• Resources Recycling
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• v.29 no.5
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• pp.28-37
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• 2020

In this study, the effect of precipitation temperature, ammonium chloride amount and addition method, vanadium and sodium hydroxide content of the solution on the precipitation of ammonium metavanadate were examined by using the sodium vanadate(NaVO₃) solution in alkali region as a starting material. As the pH of solution decreased, the addition amount of ammonium chloride and the vanadium content of the solution increased, the precipitation rate of ammonium metavanadate increased. In this research condition, the basic conditions for obtaining more than 90% of precipitation yield were 10,000mg/L of vanadium content, 2equivalents of ammonium chloride addition, room temperature, and 2 hours of precipitation time. The size of precipitated particles decreased with increasing precipitation rate. Especially when liquid ammonium chloride was injected into the solution, the precipitation rate was the slowest and the particle size of the precipitate was the largest. After the primary precipitation by adding ammonium chloride as a solid, the secondary precipitation was carried out by adding new reactants. At this time, the precipitation with added ammonium chloride solid was not affected by the precipitates present in the solution. However, when liquid ammonium chloride was added, new precipitate was deposited on the surface of the precipitate present in the solution, increasing its size. Due to the difference in ammonium metavanadate solubility to temperature, the precipitation temperature at the vanadium content of 10,000mg/L in the solution affected the precipitation rate of ammonium metavanadate and the precipitation temperature did not affect the precipitation rate at a high concentration of more than 30,000mg/L vanadium content in the solution.

• 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.

• 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.28 no.5
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• pp.42-50
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• 2019

In this study, the precipitation reaction of vanadium and ammonium chloride in aqueous solution was investigated in order to recover vanadium. Ammonium metavanadate having a crystal structure of [$NH_4VO_3$] was precipitated from aqueous solution containing vanadium at pH 9.2 ~ 9.4, and ammonium polyvanadate having a crystal structure of [$(NH_4)_2V_6O_{16}$] was precipitated when the pH of the aqueous solution containing vanadium was adjusted with sulfuric acid. Ammonium polyvanadate [$(NH_4)_2V_6O_{16}$] precipitated at a temperature of $80{\sim}90^{\circ}C$ and pH 2, and at a temperature of $40^{\circ}C$ and pH 6 ~ 8 of aqueous solution. In the acidic region of aqueous solution pH 2, the vanadium content of the aqueous solution should be at least 3,000 mg/L and the precipitation temperature should be maintained at $80^{\circ}C$ or higher in order to obtain a precipitation ratio of 99% or more. When the ammonium vanadate was precipitated in the alkaline region, the vanadium content was more than 10,000 mg/L and the precipitation temperature was maintained at $40^{\circ}C$ to increase the precipitation ratio. Aluminum was not precipitated regardless of the vanadium content and pH of the aqueous solution. However, the iron component reacts with ammonium chloride to precipitate into ammonium jarosite. Therefore, Fe component must be preferentially removed in order to increase the recovery of vanadium.

• 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.