Characterization of limonitic laterite and solids during sulfuric
- 格式:pdf
- 大小:545.60 KB
- 文档页数:3
Technical NoteCharacterization of limonitic laterite and solids during sulfuric acid pressure leaching using transmission electron microscopyD.Georgioua,*,V.G.PapangelakisbaDepartment of Environmental Engineering,Demokritos University of Thrace,Xanthi 67100,GreecebDepartment of Chemical Engineering and Applied Science,University of Toronto,200College Street,Toronto,ON,Canada M5S 3E5Received 22May 2003;accepted 26October 2003AbstractThis technical note summarizes the results from a mineralogical analysis of limonite and the solids produced during sulfuric acid pressure leaching,using transmission electron microscopy.The elemental composition was revealed by means of X-ray analysis while the crystallographic characterization was obtained using electron diffraction.Iron in the form of goethite (a -FeOOH)was the dominant phase of limonite forming needle-shape particles rich in nickel while aluminum existed mainly in gibbsite (Al(OH)3)particles.Cobalt was found to be associated with a manganese phase rich also in nickel.No structural changes were observed during heating the limonite slurry up to 270°C and before acid injection.Both Ni and Co were highly leachable in the manganese phase during sulfuric acid pressure leaching of the limonite.Ni was also highly leachable in the magnesium silicate structures that were present in minor amounts.Hematite was the only precipitation phase of iron forming spherical particles of a size of 0.1–0.3l m while;alunite was the only precipitation phase of aluminum.Ó2003Elsevier Ltd.All rights reserved.Keywords:Extractive metallurgy;Hydrometallurgy;Leaching;Mineral processing;Ore mineralogy1.IntroductionNickel and cobalt extraction using sulfuric acid pressure leaching of limonitic laterites has become increasingly important the recent years.In depth min-eralogical analysis of limonitic laterite and the solids formed during leaching is crucial to the understanding of the physicochemical nature of leaching and the deri-vation of nickel and cobalt dissolution kinetic models.Transmission electron microscopy proved a very useful tool for the implementation of the above purpose.2.Experimental2.1.MaterialsA limonitic laterite was utilized with the following elemental analysis:47.7%Fe, 3.13%Al, 1.47%Ni,0.12%Co and 0.67%Mg.2.2.LeachingLeaching tests were performed using an acid leaching pilot-plant that employed continuously agitated reac-tors in the form of a multi-compartment horizontal autoclave.The leaching conditions were pulp density:30%,temperature:270°C and acid to ore ratio:0.2.Samples from the solids during heating of the slurry and before acid injection were withdrawn at 165,225and 270°C.Following acid injection,solids were also withdrawn from the first compartment of the autoclave.2.3.Transmission electron microscopyAnalysis of the samples took place utilizing a Transmission Electron Microscope (Philips EM 430)operating at 100kV.High magnification and resolution photos of the solids were obtained by the use of the above technique.The elemental composition of the solids was revealed using X-ray analysis while the min-eralogical composition was obtained using electron dif-fraction analysis.*Corresponding author.Tel.:+30-2541-28865;fax:+30-2541-79376.E-mail address:dgeorgio@env.duth.gr (D.Georgiou).0892-6875/$-see front matter Ó2003Elsevier Ltd.All rights reserved.doi:10.1016/j.mineng.2003.10.015Minerals Engineering 17(2004)461–463This article is also available online at:/locate/mineng3.Results and discussion 3.1.LimoniteThe iron phase of goethite was found to be the dominant phase of limonite.Images of goethite at low and high magnification are shown in Fig.1.Goethite forms needle-shape particles rich in Ni while;Al and Cr constitute also part of the goethite lattice.Aluminum exists mainly in the form of relatively big gibbsite particles while cobalt was found to be associ-ated only with a manganese phase of a poor crystallin-ity.The latter phase was also rich in Fe and Ni;Al also existed in minor amount.Electron diffraction analysis also revealed the pres-ence of silica in significant amounts,chromite rich in aluminum,amorphous magnesium silicate structures rich in Fe and Ni in minor amounts and finally,mag-netite also in minor amounts.Table 1summarizes the main elements and the respective mineralogical phases found in limonite.3.2.Solids before acid injectionSolids were withdrawn during heating of the slurry at 165,225and 270°C.All the above mineralogical phases were also found in these samples.No elemental or structural change was observed in any mineralogical phase during heating of the limonitic slurry.3.3.Leaching solidsA sample from the first compartment of the autoclave was withdrawn during leaching.The dominant phases of this sample were goethite and hematite,which was theonly precipitation phase of iron.A low and a high magnification photo of a mixture of goethite with hematite particles are shown in Fig.2.Hematite formed spherical particles of a size of 0.1–0.3l m.Alunite was the only precipitation phase of alumi-num.Alunite was found to form big structures as the ones shown in Fig.3(some hematite particles were also entrapped).Chromite and silica particles were found unchanged however,magnesium iron silicate structures were found depleted of Ni;nickel in this phase proved highly leachable.Finally,nickel and cobalt also proved highly leachable in the manganese phase too;manganese structures were identified depleted of both Ni andCo.Fig.1.Images of goethite particles at a low and a high magnification (limonite).Table 1Main elements and the respective mineralogical phases in limonite Element Mineralogical structureFeGoethite (a -FeOOH)Chromite (FeCr 2O 4)Magnesium iron silicate (amorphous)Magnetite (Fe 3O 4)AlGibbsite (Al(OH)3)Goethite (a -Al 1Àx Fe x OOH)Chromite (Al 1Àx Fe x Cr 2O 4)NiGoethite (a -FeOOH)Magnesium iron silicate (amorphous)Manganese particles Co Manganese particles Cr Chromite (FeCr 2O 4)Goethite (a -FeOOH)Si Silica (SiO 2)Magnesium iron silicate (amorphous)MgMagnesium iron silicate (amorphous)462 D.Georgiou,V.G.Papangelakis /Minerals Engineering 17(2004)461–4634.ConclusionsIn depth mineralogical analysis of limonitic laterite and the solids formed during sulfuric acid pressure leaching was obtained using transmission electron microscopy.Goethite (a -FeOOH)was the dominant phase of limonite forming needle-shape particles rich in nickel while;Al existed mainly in gibbsite particles.Co was found to be associated only with a manganese phase that was also rich in Ni.Both Ni and Co were highly leachable in the latter phase during sulfuric acid pressure leaching.Ni was also highly leachable in the magnesium silicate structures that were present in minor amounts.Hematite was the only precipitation phase of Fe formingspherical particles of a size of 0.1–0.3l m while;alunite was the only precipitation phase of Al.The above analysis proved crucial to the understanding of the physicochemical nature of leaching and the derivation of Ni and Co dissolution kinetic models.AcknowledgementsThe J.Roy Gordon Research Laboratory of INCO Ltd.and the Natural Sciences and Engineering Research Council of Canada (NSERC)are gratefully acknowl-edged for their financialsupport.Fig.2.A mixture of goethite–hematite particles at low and high magnification (leachingsolids).Fig.3.Two different alunite structures (leaching solids).D.Georgiou,V.G.Papangelakis /Minerals Engineering 17(2004)461–463463。