Iron sulfate, in particular FeSO4·7H2O, is derived from titanium dioxide production and the steel pickling process. Regarding TiO2 manufacturing, the amount of the resultant FeSO4·7H2O can be as high as 6 tons per ton of produced TiO2, leading to a huge amount of ferrous sulfate heptahydrate, which is considered an environmental and economic concern for the titanium dioxide industry in European countries. The present paper focuses on the thermal treatment of ferrous sulfate (heptahydrate and monohydrate) samples under different conditions. Nonisothermal thermogravimetric (TG) analysis was used to study the behavior of iron sulfate samples at temperatures of up to 1000 °C in Cl2 + O2, O2, and N2 atmospheres. Results showed that the dehydration of iron sulfate heptahydrate in nitrogen started at room temperature and resulted in iron sulfate tetrahydrate (FeSO4·4H2O). The ferrous sulfate monohydrate (FeSO4·H2O) was formed at temperatures close to 150 °C, while the anhydrous ferrous sulfate (FeSO4) was obtained when the samples were heated in nitrogen at over 225 °C. The kinetic features of FeSO4 decomposition into Fe2O3 were revealed under isothermal conditions at temperatures ranging from 500 to 575 °C. The decomposition of iron sulfate was characterized by an apparent activation energy of around 250 kJ/mol, indicating a significant temperature effect on the decomposition process. The obtained powder iron oxide could be directed to the agglomeration unit of iron and the steelmaking process.
Development of our modern society requests a number of critical and strategic elements (platinum group metals, In, Ga, Ge…) and high value added elements (Au, Ag, Se, Te, Ni…) which are often concentrated in by-products during the extraction of base metals (Cu, Pb, Zn…). Further, recycling of end-of-life materials employed in high technology, renewable energy and transport by conventional extractive processes also leads to the concentration of such chemical elements and their compounds in metallurgical by-products and/or co-products. One of these materials, copper anode slime (CAS), derived from a copper electrolytic refining factory, was used for this study. The sample was subjected to isothermal treatment from 225 to 770 °C under air atmosphere and the reaction products were systematically analyzed by scanning electron microscopy through energy dispersive spectroscopy (SEM-EDS) and X-ray diffraction (XRD) to investigate the thermal behavior of the treated sample. The main components of the anode slime (CuAgSe, Cu2-xSeyS1-y, Ag3AuSe2) react with oxygen, producing mostly copper and selenium oxides as well as Ag-Au alloys as final products at temperatures higher than 500 °C. Selenium dioxide (SeO2) is volatilized and recovered in pure state by cooling the gaseous phase, whilst copper(II) oxide, silver, gold and tellurium remain in the treatment residue.
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