Resources Recycling (자원리싸이클링)

The Korean Institute of Resources Recycling (한국자원리싸이클링학회)
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Preparation of Iron Nano-particle by Slurry Reduction Method from Leaching Solution of Spent Nd magnet

폐네오디뮴 자석 침출용액으로부터 Slurry 환원법을 이용한 철 Nano 분말 제조

  • Ahn, Jong-Gwan (Department of Resource Recycling and Environmental Engineering, Jungwon University) ;
  • Gang, Ryunji (Department of Resource Recycling and Environmental Engineering, Jungwon University) ;
  • You, Haebin (Department of Resource Recycling and Environmental Engineering, Jungwon University) ;
  • Yoon, Ho-Sung (Mineral Resource Research, Korea Institute of Geoscience and Resources)
  • 안종관 (중원대학교 자원순환환경공학과) ;
  • 강윤지 (중원대학교 자원순환환경공학과) ;
  • 유혜빈 (중원대학교 자원순환환경공학과) ;
  • 윤호성 (한국지질자원연구원)
  • Received : 2014.09.12
  • Accepted : 2014.11.10
  • Published : 2014.12.31
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Abstract

Recycling process of iron should be developed for efficient recovery of neodymium (Nd), rare metal, from acid-leaching solution of Nd magnet. In this study, $FeCl_3$ solution as iron source was used for preparation of iron nano particles with the condition of various factors, such as, reductant, and surfactant. $Na_4P_2O_7$ and Polyvinylpyrrolidone (PVP) as surfactants, $NaBH_4$ as reductant, and palladium chloride ($PdCl_2$) as a nucleation seed were used. Iron powder was analyzed by using XRD, SEM for measuring shape and size. Iron nano particles were prepared at the ratio of 1:5 (Fe (III) : $NaBH_4$). Size and shape of iron particles were round-form and 50 ~ 100 nm size. Zeta-potential of iron at the 100 mg/L of $Na_4P_2O_7$ was negative value, which was good for dispersion of metal particle. When $Na_4P_2O_7$ (100 mg/L), PVP($FeCl_3:PVP$ = 1 : 4, w/w) and Pd($FeCl_3:PdCl_2$ = 1 : 0.001, w/w) were used, iron nano particles which were round-shape, well-dispersed and near 100 nm-sized range. In this condition, $FeCl_3$ solution changed with spent Nd leachate solution, and then it is possible to be made round-formed iron nano particles at pH 9 and at the reaction bath over 20 L which is not include any surfactant.

네오디뮴 폐자석 침출액으로부터 희유금속인 네오디뮴을 회수하는 연구와 함께 네오디뮴과 같이 침출되는 철의 부가가치를 높이는 연구가 필요하다. 본 연구에서는 네오디뮴과 같이 침출되는 철의 유용자원화를 위한 기초연구로 철 나노분말을 제조하는 실험을 수행하였다. 본 연구는 $FeCl_3$ 용액을 철 분말 원료로, 분산제는 $Na_4P_2O_7$와 Polyvinylpyrrolidone를 이용하였고, 환원제로는 $NaBH_4$, 철 나노분말 핵생성 촉진제 seed로 염화팔라듐을 사용하였다. 제조한 철 나노분말을 XRD, SEM을 이용하여 분말의 형상 및 크기를 분석하였다. Fe와 $NaBH_4$의 몰 비를 1 : 5로 조절하여 철 분말을 제조하였으며, 이 때 철 분말은 구형이었으며, 입도는 약 50 ~ 100 nm 였다. 분산제 $Na_4P_2O_7$의 경우 100 mg/L에서 철 이온의 제타포텐셜이 음의 값을 가졌고, $FeCl_3$ 과 PVP와 Pd의 질량비 1 : 4 : 0.001에서 분산이 양호하고, 입도가 100 nm 인 철 나노분말을 합성하였다. 같은 반응 조건에서 폐 Nd 침출액의 Fe 이온을 pH를 조절하여 슬러리화한 후 실험을 진행한 결과, pH 9에서 구형의 철 분말을 합성할 수 있었으며, 20 L 이상의 Scale-up 공정에서는 분산제 없이 환원제로 175 nm 크기의 철 분말을 합성할 수 있었다.

Keywords

References

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