DOI QR코드

DOI QR Code

A Study on the Removal of Sulfate in Li2CO3 by Recrystallization

재결정화법을 이용한 탄산리튬 내 황산이온 제거에 관한 연구

  • Kim, Ki-Hun (Department of Advanced Materials Sci. & Eng., Daejin University) ;
  • Cho, Yeon-Chul (Department of Advanced Materials Sci. & Eng., Daejin University) ;
  • Jang, In-Hwan (Department of Advanced Materials Sci. & Eng., Daejin University) ;
  • Ahn, Jae-Woo (Department of Advanced Materials Sci. & Eng., Daejin University)
  • 김기훈 (대진대학교 신소재공학과) ;
  • 조연철 (대진대학교 신소재공학과) ;
  • 장인환 (대진대학교 신소재공학과) ;
  • 안재우 (대진대학교 신소재공학과)
  • Received : 2020.09.28
  • Accepted : 2020.11.18
  • Published : 2020.12.30

Abstract

In order to remove sulfate(SO42-) and purify the Li2CO3, dissolution and recrystallization of crude Li2CO3 using distilled water and HCl solution was performed. When Li2CO3 was dissolved using distilled water, the amount of dissolved Li2CO3(wt.%) increased as the solution temperature decrease and showed about 1.50 wt.% at 2.5℃. In addition, when Na2CO3 was added and the Li2CO3 solution was recrystallized, the recrystallization(%) increased with increasing temperature, resulting in a 49.00 % at 95 ℃. On the other hand, when Li2CO3 was dissolved using HCl solution, there was no effect of reaction temperature. As the concentration of HCl solution increased, the amount of dissolved Li2CO3(wt.%) increased, indicating 7.10 wt.% in 2.0 M HCl solution. When the LiCl solution was recrystallized by adding Na2CO3, it exhibited a recrystallization(%) of 86.10 % at a reaction temperature of 70 ℃, and showed a sulfate ion removal(%) of 96.50 % or more. Finally, more than 99.10 % of Na and more than 99.90 % of sulfate were removed from the recrystallized Li2CO3 powder through water washing, and purified Li2CO3 with a purity of 99.10 % could be recovered.

증류수 및 염산용액을 사용하여 용해 및 재결정화 공정을 통한 탄산리튬 내 황산이온(SO42-) 제거에 관한 연구를 진행하였다. 증류수를 사용하여 탄산리튬 용해 시 용액 온도가 감소할수록 탄산리튬의 용해량이 증가하여 2.5 ℃에서 약 1.50 wt.%의 용해량을 나타내었다. 또한 해당 탄산리튬 용해액을 사용하여 탄산나트륨을 첨가하며 재결정화할 경우, 온도 증가에 따라 재결정화율이 증가하여 95 ℃에서 49.00 %의 재결정화율을 나타내었다. 한편, 염산 용액을 사용한 탄산리튬 용해 시 반응 온도의 영향은 없었으며 염산농도가 증가함에 따라 탄산리튬의 용해량이 증가하여 2.0 M 염산 용액에서 7.10 wt.%를 나타내었다. 또한 이 용액을 사용하여 탄산나트륨을 첨가하며 재결정화를 진행하였을 때 반응 온도 70 ℃에서 탄산리튬의 재결정화율은 86.10 %이었고, 황산이온 제거율은 96.50 % 이상이었다. 이후 수세 과정을 통하여 재결정화된 탄산리튬으로부터 나트륨을 99.10 % 이상, 황산이온을 99.90 % 이상 제거하여 순도 99.10 %의 정제된 탄산리튬을 회수할 수 있었다.

Keywords

References

  1. J. U. Ahn, 2012 : A study on producing lithium carbonate from brine, pp.3-5, Doctoral degree thesis, Chonnam National University, Republic of Korea.
  2. J. E. Lee, H. I. So, Y. C. Jo, et al., 2019 : A study on the separation and concentration of Li from Li-containing waste solutions by electrodialysis, Korean J. Met. Mater, 57(10), pp.656-662. https://doi.org/10.3365/KJMM.2019.57.10.656
  3. C. K. Lee, K. I. Rhee, 2003 : Reductive leaching of cathodic active materials from lithium ion battery wastes, Hydrometallurgy, 68, pp.5-10. https://doi.org/10.1016/S0304-386X(02)00167-6
  4. H. S. Hong, D. W. Kim, H. L. Choi, 2017 : Solvent extraction of Co, Ni and Mn from NCM surfate leaching solution of Li(NCM)O2 secondary battery ccraps, Arch. Metall. Mater., 62(2B), pp.1011-1014. https://doi.org/10.1515/amm-2017-0143
  5. M. S. Lee, S. M. Shin, 2010 : Ionic equilibria and comparison of solvent extraction of Cobalt(II) and Manganese (II) from HCl solution by alamine336, J. of Korean Inst. of Resource Recycling, 19(4), pp.29-34.
  6. J. K. Yang, Y. H. Jin, D. H. Yang, 2019 : A study on the reaction of carbonation in the preparation of lithium carbonate powders, Journal of the Korean Crystal Growth and Crystal Technology, 29(5), pp.222-228.
  7. C. Wei, C. Ruosong, Y. Yurong, 2018 : Removal of SO42- from Li2CO3 by recrystallization in Na2CO3 solution, Crystals, 8(1), p.19. https://doi.org/10.3390/cryst8010019
  8. J. Ahn, Y. Cho, I. Jang, 2020. KR. 10-2085016.
  9. J. E. Lee, 2019 : A study of lithium concentration from lithium-containing waste solution by electrodialysis, p.9, Master's degree thesis, Daejin University, Republic of Korea.
  10. Z. Sha, W. Huang, X. Wang, et al., 2009 : Article 41., Saline Lakes Around the World: Unique Systems with Unique Values, Vol. 15, Aharon Oren, et al., pp.202., University of Utah, Salt Lake City, Utah.