• Resources Recycling
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• v.4 no.3
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• pp.19-25
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• 1995

A Study on the recovery of the valuable metals(Vanadium Molybdenium) was carried out using spent catalysts originated from desulfurizing process of oil refinery. Experiments consisted of pre-roasting for Sulfur and Carbon removal, soda roasting and leaching for the extraction of valuable metals, and selective precipitation of Vanadium and Molybdenium. Effects of temperature and time in roasting for Sulfur removal, of $Na_2CO_3$ concentrations in soda roasting, and of pulp density, temperature and time in leaching were investigated for the recovery of Vanadium and Molybdenium. A optimum condition having over 85% in yield of Vanadium and Molybdenium was found. In the selective precipitation, more than 98% of Vanadium and Molybdenium were obtained by the variation of pH and concentration of additives.

• Resources Recycling
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• v.31 no.2
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• pp.40-48
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• 2022

In this study, the effects of solution components were investigated in the recovery of vanadium as ammonium metavanadate from vanadium-ore-salt roasting-water leaching solution. The vanadium-containing solution is strongly alkaline (pH 13), so the pH must be lowered to 9 or less to increase the ammonium metavanadate precipitation efficiency. However, in the process of adjusting the solution pH using sulfuric acid, aluminum ions are co-precipitated, which must be removed first. In this study, aluminum was precipitated in the form of an aluminum-silicate compound using sodium silicate, and the conditions for minimizing vanadium loss in this process were investigated. After aluminum removal, the silicate was precipitated and removed by adjusting the solution pH to 9 or less using sulfuric acid. In this process, the concentration and addition rate of sulfuric acid have a significant influence on the loss of vanadium, and vanadium loss was minimized as much as possible by slowly adding dilute sulfuric acid. Ammonium metavanadate was precipitated using three equivalents of ammonium chloride at room temperature from the aluminum-free, aqueous solution of vanadium following the pH adjustment process. The recovery yield of vanadium in the form of ammonium metavanadate exceeded 81%. After washing the product, vanadium pentoxide with 98.6% purity was obtained following heat treatment at 550 ℃ for 2 hours.

• Resources Recycling
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• v.32 no.3
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• pp.26-37
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• 2023

Good control of the solution pH and temperature is required to recover vanadium from the water leaching solution of vanadium ore after sodium roasting. However, such adjustments could lead to aluminum-vanadium and sodium-vanadium co-precipitation, which greatly affects the efficiency of vanadium recovery. In this study, a process that can increase the efficiency of vanadium recovery as ammonium metavanadate [NH₄VO₃] and ammonium polyvanadate [(NH₄)₂V₆O₁₆·H₂O] was investigated by examining the characteristics of vanadium-containing aqueous solutions during precipitation. The aluminum content of vanadium-containing water leaching solutions has a great effect on the loss of vanadium when the pH of the aqueous solution is adjusted to 9. Therefore, a process to minimize aluminum leaching is also required. In this study, ~99% or more of vanadium present in vanadium-containing aqueous solutions was precipitated and recovered as NH₄VO₃ by adding 3 equivalents of ammonium chloride relative to the vanadium content at pH 9 and room temperature. (NH₄)₂V₆O₁₆·H₂O was precipitated from the aluminum-vanadium coprecipitates generated during the pH-adjustment of the aqueous solutions to 9 by dissolving the coprecipitate in the solutions at pH 2.5 and controlling their sodium content to 2,000 mg/L or less. Approximately, 98% or more of the available (NH₄)₂V₆O₁₆·H₂O could be precipitated and recovered from a solution with a vanadium content of 2,200 mg/L and a sodium content of 1,875 mg/L at pH 2.5 by adding approximately 3 equivalents of ammonium chloride relative to the vanadium content at 95℃ or higher. The overall process could precipitate and recover, approximately 91% or more of the total vanadium in the water leaching solution as NH₄VO₃ and (NH₄)₂V₆O₁₆·H₂O.

• Resources Recycling
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• v.31 no.2
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• pp.20-32
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• 2022

