Applied Chemistry for Engineering (공업화학)

The Korean Society of Industrial and Engineering Chemistry (한국공업화학회)
권호 표지
DOI QR코드

DOI QR Code

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
Download PDF
⟨ Previous Next ⟩

Abstract

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.

본 연구에서는 p-diiodobenzene (PDIB)으로부터 p-phenylenediamine (PPD) 합성 후 생성되는 부산물인 $NH_4I$를 PDIB 합성의 원료로 재활용하기 위하여 $I_2$ 회수 공정의 최적화에 관한 연구를 진행하였다. 양이온교환수지를 사용하여 $NH_4I$ 시약 용액으로부터 $I_2$ 회수에 관한 연구를 진행하였고 양이온교환수지의 파과곡선을 통해 파과점 및 관류교환용량을 조사하였다. 회수되는 요오드의 수율 및 순도 향상을 위해 $NH_4I$의 공급용액 및 산화제($H_2O_2$)의 농도 변화, 상온과 저온 건조공정 그리고 산화시간에 따른 순도와 수율을 측정하여 $NH_4I$ 용액으로부터 요오드를 회수하는 공정의 최적조건을 확립하였다. 또한 산화공정 후 발생하는 여액을 재사용하는 과정을 도입하여 실험한 결과 수율 94.96%, 순도 96.65%의 $I_2$를 회수할 수 있었다.

Keywords

References

  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). https://doi.org/10.1002/pat.3141
  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). https://doi.org/10.1021/ed076p1421
  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). https://doi.org/10.1021/bi00761a013
  10. L. I. Katzin and E. Gebert, Solvent effects in the iodide-iodine-triiodide complex equilibrium, J. Am. Chem. Soc., 76, 2049-2054 (1954). https://doi.org/10.1021/ja01637a006
  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). https://doi.org/10.1021/ja01674a006
  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). https://doi.org/10.1021/ja01527a005
  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). https://doi.org/10.1016/S0967-0637(02)00020-1