• Resources Recycling
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• v.30 no.4
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• pp.27-34
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• 2021

In this study, the leaching behavior of vanadium (V) was investigated through CaO roasting and sulfuric acid leaching from domestic V-bearing titanomagnetite (VTM). Changes in the phase according to the amount of CaO added and roasting temperature were analyzed. Regardless of the roasting conditions, perovskite (CaTiO₃) was preferred to form. When the CaO content was increased, the calcium ferrite (CaFeO_x) phase was formed; otherwise, ferrite (Fe₂O₃) was preferred. After CaO was roasted, leaching was performed for 6 h with 1M sulfuric acid at 50℃ and a 10% solid-liquid ratio. Results of leaching revealed that when the roasted product was sintered, V was not sufficiently oxidized, and the leaching efficiency decreased. In addition, when the roasting temperature was low, the leaching efficiency of V decreased due to the influence of unreacted excess CaO. To lower the leaching efficiency of iron and titanium in VTM concentrates, suppressing the formation of CaTiO₃ and CaFeO_x was necessary by minimizing the amount of CaO added. Consequently, a leaching efficiency of 86% V, 4.3% Fe, and 6.5% Ti was obtained when the roasted product of 1150℃ and 10 wt% CaO was leached.

• Resources Recycling
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• v.7 no.4
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• pp.64-75
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• 1998

The purpose of this study is to produce high putity composite powder composed of Fe-oxide, Mn-oxide and Mn-ferrite having superior homogencity in composition and particle size distribution by co-roasting process. Binary component metal (Fe, Mn) chloride solutions were produced by dissolving mill scale and ferro-mangancse alloy in hydrochloric acid. These chloride solutions contained the impurities such as SiO$_{2}$, P, Al, Ca and Na, which were originated from the Fe/Mn source materials. The neutralization and polymeric coagulant method were adoped to refine the hydrochloric liquor. When pH is far below the isoelectric point (pH 2-3), the SiO$_{2}$ was the most effectively reduced element, while other impurities remained unchanged. By increasing pH above 3, most of the impurities could be reduced effectively due to the coprecipitation reaction. The polymeric coagulants such as poly vinyl alcohol, resin amine and ammonium molybdate were found to have no effect on the spray roaster designed by the authors. The produced oxide powders were confirmed to be mixtures of Fe-oxide, Mn-oxide and mn-ferrite. the powders were homogeneously mixed and the particle size increased sleeply with increasing co-roasting temperature.

• Resources Recycling
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• v.13 no.3
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• pp.27-36
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• 2004

Nickel oxide was recovered through roasting of a spent catalyst for hydrogenation reaction. Nickel on Kieselguhr catalysts were prepared by a precipitation method after a treatment of the recovered-nickel oxide with an acid. Effects of roasting temperature of the spent catalyst on recovery of nickel oxide was investigated. Most of nickel oxide could be recovered through roasting of the spent catalyst at $1000^{\circ}C$. In regeneration of catalysts by the precipitation method after the treatment of nickel oxide with an acid, the effect of promoter, precipitation condition and reduction condition on catalytic performance in vegetable oil hydrogenation were investigated. The addition of CaO or $Ce_2$$O_3$ resulted in an increase of catalytic activity.

• Resources Recycling
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• v.11 no.1
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• pp.3-8
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• 2002

In order to make the high purity Mn$_3$O$_4$powder for the raw material of soft ferrite, Mn is extracted from the dust and the extracted solution is refined. The dust is generated in producing a medium-low carbon ferromanganese and contains 90% Mn$_3$O$_4$. Mn$_3$O$_4$in the dust was reduced into MnO by roasting with charcoal. Injection of the 180g/L of the reduced dust into 4N HCI solution increased pH of the leaching solution higher than 5 and then a ferric hydroxide was precipitated. Because the ferric hydroxide co-precipitates with Si ion etc, Fe and Si ion was removed from the solution and the about 10% Mn solution was obtained. The solution was diluted with water to Mn-15000 ppm and $NH_4$F was injected into the diluted solution at $70^{\circ}C$ to the F-3000 ppm. As a result, Ca ion is precipitated as $CaF_2$and the residual concentration of Ca was 14 ppm. Injection of the equivalent (NH$1.5M_4$)$_2$$CO_3$solution as 2 L/min at $25^{\circ}C$ into the above solution precipitated a fine and high purity $MnCO_3$powder. The deposition was filtrated and roasted at $1000^{\circ}C$ for 2 hours. As a result, $MnCO_3$powder is converted into $Mn_3$$O_4$powder and it had $8.2\mu$m of median size. The final production is above 99% $Mn_3$$O_4$powder and it satisfied the requirement of high purity $Mn_3$$O_4$powder for a raw material of soft ferrite.