This study implemented a chelating agent (Ethylenediaminetetraacetic acid, EDTA) in purification to obtain high-purity vanadium pentoxide (V₂O₅) for use in VRFB (Vanadium Redox Flow Battery). V₂O₅ (powder) was produced through the precipitation recovery of ammonium metavanadate (NH₄VO₃) from a vanadium solution, which was prepared using a low-purity vanadium raw material. The initial purity of the powder was estimated to be 99.7%. However, the use of a chelating agent improved its purity up to 99.9% or higher. It was conjectured that the added chelating agent reacted with the impurity ions to form a complex, stabilizing them. This improved the selectivity for vanadium in the recovery process. However, the prepared V₂O₅ powder exhibited higher contents of K, Mn, Fe, Na, and Al than those in the standard counterparts, thus necessitating additional research on its impurity separation. Furthermore, the vanadium electrolyte was prepared using the high-purity V₂O₅ powder in a newly developed direct electrolytic process. Its analytical properties were compared with those of commercial electrolytes. Owing to the high concentration of the K, Ca, Na, Al, Mg, and Si impurities in the produced vanadium electrolyte, the purity was analyzed to be 99.97%, lower than those (99.98%) of its commercial counterparts. Thus, further research on optimizing the high-purity V₂O₅ powder and electrolyte manufacturing processes may yield a process capable of commercialization.

• Resources Recycling
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• v.30 no.6
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• pp.3-11
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• 2021

In this study, the effect of the solubility of ammonium metavanadate and the decomposition ratio of ammonium ions on a precipitation reaction-the precipitation of ammonium metavanadate by adding ammonium chloride to a sodium vanadate solution-was investigated. As the precipitation temperature and pH increased, the decomposition ratio of ammonium ions increased, and the decomposition ratio was greater than 81% at 45 ℃ and pH 9.3. This was approximately four times higher than that at pH 8. The result of the precipitation reaction, in view of these two factors that significantly influence the precipitation reaction, was that the precipitation yield increased as the temperature increased. However, the effect of temperature was not significant above 35 ℃. A kinetic study of the precipitation reaction revealed that the activation energy of the reaction was 42.3 kJ/mol. Therefore, considering the solubility of ammonium metavanadate, the lower the temperature, the better the vanadium recovery yield. Additionally, considering the decomposition of ammonium ions, the lower the pH of the aqueous solution, the more advantageous. However, at pH 8 or less, sodium polyvanadate is precipitated and the purity of vanadium oxide may reduce.

• Proceedings of the IEEK Conference
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• 2001.10a
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• pp.633-637
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• 2001

Oil fly ash is known as one source of raw materials from which vanadium and nickel metals can be recovered. The current recovery process of valuable metals from oil fly ash is mainly the hydrormetallurgy one. Nevertheless, a great amount about 50~80%, of unburned carbon remains as byproduct after hydrormetallursy process. In Taiwan, if hydrormetallursy processes have proceeded, it can be estimated that the annual production of unburned carbon is 25 thousand tons. From the viewpoint of resource recycling, this study is a preliminary study and investigates in recovery of sub micron- graphitized carbon from unburned carbon by a designed process. The designed process included the following steps: 1.selecting a portion with +400mesh size from unburned carbon; 2.treating the selected in ultrasonic waves; 3.using a 400mesh sieve to obtain the product which is under 400mesh; 4.Removal ash from the product. In regard to treatment by ultrasonic waves in the designed process, treating time of ultrasonic waves is a simple and only variance in this study. The results indicate that the production yields increase with the treating time of ultrasonic waves; the production yield in specific conditions of this study can reach about 23%, in which ash content in product is about 2.5%. According to results of SEM, TEM and XRD, the products from the designed process are flakes in shape, several microns in size and graphitized carbon in carbon crystal phase. Except to graphitized carbon, there are a little carbon blacks, which are graphite 2H in carbon crystal phase in the products. Conclusively, the designed process is possibly applicable, by which comes to the recovery of micron- graphitized carbon.

• Resources Recycling
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• v.32 no.6
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• pp.54-66
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• 2023

Titanium's importance as a mineral resource is increasing, but the Korean industry depends on imports. Ilmenite is the principal titanium ore. However, research and development from raw materials have not been investigated yet in detail. Hence, measures to secure a stable titanium supply chain are urgently needed. Accordingly, through beneficiation technology, we evaluated the possibility of technological application for the efficient recovery of valuable minerals. As a result of the experiments, we confirmed that mineral particles existed as fine particles due to weathering, making recovery through classification difficult. Consequently, applying beneficiation technologies, i.e., specific gravity separation, magnetic separation, and flotation, makes it possible to recover valuable minerals such as hematite and rutile. However, there are limitations in increasing the quality and yield of TiO₂ due to the mineralogical characteristic of the hematite and rutile contained in titanium ore. Hametite is combined with rutile even at fine particles. Therefore, it is essential to develop mineral processing routes, to recover iron, vanadium, and rare earth elements as resources. On that account, we used grinding technology that improves group separation between constituent minerals and magnetic separation technology that utilizes the difference in magnetic sensitivity between fine mineral particles. The development of beneficiation technology that can secure the economic feasibility of valuable materials after reforming iron oxide and titanium oxide components is necessary.