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Recovery of Mo by liquid-liquid extraction from synthetic leaching solution of spent Inconel 713C super alloy and preparation of Mo compounds

폐 인코넬계(Inconel 713C)내열합금 모의 침출액으로부터 액-액 추출법에 의한 Mo의 회수 및 Mo 화합물 제조

  • Ahn, Jong-Gwan (Department of Renewable Energy Resources, Jungwon University) ;
  • Kim, Da-young (Department of Renewable Energy Resources, Jungwon University) ;
  • In, Yong-Hyeon (Department of Renewable Energy Resources, Jungwon University)
  • 안종관 (중원대학교 신재생에너지자원학과) ;
  • 김다영 (중원대학교 신재생에너지자원학과) ;
  • 인용현 (중원대학교 신재생에너지자원학과)
  • Received : 2018.05.23
  • Accepted : 2018.08.03
  • Published : 2018.08.31

Abstract

Inconel 713C which of a commercial Ni super alloy have the composition of 70 % Ni, 12 % Cr, 6 % Al and 4 % Mo. Mo is very expensive and have some economic value to recover in the alloy. In this study, liquid-liquid exraction(solvent extraction and stripping) has been performed to separate Mo from the synthetic leaching solution of spent Inconel 713C alloy and prepare to Mo powder by dying, evaporation and heat treatment. The experiments were conducted by using synthetic leaching solution which was prepared $NaMoO_4$ $2H_2O$ by dissolved in distilled water. Alamine336 and Cyanex272 dissolved in kerosene were used as extractants. The extraction percentage of Mo by Alamine336 is 99 % in the condition of the range of pH 1 to 4 and 1 % of concentration of Alamine336. The stripping solutions are used by HCl, $H_2SO_4$ and $HNO_3$ solutions and the concentrations were controlled by distilled water. The concentrations of HCl, $H_2SO_4$ and $HNO_3$ as stripping solutions are increased, the stripping percentages of Mo are increased and the stripping percentage of Mo by $HNO_3$ is higher than other stripping solutions. After liquid-liquid extraction and heat treatment, $MoO_3$ powder which of the purity of 97.5 % was prepared.

고온 부품 소재로 사용하는 니켈계 내열합금인 Inconel 713C에는 Ni 70 %, Cr 12 %, Al 6 % 및 Mo 4% 등의 유가금속을 함유되어 있다. 이중 유가금속에서 경제적 가치를 가지는 원소는 Mo이므로 회수하여 재활용하여야 한다. 본 연구는 폐 인코넬계(Inconel 713C) 모의 내열합금 침출액으로부터 액-액 추출법(용매추출법 및 역추출법)을 이용하여 Mo을 분리 회수하였다. 회수된 수상을 증발 건조 및 열처리법을 이용하여 Mo 화합물을 제조하였다. 수상은 $NaMoO_4$ $2H_2O$을 증류수에 용해하여 사용하였으며, 추출제로는 음이온추출제인 Alamine 336과 양이온추출제인 Cyanex 272, 희석제로는 등유(Kerosene) 사용하였고, 음이온추출제인 Alamine 336 1 %이상에서 99 % 이상의 추출률을 확인하였다. 역추출제로는 황산, 염산 및 질산을 사용하였고, 각각 농도가 증가할수록 탈거율이 증가하였으며, 질산의 경우 4 M에서 96 %의 탈거율을 나타냈었다. 용매추출과 역추출에서 얻은 Mo 함유 수상을 증발 건조하여 순도 97.5 %의 $MoO_3$를 제조하였다. 본 연구를 통해 Mo이 함유된 순환자원으로부터 Mo을 효율적으로 회수하면 국내의 자원효율성과 자원수요의 공급경쟁력을 향상시킬 수 있다.

Keywords

References

  1. KORES webpage, 2017 : https://m.kores.net/mobile/mprice/mbasemetal.
  2. All Metals & Forge Group webpage, 2018 : http://www.steelforge.com/.
  3. Korea Institute of Geoscience & Resoueces(KIGAM): "Annual report", pp. 35-38, 2017.
  4. KITA, 2015 : Trade trends of Ni alloy, https://unipass.customs.go.kr:38030/ets/.
  5. Ahn, J.-W., J.-G. Ahn, and M.-S. Lee, "Recovery of Nitric Acid and Valuable metals from Spent Nitric Etching Solutions of Printed Circuit Board", Journal of the Korean Institute of Metals and Materials, vol 40, no. 1, pp. 116-121, 2002. DOI: http://www.riss.kr/link?id=A19618101
  6. Yonghwang Ha, Ryun-Ji Gang, Seong-Ho Son, Wonsik Lee, and Jong-Gwan Ahn, "Recovery of Nitric acid and Copper from Plating Waste of Automobile Wheel", Journal of the Korea Academia-Industrial cooperation Society, vol. 14, No. 11 pp. 6015-6022, 2013. DOI: https://doi.org/10.5762/kais.2013.14.11.6015
  7. Jong-gwan Ahn, Hee-Kyeoung Jung, Jae-Young Jang and Min-Seuk Kim, " Solvent Extraction Separation of Re (VI) from Hydrochloric Acid Leaching Solution of Spent Super Alloy by Alamine 304-1", J. of Korean Inst. of Resources Recycling, vol. 24, No. 5, 56-62, 2015. DOI: https://doi.org/10.7844/kirr.2015.24.5.56
  8. Wonguen L., Bumrae C., "Eco-frendly hydrometallurgy process for the recovery of Mo from spent petroleum catalyst". KR. Patent No. 101727891B1. 2017.
  9. Minwoo K., Master thesis, "Selective recovery of V, Mo by solvent extraction from sodium leaching solution of spent DSC", Korea Univ., pp. 10-15. 2011.
  10. Parhi, P.K., Park, K.H., Kim, H.I., Park, J.T.,"Recovery of molybdenum from the sea nodule leach liquor by solvent extraction using Alamine 304-I", Hydrometallurgy, vol 105, pp. 195-200, 2011. DOI: https://doi.org/10.1016/j.hydromet.2010.09.004
  11. Zeng L., Cheng C. Y., "A literature review of the recovery of molybdenum and vanadium from spent hydrodesulphurisation catalyst. Part I Metallurgical processes", Hydrometallurgy, vol. 98, pp. 1-9, 2009. DOI: https://doi.org/10.1016/j.hydromet.2009.03. 012
  12. Nguyen Hong Thi, Lee, Man Seung, "Recovery of Molybdenum and Vanadium from Acidic Leaching Solution of Spent Catalysts by Solvent Extraction", J. the Korean Inst. of Resources Recycling, vol. 22, no. 4, pp. 3-11. 2013. DOI: https://doi.org/10.7844/kirr.2013.22.4.3
  13. Nguyen Thi Hong, Lee, Man Seung, "Separation of Molybdenum and Tungsten from Sulfuric acid Solution by Solvent Extraction with Alamine 336", J. the Korean Inst. of Resources Recycling, vol. 25, no. 1, pp. 16-23. 2016. DOI: https://doi.org/10.7844/kirr.2016.25.1.16