• Resources Recycling
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• v.12 no.1
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• pp.33-40
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• 2003

Mn was extracted by using a nitric acid from the reduced ferromanganese dust and the basic experiments were taken to refine the manganese nitrate solution by means of precipitation of Ca, Mg oxalate. The dust was generated in AOD process producing a medium-low carbon ferromanganese and collected in the bag filter. Manganese oxide content in the dust was about 90% and its phase was confirmed as $Mn_3$$O_4$. $Mn_3$$O_4$ in the dust was reduced to MnO by roasting with activated charcoal. The main impurities in the extracted solution prepared by leaching the reduced dust with nitric acid were Na, K, Fe, Si, Ca, Mg etc. Among them, Fe was removed by controlling pH of the solution more than 4 and precipitating $Fe(OH)_3$, simultaneously silicious material solved in the solution was removed by co-precipitation with the ferric hydroxide. Addition of 150 g reduced dust into 4N HNO3 solution 1$\ell$ was appropriate to control the pH of the solution to pH 4. To differ greatly the solubilities of manganese oxalate and calcium or magnesium oxalate in a solution containing a high concentration of Mn, pH of 4 or less and addition of ($NH_4$)$_2$$C_2$$O_4$ in equivalent with Ca and Mg are recommended. At this time, the higher temperature was the shorter the precipitation reaction time was needed.

• Journal of Conservation Science
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• v.36 no.3
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• pp.162-177
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• 2020

Research was conducted to characterize the copper production and smelting process with 11 copper smelting by-products (copper slag and copper crucible) excavated from the NA and LA areas at the Gwanbuk-ri archeological site in Buyeo. Scanning electron microscopy-energy dispersive spectroscopy, wavelength dispersive X-ray fluorescence, X-ray diffraction, and Raman microspectroscopy were employed in the analysis. The research results reveal that the copper slag from Gwanbuk-ri contained silicate oxide, magnetite, fayalite, and delafossite, which are typical characteristics of crucible slag and refined slag. The outward appearance and microstructure of the slag were grouped as follows: 1. glassy matrix + Cu prill, 2. glassy matrix + Cu prill + magnetite, 3. silicate mineral matrix + Cu prill, 4. crystalline (delafossite and magnetite) + amorphous (Cu prill), 5. magnetite + fayalite, and 6. slag from slag. The copper slags from Guanbuk-ri were found to contain residues of impurities such as SiO₂, Al₂O₃, CaO, SO₄, P₂O₅, Ag₂O, and Sb₂O₃ in their microstructure, and, in some cases, it was confirmed that copper, tin and lead are alloys. These results indicate that refining of intermediate copper(including impurities) and refining of alloys of copper(including impurities) - tin and refining of copper(including impurities) - tin - lead took place during the copper production process at Gwanbuk-ri, Buyeo.

• Journal of Conservation Science
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• v.32 no.4
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• pp.579-588
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• 2016

This study analyzed nonmetallic inclusions in iron swords with a ring pommel excavated in the Ipbuk-dong, Suwon. Scanning electron microscopy with energy dispersive spectroscopy(SEM-EDS) was used to estimate the iron-making temperature, and we compared the oxide with $SiO_2$ to investigate the heat-treatment technology in the production of iron swords with a ring pommel by investigating the artificial insertion of a slag former and the metallurgical structure. From the wustite observed in most of the specimens, it is judged that these swords were produced by heating and forging iron smelted at a low temperature using the solid reduction method. In addition, judging from the partial presence of $P_2O_5$, it is assumed that they were smelted directly with natural ore, not calcined. From the ratios of $CaO/SiO_2$ and $TiO_2/SiO_2$, it is judged that the raw material for iron-making was iron ore and that a calcareous slag former was not artificially inserted. The structure of the blade part on the front end was pure iron. From the high carbon content of the blade part on the ring pommel and the formation of a martensitic structure and pearlite colony, it is judged that they were tempered after carburizing and that the back, handle part, and ring pommel were unintentionally carburized. Judging from the structure of these specimens, it was noted that they were produced by applying artificial partial heat-treatment technology. This study attempted to present a more scientific analysis by using the method of interpretation through component analysis of nonmetallic inclusions appearing in one relic by the ratio of the oxide divided by $SiO_2$. It is judged that reinterpreting the arguments by the results of the existing analysis and research in this way can obtain different interpretations.