A Study on the Synthesis of Aluminum Oxalate from Aluminum Hydroxide

수산화(水酸化)알루미늄으로부터 Aluminum Oxalate의 합성(合成) 연구(硏究)

  • Lee, Hwa-Young (Battery Research Center, Korea Institute of Science & Technology) ;
  • Cho, Byung-Won (Battery Research Center, Korea Institute of Science & Technology)
  • 이화영 (한국과학기술연구원 이차전지연구센터) ;
  • 조병원 (한국과학기술연구원 이차전지연구센터)
  • Published : 2009.08.27

Abstract

The synthesis of aluminum oxalate, one of the aluminum organic compounds, has been performed using aluminum hydroxide as a raw material. For this aim, domestic aluminum hydroxide of 99.7% purity was dissolved by oxalic acid to produce an aqueous aluminum solution. As a result, it was found that aluminum hydroxide could be dissolved almost completely by the reaction with 1.0 mole/l oxalic acid solution at $90^{\circ}C$ for 16 hr. It was strongly required to keep the ratio of ethanol/Al solution more than 2.0 for the synthesis of aluminum oxalate from the aluminum solution. Furthermore, the pH should be controlled to be more than 8.2 in order to obtain the recovery of aluminum oxalate higher than 90%. From the chemical analysis of aluminum oxalate prepared in this work, the content of $NH_4$, Al and C was found to be 14.5, 7.18 and 17.4%, respectively. Accordingly, the aluminum oxalate synthesized from the aluminum solution was confirmed to be $(NH_4)_3Al(C_2O_4)_3$ $3H_2O$.

수산화알루미늄을 원료물질로 하여 알루미늄 유기화합물인 aluminum oxalate 합성실험을 수행하였다. 이를 위해 국산 99.7% 순도의 수산화알루미늄을 옥살산으로 용해하는 방법으로 알루미늄 수용액을 제조하였으며, 실험결과 옥살산 농도 1.0 mole/l, 반응온도 $90^{\circ}C$에서 16시간 용해시 거의 100%에 가까운 용해율을 얻을 수 있었다. 알루미늄 수용액으로부터 aluminum oxalate를 합성하기 위해서는 ethanol/Al solution 혼합비율을 2.0이상으로 유지하여야 하는 것으로 나타났다. 또한, 90% 이상의 회수율을 얻기 위해서는 혼합액의 pH를 8.2이상으로 조절하여야 하는 것으로 나타났다. 합성반응을 통해 얻은 aluminum oxalate의 화학분석결과 $NH_4$ 14.5%, Al 7.18% 및 C 17.4%이었으며, 이의 화학식은 $(NH_4)_3Al(C_2O_4)_3$ $3H_2O$임을 확인할 수 있었다.

Keywords

References

  1. 이화영, 조성백, 2008, 유기산을 이용한 Aluminum Hydroxide의 미량원소 제거연구, 한국자원리싸이클링학회지, 17(5), pp. 44-51
  2. Li, H. et al., 2009: Preparation of a nano-sized a-alumina powder from a supersaturated sodium aluminate solution, Ceramics International, 35, pp. 901-904 https://doi.org/10.1016/j.ceramint.2008.01.030
  3. Dash, B. et aI., 2009: Precipitation (!f boehmite in sodium aluminate liquor, Hydrometallurgy, 95, pp. 297-301 https://doi.org/10.1016/j.hydromet.2008.07.002
  4. Martin, E. S., and Weaver, M. L., 1993: Synthesis and properties of high-purity alumina, American Ceramic Society Bulletin, 72, pp. 71-77
  5. U. S. Patent 4,650,653, 1987: Production of alumina from gibbsite-bearing bauxite of low reactive silica content
  6. Teir, S. et al., 2007: Dissolution of natural serpentinite in mineral and organic acids, Int. J. Miner. Process., 83, pp. 36-46 https://doi.org/10.1016/j.minpro.2007.04.001
  7. Cameselle. C., Nunez, M. J., and Lema, 1. M., 1997: Leaching of kaolin iron-oxides with organic acids, J. Chem. Tech. Biotechnol., 70, pp.349-354 https://doi.org/10.1002/(SICI)1097-4660(199712)70:4<349::AID-JCTB791>3.0.CO;2-4
  8. Hernandez, c., Banza, A. N., and Gock, E., 2007: Recovery of metals from Cuban nickel tailings by leaching with organic acids followed by precipitation and magnetic separation, Journal of Hazardous Materials, B139, pp. 25-30
  9. C. Clar, A. N. Scian, and E. F. Aglietti, 2003: Synthesis and characterilfltWn of aluminum carboxylate gels, Thennochimica Acta, 407, pp. 33-40 https://doi.org/10.1016/S0040-6031(03)00265-X
  10. L. Weng, D. Huang, and X. Jiang, 1993: Synthesis of aluminum nitride from aluminum citrate precursor, Materials Letters, 18, pp. 159-162 https://doi.org/10.1016/0167-577X(93)90118-H
  11. Matzapetakis, M. et al., 1999: Synthesis, structural characterization, and solution behavior of the first monolayer, aqueous aluminum citrate complex, Inorganic Chemistry, 38, pp. 618-619 https://doi.org/10.1021/ic9806131
  12. Matzapetakis, M. et aI., 2001: Synthesis, pH-dependent structural characterization, and solution behavior of aqueous aluminum and gallium citrate complexes, Inorganic Chemistry, 40, pp. 1734-1744 https://doi.org/10.1021/ic000461l