바나듐 함유 수용액의 암모늄바나데이트 침전거동 고찰
Precipitation Behavior of Ammonium Vanadate from Solution Containing Vanadium
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초록
본 연구에서는 바나듐을 회수하기 위하여 수용액의 바나듐과 염화암모늄 침전반응에 관하여 고찰하였다. 바나듐 함유 수용액 pH 9.2 ~9.4에서는 결정구조가 [NH4VO3]인 암모늄메타바나데이트가 침전되었고, 바나듐 함유 수용액의 pH를 황산으로 조절하면 결정구조가 [(NH4)2V6O16]인 암모늄폴리바나데이트가 침전되었다. 암모늄폴리바나데이트[(NH4)2V6O16]는 바나듐 함유 수용액 pH 2에서는 침전온도 80 ~ 90o C에서, 그리고 수용액 pH 6 ~ 8에서는 침전온도 40o C에서 침전되었다. 또한 수용액 pH 2인 산성 영역에서99% 이상의 침전률을 얻기 위해서는 수용액의 바나듐 함량이 3,000 mg/L 이상은 되어야 하며, 침전온도는 80o C 이상으로 유지해야 한다. 알칼리 영역에서 암모늄메타바나데이트를 침전시킬 때, 바나듐 함량은 10,000 mg/L 이상 그리고 침전온도는 40o C로 유지해야 침전률을 높일 수 있었다. 알루미늄은 수용액의 바나듐 함량 및 pH에 상관없이 거의 침전이 일어나지 않았으나, 철 성분은염화암모늄과 반응하여 암모늄 자로사이트 형태로 침전되며, 따라서 바나듐의 회수율을 높이기 위해서는 Fe 성분을 우선적으로 제거해야만 한다.
Abstract
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 [NH4VO3] was precipitated from aqueous solution containing vanadium at pH 9.2 ~ 9.4, and ammonium polyvanadate having a crystal structure of [(NH4)2V6O16] was precipitated when the pH of the aqueous solution containing vanadium was adjusted with sulfuric acid. Ammonium polyvanadate [(NH4)2V6O16] precipitated at a temperature of 80 ~ 90 ℃ and pH 2, and at a temperature of 40 ℃ 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 ℃ 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 ℃ to increase the precipitation ratio. Aluminum was not pre-cipitated 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.
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