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Recovery of Zirconium from Spent Pickling Acid through Precipitation Using BaF2 and Electrowinning in Fluoride Molten Salt

BaF2 침전 및 불화물 용융염 전해 제련을 통한 폐 산세액 내 지르코늄 회수

  • Han, Seul Ki (Graduate School of Department of Materials Science & Engineering, Chungnam National University) ;
  • Nersisyan, Hayk H. (Graduate School of Department of Materials Science & Engineering, Chungnam National University) ;
  • Lee, Young Jun (RASOM, Chungnam National University) ;
  • Choi, Jeong Hun (Graduate School of Department of Materials Science & Engineering, Chungnam National University) ;
  • Lee, Jong Hyeon (Graduate School of Department of Materials Science & Engineering, Chungnam National University)
  • 한슬기 (충남대학교 신소재공학과) ;
  • ;
  • 이영준 (충남대학교 급속응고신소재연구소) ;
  • 최정훈 (충남대학교 신소재공학과) ;
  • 이종현 (충남대학교 신소재공학과)
  • Received : 2016.10.03
  • Accepted : 2016.10.31
  • Published : 2016.12.27

Abstract

Zirconium(Zr) nuclear fuel cladding tubes are made using a three-time pilgering and annealing process. In order to remove the oxidized layer and impurities on the surface of the tube, a pickling process is required. Zr is dissolved in HF and $HNO_3$ mixed acid during the process and pickling waste acid, including dissolved Zr, is totally discarded after being neutralized. In this study, the waste acid was recycled by adding $BaF_2$, which reacted with the Zr ion involved in the waste acid; $Ba_2ZrF_8$ was subsequently precipitated due to its low solubility in water. It is very difficult to extract zirconium from the as-recovered $Ba_2ZrF_8$ because its melting temperature is $1031^{\circ}C$. Hence, we tried to recover Zr using an electrowinning process with a low temperature molten salt compound that was fabricated by adding $ZrF_4$ to $Ba_2ZrF_8$ to decrease the melting point. Change of the Zr redox potential was observed using cyclic voltammetry; the voltage change of the cell was observed by polarization and chronopotentiometry. The structure of the electrodeposited Zr was analyzed and the electrodeposition characteristics were also evaluated.

Keywords

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