폐 영구자석 스크랩 황산침출용액으로부터 황산나트륨에 의한 희토류 원소 복염침전 거동 고찰
Double Salt Precipitation Behavior of Rare Earth by Sodium Sulfate in Sulfuric Liquor of Waste Permanent Magnet Scrap
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본 연구에서는 희토류 황산수용액으로부터 희토류 원소를 철로부터 분리/회수하고자, 황산나트륨을 이용한 희토류 황산복염 침전반응에 관하여 고찰하였다. 네오디뮴(Nd)은 황산나트륨과 결합하여 복염으로 침전이 용이하게 일어나는 반면에 디스프로슘(Dy)은황산복염으로 침전되기 위해서 과량의 황산나트륨이 필요하였다. 또한 황산수용액에서 네오디뮴의 존재는 디스프로슘 황산복염 침전을 촉진시켜서 디스프로슘 황산복염 침전률을 증가시켰다. 본 연구에서 사용된 네오디뮴 함량 23.39 mg/ml, 디스프로슘 함량8.67 mg/ml인 황산수용액으로부터 반응온도 60 o C, 반응 3시간에서 황산나트륨을 7 당량 첨가하였을 때, 네오디뮴 복염 침전률은99.7%, 디스프로슘 복염 침전률은 94.3%이었다. 또한 네오디뮴과 디스프로슘의 황산복염 침전특성을 이용한 두 원소의 분리 가능성을 고찰한 결과, 염화나트륨 첨가에 의한 염석효과가 디스프로슘 품위 증가에 중요한 역할을 하며 본 연구조건에서 최대 98.7% 품위의 디스프로슘을 얻을 수 있었다.
Abstract
In this study, the precipitation of rare earth-sodium sulfate with sodium sulfate was conducted in order to separate rare earth from Fe in rare earth sulfate solution. Neodymium (Nd) was easily precipitated as Nd-sulfate salt with sodium sulfate, on the other hand, excessive sodium sulfate was needed for the precipitation of Dy-sulfate salt. Also neodymium not only promoted the precipitation of dysprosium sulfate salt but also increased recovery of dysprosium sulfate salt in sulfuric acid solution. At the condition of 60 o C precipitation temperature, 3 h reaction time, 7 equivalents sodium sulfate, the recovery of neodymium and dysprosium sulfate salt was 99.7% and 94.3% respectively from the sulfuric acid solution containing Nd of 23.39 mg/ml and Dy of 8.67 mg/ml. Lastly, from the results of separation of Dy to Nd by the method of sulfate double salt, the effect of salting out with NaCl is important to increase the grade of Dy, and 98.7% of Dy grade could be obtained in this study.
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