite; leaving an enriched solid residue. A QEMSCAN analysis of the solid residue confirmed that most of the pyrrhotite had been dissolved and showed that pentlandite was still the main Ni-mineral. Chemical assays showed that more than 95% of the Ni, Co, and Cu remained in the final residue.    The utilized leaching process generates by-products, in the form of large quantities of Fe2+ in solution and gaseous H2S. To recover Fe2+, crystallization of iron(ii) sulfate (FeSO4∙nH2O) from leach solution through cooling have been studied. The crystallized crystals were further dehydrated into the monohydrate (FeSO4∙H2O) through a strong sulfuric acid treatment (80%H2SO4). XRD analysis confirmed that FeSO4∙H2O was the main phase in the final crystals, and a chemical analysis showed a Fe content of about 30%, 1.5% Mg, 0.4% Ca, and 0.2% Ni.    The possibility to leach the concentrate by circulating the acidic solution from the crystallization stage has been tested. The recirculation of the solution showed no negative effects, as the recoveries of elements and chemical assays of the final solid residue were found to be similar to the obtained assay when the concentrate was leached in a fresh solution. / Icke-oxidativ syralakning av magnetkis från Kevitsas Ni-koncentrat har studerats samt metoder för tillvaratagande av biprodukter. Genom en selektiv upplösning av magnetkis (Fe1-xS, 0<x<0.25) kan värdefulla metaller som Ni och Co anrikas i det slutliga koncentratet. Samtidigt som mängden Fe och S som skickas till smältverken minskar, vilket också innebär att mindre biprodukter i form av slagg och SO2 erhålls vid den pyrometallurgiska smältningen av Ni-koncentratet. En experimentell design plan genomfördes för att studera lakningen där syrakoncentrationen varierades från 38.8% till 57.8%H2SO4 och temperatur från 60 till 100°C. Bäst resultat erhölls vid de lägre parameterinställningarna. Lakning vid 60°C med en initial syrakoncentration på 38.8%H2SO4 visade sig vara tillräcklig för att selektivt lösa upp merparten av all magnetkis och lämna kvar en anrikad produkt. Via QUEMSCAN bekräftades att merparten av all magnetkis hade löst upp sig och att huvudsakligt Ni-mineral fortfarande var pentlandit. Kemiska analyser visade att mer än 95% av Ni, Co och Cu stannade kvar i fasta godset.    Den tillämpade lakningsmetoden genererar biprodukter i form av stora mängder Fe2+ i lösning och H2S i gasform. För att tillvarata Fe2+ har kristallisering av laklösning som järn(ii) sulfat (FeSO4∙nH2O) studerats genom kylning. De kristalliserade kristallerna avvattnades till monohydrat, FeSO∙1H2O, genom avvattning i stark svavelsyra (80%H2SO4). XRD bekräftade FeSO∙1H2O som huvudfas i slutliga kristallerna och kemisk analys visade på ca 30%Fe med huvudsakliga orenheter i form av 1.5% Mg, 0.4%Ca och 0.2% Ni.    Möjligheten till att laka i återcirkulerad lösning efter kristallisering har undersökts. Lakning i återcirkulerad lösning visade inga negativa effekter då liknande halter och utbyten erhölls till det fasta godset.