Studies on the Development of Iodine Recovery Process with High Yield and Purity from NH4I Solution

NH4I 용액으로부터 고효율/고순도의 요오드 회수 공정개발에 관한 연구

  • Yoon, Jong Sun (Department of Chemical & Biomolecular Engineering, Sogang University) ;
  • Lim, Seong Bin (Department of Chemical & Biomolecular Engineering, Sogang University) ;
  • Oh, Se Yong (Department of Chemical & Biomolecular Engineering, Sogang University)
  • 윤종선 (서강대학교 화공생명공학과) ;
  • 임성빈 (서강대학교 화공생명공학과) ;
  • 오세용 (서강대학교 화공생명공학과)
  • Received : 2015.03.20
  • Accepted : 2015.04.02
  • Published : 2015.06.10


In this paper, we have investigated the optimization of $I_2$ recovery process from $NH_4I$ solution, which is generated as by-product during the amination reaction of p-diiodobenzene (PDIB) for p-phenylenediamine (PPD) synthesis. The recovered $I_2$ is then recycled as a raw material for PDIB synthesis. We have employed a cation exchange resin to recover $I_2$ from $NH_4I$ sample solution, and determined the breakthrough point and exchange capacity from the breakthrough curve. Furthermore, we have suggested optimum conditions of our $I_2$ recovery process by measuring the purity and yield of recovered $I_2$ with respect to the concentrations of $NH_4I$ and oxidant ($H_2O_2$) solutions, the oxidation time, and the temperature of drying process. Finally, the yield and purity as high as 94.96% and 96.65%, respectively were obtained by reusing the residual solution still containing unrecovered iodide ions.


  1. D. B. Stojanovic, M. Zrilic, R. Jancic-Heinemann, L. Zivkovic, A. Kojovic, P. S. Uskokovic, and R. Aleksic, Mechanical and anti-stabbing properties of modified thermoplastic polymers impregnated multiaxial p-aramid fabrics, Polym. Adv. Technol., 24, 772-776 (2013).
  2. I. S. Han, Method of making aramid fiber, Korea Patent 10-0910537 (2009).
  3. Y. J. Shin, J. C. Kim, J. B. Lim, and D. J. Lee, Preparation method for para phenylene diamine, Korea Patent 10-2012-0018950 (2012).
  4. Y. J. Joo, J. U. Kim, and J. I. Won, A novel method of preparing p-phenylenediamine, Korea Patnet 10-0362772 (2000).
  5. J. S. Lee, Removal of Phosphate with Ion Exchange Resins, Master Dissertation, Gyeongsang National Uinversity, Jinjoo, Korea (2011).
  6. K. G. Park, Ion Exchange Resins for Treatment and Reuse of Chromium Rinse Wastewater from Thin Metal Sheet, Master Dissertation, Yeungnam University, Daegu, Korea (2005).
  7. J. S. Han, R. I. Choi, C. J. Park, H. R. Noh, B. G. Kim, S. Y. Kim, J. Y. Ahn, C. G. Kang, I. W. Jung, and J. C. Lee, Evaluation of acid deposition and impact assessment in Korea, National Institute of Environmental Research., 21, 119-136 (1999).
  8. C. R. Silva, J. A. Simoni, C. H. Collins, and P. L. O. Volpe, Ascorbic acid as a standard for iodometric titrations, J. Chem. Educ., 76, 1421-1422 (1999).
  9. R. Roman and H. B. Dunford, pH dependence of the oxidation of iodide by compound I of Horseradish Peroxidase, Biochemistry, 11, 2076-2082 (1972).
  10. L. I. Katzin and E. Gebert, Solvent effects in the iodide-iodine-triiodide complex equilibrium, J. Am. Chem. Soc., 76, 2049-2054 (1954).
  11. I. M. Kolthoff, The volumetric analysis of hydrazine by the iodine, bromate, iodate and permanganate methods, J. Am. Chem. Soc., 46, 2009-2016 (1924).
  12. S. B. Lee, I. J. park, D. K. Kim, J. H. Kim, K. W. Lee, J. W. Ha, K. J. Kim, H. D. Lee, J. K. Jung, and J. H. Lim, Method for Iodine recovery from nitrogen compound solution using an ion exchange resin, Korea Patent 10-0434725 (2004).
  13. D. A. Shirley and W. F. Giauque, The entropy of iodine. heat capacity from 13 to 327 K. Heat of Sublimation, J. Am. Chem. Soc., 81, 4778-4779 (1959).
  14. K. S. Johnson and L. J. Coletti, In situ ultraviolet spectrophotometry for high resolution and long-term monitoring of nitrate, bromide and bisulfide in the ocean, Deep-Sea Res. I, 49, 1291-1305 (2002).