NH4I 용액으로부터 고효율/고순도의 요오드 회수 공정개발에 관한 연구

윤종선; 임성빈; 오세용; Jong Sun Yoon; Seong Bin Lim; Se Yong Oh

Applied Chemistry for Engineering, Vol.26, No.3, 377-380, June, 2015

DOI10.14478/ace.2015.1040 Export Citation

NH4I 용액으로부터 고효율/고순도의 요오드 회수 공정개발에 관한 연구

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

윤종선, 임성빈, 오세용 ^†

서강대학교 화공생명공학과

Jong Sun Yoon, Seong Bin Lim, and Se Yong Oh^†

Department of Chemical & Biomolecular Engineering, Sogang University, Seoul 121-742, Korea

E-mail:

초록

본 연구에서는 p-diiodobenzene (PDIB)으로부터 p-phenylenediamine (PPD) 합성 후 생성되는 부산물인 NH4I를 PDIB 합성의 원료로 재활용하기 위하여 I2 회수 공정의 최적화에 관한 연구를 진행하였다. 양이온교환수지를 사용하여 NH4I 시약 용액으로부터 I2 회수에 관한 연구를 진행하였고 양이온교환수지의 파과곡선을 통해 파과점 및 관류교환용량을 조사하였다. 회수되는 요오드의 수율 및 순도 향상을 위해 NH4I의 공급용액 및 산화제(H2O2)의 농도 변화, 상온과 저온 건조공정 그리고 산화시간에 따른 순도와 수율을 측정하여 NH4I 용액으로부터 요오드를 회수하는 공정의 최적조건을 확립하였다. 또한 산화공정 후 발생하는 여액을 재사용하는 과정을 도입하여 실험한 결과 수율 94.96%, 순도 96.65%의 I2를 회수할 수 있었다.

In this paper, we have investigated the optimization of I2 recovery process from NH4I solution, which is generated as by-product during the amination reaction of p-diiodobenzene (PDIB) for p-phenylenediamine (PPD) synthesis. The recovered I2 is then recycled as a raw material for PDIB synthesis. We have employed a cation exchange resin to recover I2 from NH4I sample solution, and determined the breakthrough point and exchange capacity from the breakthrough curve. Furthermore, we have suggested optimum conditions of our I2 recovery process by measuring the purity and yield of recovered I2 with respect to the concentrations of NH4I and oxidant (H2O2) 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.

Keywords:iodine recovery process;cation exchange resin;ammonium iodide;PPD;PDIB

[References]

Stojanovic DB, Zrilic M, Jancic-Heinemann R, Zivkovic L, Kojovic A, Uskokovic PS, Aleksic R, Polym. Adv. Technol., 24, 772 (2013)
Han IS, Method of making aramid fiber, Korea Patent 10-0910537 (2009).
Shin YJ, Kim JC, Lim JB, Lee DJ, Preparation method for para phenylene diamine, Korea Patent 10-2012-0018950 (2012).
Joo YJ, Kim JU, Won JI, A novel method of preparing p-phenylenediamine, Korea Patnet 10-0362772 (2000).
Lee JS, Removal of Phosphate with Ion Exchange Resins, Master Dissertation, Gyeongsang National Uinversity, Jinjoo, Korea (2011).
Park KG, Ion Exchange Resins for Treatment and Reuse of Chromium Rinse Wastewater from Thin Metal Sheet, Master Dissertation, Yeungnam University, Daegu, Korea (2005).
Han JS, Choi RI, Park CJ, Noh HR, Kim BG, Kim SY, Ahn JY, Kang CG, Jung IW, Lee JC, Evaluation of acid deposition and impact assessment in Korea, National Institute of Environmental Research., 21, 119-136 (1999).
Silva CR, Simoni JA, Collins CH, Volpe PLO, J. Chem. Educ., 76, 1421 (1999)
Roman R, Dunford HB, Biochemistry, 11, 2076 (1972)
Katzin LI, Gebert E, J. Am. Chem. Soc., 76, 2049 (1954)
Kolthoff IM, J. Am. Chem. Soc., 46, 2009 (1924)
Lee SB, Park IJ, Kim DK, Kim JH, Lee KW, Ha JW, Kim KJ, Lee HD, Jung JK, Lim JH, Method for Iodine recovery from nitrogen compound solution using an ion exchange resin, Korea Patent 10-0434725 (2004).
Shirley DA, Giauque WF, J. Am. Chem. Soc., 81, 4778 (1959)
Johnson KS, Coletti LJ, Deep-Sea Res. I, 49, 1291 (2002)

[Related Articles]

[1] Stojanovic DB, Zrilic M, Jancic-Heinemann R, Zivkovic L, Kojovic A, Uskokovic PS, Aleksic R, Polym. Adv. Technol., 24, 772 (2013)

[2] Han IS, Method of making aramid fiber, Korea Patent 10-0910537 (2009).

[3] Shin YJ, Kim JC, Lim JB, Lee DJ, Preparation method for para phenylene diamine, Korea Patent 10-2012-0018950 (2012).

[4] Joo YJ, Kim JU, Won JI, A novel method of preparing p-phenylenediamine, Korea Patnet 10-0362772 (2000).

[5] Lee JS, Removal of Phosphate with Ion Exchange Resins, Master Dissertation, Gyeongsang National Uinversity, Jinjoo, Korea (2011).

[6] Park KG, Ion Exchange Resins for Treatment and Reuse of Chromium Rinse Wastewater from Thin Metal Sheet, Master Dissertation, Yeungnam University, Daegu, Korea (2005).

[7] Han JS, Choi RI, Park CJ, Noh HR, Kim BG, Kim SY, Ahn JY, Kang CG, Jung IW, Lee JC, Evaluation of acid deposition and impact assessment in Korea, National Institute of Environmental Research., 21, 119-136 (1999).

[8] Silva CR, Simoni JA, Collins CH, Volpe PLO, J. Chem. Educ., 76, 1421 (1999)

[9] Roman R, Dunford HB, Biochemistry, 11, 2076 (1972)

[10] Katzin LI, Gebert E, J. Am. Chem. Soc., 76, 2049 (1954)

[11] Kolthoff IM, J. Am. Chem. Soc., 46, 2009 (1924)

[12] Lee SB, Park IJ, Kim DK, Kim JH, Lee KW, Ha JW, Kim KJ, Lee HD, Jung JK, Lim JH, Method for Iodine recovery from nitrogen compound solution using an ion exchange resin, Korea Patent 10-0434725 (2004).

[13] Shirley DA, Giauque WF, J. Am. Chem. Soc., 81, 4778 (1959)

[14] Johnson KS, Coletti LJ, Deep-Sea Res. I, 49, 1291 (2002)