DOI QR코드

DOI QR Code

옥살레이트 침전법에 의한 폐솔더 박리액에서 주석 및 구리의 회수

Recovery of Tin and Copper from Waste Solder Stripper by Oxalate Precipitation

  • Ryu, Seong-Hyung (Dept. of Advanced Materials Sci. & Eng., Daejin University) ;
  • Ahn, Jae-Woo (Dept. of Advanced Materials Sci. & Eng., Daejin University) ;
  • Ahn, Hyo-Jin (Dept. of Advanced Materials Sci. & Eng., Daejin University) ;
  • Kim, Tae-Young (Dept. of Advanced Materials Sci. & Eng., Daejin University)
  • 투고 : 2013.04.18
  • 심사 : 2014.05.22
  • 발행 : 2014.06.30

초록

폐솔더 박리액으로부터 옥살산 침전법을 이용하여 주석 및 구리의 분리 침전을 통해 각각 금속염으로 회수하기 위한 기초 연구를 실시하였다. 먼저 옥살산의 첨가에 따라 주석의 침전 제거율이 증가하였으며 당량비(옥살산/주석)의 1.0-1.5배를 첨가할 경우 주석이 99.5%의 이상 제거율을 나타내었다. 이 경우에 구리는 2.0% 정도 침전되었고 철, 납등은 침전되지 않아 주석만 선택적으로 침전되는 것을 확인 하였다. 반응온도 증가에 따라 주석의 침전율은 증가하여 $60^{\circ}C$ 부근에서 최대값을 보이다가 온도가 더 증가하면 오히려 감소 경향을 보였다. 침전물을 여과 건조시켜 $SnO_2$의 산화물을 얻을 수 있었다. 주석이 제거된 폐솔더 박리액에 옥살산을 첨가하여 구리를 납, 철 등의 금속이 선택적으로 약 91% 이상 침전되어 회수가 가능하였다.

A study has been made on the recovery of tin and copper from waste solder stripper by oxalate precipitation. With the increasing of the oxalic acid addition, tin was precipitated effectively and removed above 99.5% of tin when the oxalic acid, in an amount 1.0-1.5 times the stoichometric requirement, was added. But, in this case, only 2.0% of copper was precipitated and lead, iron were not precipitated. So, tin was selectively removed from the waste solution. With the increasing of the reaction temperature, the removal percentage of tin was increased and maximum value at arounf $60^{\circ}C$ and decreased with increase in the temperature any more. After filtering the precipitate and drying in oven, $SnO_2$ was obtained from the precipitate. After removal of tin in stripping solution, above 91% of copper was selectively removed by Cu-oxalate by addition of oxalic acid.

키워드

참고문헌

  1. Charlie Kerr, 2004 : Sustainable technologies for the regeneration of acidic tin stripping solutions used in PCB fabrication" Circuit world 30(3), 51-58. https://doi.org/10.1108/03056120410520623
  2. T. Keskitalo, J. Tanskanen, T. Kuokkanen, 2007 : "Analysis of key patents of the generation of acdic cupric chloride etchant waste and tin stripping waste" Resources, Conservation and Recycling" 49, 217-243. https://doi.org/10.1016/j.resconrec.2006.05.001
  3. Man-Seung Lee, Jong-Gwan Ahn, Jae-Woo Ahn, 2003 : Recovery of copper, tin and lead from the spent nitric etching solutions of printed circuit board and regeneration of the etching solution" Hydrometallurgy, 70, 23-29. https://doi.org/10.1016/S0304-386X(03)00045-8
  4. Norvell J. Nelson : "Regenerative copper etching process and solution" U.S. Patent, 4,545,850
  5. Jae-Woo Ahn, Meong-Woon Kim, Jin-Ki Jeong, Jae-Chun Lee, 2006 : "Recovery Cu and Sn from the bioleaching solution of electronic scrap." J. of Korean Inst. of Resources Recycling, 15(6), 41-47.
  6. C.J. Brown, D. Davy and P.J. Simmons, 1980 : " Recovery of nitric acid from solutions used for treating metal surface." Plating and surface finishing. vol 2. 60-62.
  7. T.K. Mattila, 1977 : "Nitrate removal from waste solutions by solvent extraction" Ind. Eng. Chem., Process Des. Dev. 16(4), 469-472. https://doi.org/10.1021/i260064a006
  8. I. Mockrin, Martin A. Hobin, 1977 : "Recovery of copper from waste nitrate liquors by electrolysis." U.S. Patent, 4,033,838.
  9. S. Roy, R. Buckle, 2009 : "The recovery of copper and tin from waste tin stripping solution PartII: Kinetics analysis of synthetic and real process waste" Separation and purification technology, 68, 185-192. https://doi.org/10.1016/j.seppur.2009.05.005
  10. O. Gyliene and M. Salkauskas, 1995 : "Metal recovery from spent electroless plating solutions by oxalate precipitation" Plating and surface finishing, 61-63.
  11. Shi Juan, Wu Shi-Hua, Zhang Shou-Min, Huang Wei-Ping, Wang Shu-Rong, 2004 : "Synthesis of nano-$SnO_2$ through pyrolysis method and its gas sensitivity property" Chemical Journal of Chinese Universities, 25(4), 607-609.
  12. JP 11-021681 "Method for regenerating removing solution for tin or solder"
  13. L. C. Soare, J. Lemaitre, P.Bowen, H. Hofmann, 2006 : "A thermodynamic model for the precipitation of nanostructured copper oxalate" J. Crystal Growth, 289, 278-285. https://doi.org/10.1016/j.jcrysgro.2005.11.085