Journal of the Korean Ceramic Society (한국세라믹학회지)

The Korean Ceramic Society (한국세라믹학회)
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Preparation of Porous Boehmite Gel from Waste AlCl3 Solution

AlCl3 폐액으로부터 다공성 Boehmite Gel의 제조

  • 박병기 (한국화학연구원 화학공정연구센터) ;
  • 이학수 (충남대학교 정밀공업화학과) ;
  • 김영호 (충남대학교 정밀공업화학과) ;
  • 이정민 (한국화학연구원 화학공정연구센터)
  • Published : 2004.11.01
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Abstract

Porous pseudo-boehmite gel was prepared through the aging process of amorphous aluminum hydroxides gel precipitated by the hydrolysis reaction of dilute NaOH solution and AlCl$_3$ solution. In this study, the synthesis method was studied on porous pseudo-boehmite gel having maximum pore volume, as being investigated the changes of crystal structure, infrared rays absorption spectrum, BET surface area and pore structure when the hydrolysis reaction is controlled in the range of pH 7.6~11.6 and the aging process is hold up for 2~24 h at 60~10$0^{\circ}C$. We could find that the gel precipitates deposited in in range of pH 7.6~9.6 were developed into porous pseudo-boehmite which surface area was 250~357 $m^2$/g, pore volume was 0.4~0.7 cc/g and average pore size was 58~l14$\AA$. However, the gel precipitates deposited in range of pH 10.6~11.6 were developed into bayerite which pore volume was very little.

폐 염화알루미늄(AlCl$_3$) 수용액과 수산화나트륨(NaOH) 용액의 가수분해 반응에 의해 무정형의 수산화알루미늄 겔을 석출시키고, 이를 숙성하여 다공성 유사베마이트(pseudo-boehmite) 겔을 제조하였다 pH를 7.6～11.6 범위로 조절하고 반응온도를 60～10$0^{\circ}C$로 변화시켜 2～24시간 숙성시켰을 때, 겔 침전물의 결정변화, 적외선흡수스펙트럼의 변화, 비표면적 및 기공구조의 변화를 조사하여 최대 기공부피를 갖는 유사베마이트 겔의 제조조건을 확립하였다. pH 7.6～9.6 범위에서 석출된 겔 침전물로부터 250～357 $m^2$/g 정도의 비표면적과 0.4～0.74 cc/g의 기공부피 그리고 58～l14$\AA$의 평균기공크기를 갖는 다공성 유사베마이트가 제조되었으며, pH 10.6～11.6 범위에서 석출된 겔 침전물로부터는 기공이 거의 없는 베이어라이트(bayerite)가 제조되었다.

Keywords

References

  1. R. K. Oberlander, 'Aluminas for Catalysts-their Preparation and Properties,' Appl. Ind. Catalysis, 3 63 (1984)
  2. P. Nortier and M. Soustelle, 'Alumina Carriers for Automotive Pollution Contro,' Catalysis and Automotive Pollution Control, ed. by Crucq and A. Frennet, Elsevier Sci. Pub. 275 (1987)
  3. R. B. Bagwell and G. L. Messing, 'Critical Factor in the Production of Sol-Gel Derived Porous Alumina,' Key Eng. Mater., 115 45-64 (1996) https://doi.org/10.4028/www.scientific.net/KEM.115.45
  4. C. Misra, 'Aluminum Oxide (Hydrate),' Encyclopedia of Chem. Tech., 4th ed., 2 317 (1992)
  5. L. K. Hudson, C. Misra, and K. Wefers, 'Aluminum Oxide,' Ullmann's Encyclopedia of Ind. Chem., 5th ed., A1 557 (1985)
  6. B. C. Lippens and J. J. Steggerda, 'Active Alumina,' Phys. and Chem. Aspects of Adsorbents and Catalysts, 4 171 (1970)
  7. R. Dale Woosley, 'Activated Alumina Desiccants,' Alumina Chem., 2nd ed. Am. Ceram. Soc., 241 (1990)
  8. C. N. Satterfield, 'Heterogeneous Catalysis in Practice,' Mcgraw Hill (1980)
  9. W. A. Deer, R. A. Howie, and J. Zussman, 'Rock Forming Minerals,' Longmans, London, 5 111-16 (1969)
  10. L. Farkas, P. Gado, and P. E. Wermer, Mat. Res. Bull., 12 1213-18 (1977) https://doi.org/10.1016/0025-5408(77)90176-3
  11. B. K. Park, J. K. Suh, J. M. Lee, and D. S. Suhr, 'The Rehydration Properties of Amorphous Alumina Powder in Low Water/Alumina Ratio,' J. Kor. Ceram. Soc., 35 [10] 1085-93 (1998)
  12. K. Okada and T. Nagashima, 'Relationship between Formation Conditions, Properties, and Crystalline Size of Boehmite,' J. Colloid and Int. Sci., 253 308-14 (2002) https://doi.org/10.1006/jcis.2002.8535
  13. K. H. Lee and B. H. Ha, 'Preparation and Characteristic for $\gamma$-Alumina,' J. Kor. Chem. Eng., 34 [1] 28-35 (1996)
  14. J. A. Gadsden, 'Intrared Spectra of Minerals and Related Inorganic Compounds,' Batterworths, Reading, Mass (1975)
  15. K. Nakamoto, 'Infrared and Raman Spectra of Inorganic and Coordination Compounds,' Wiley, New York (1978)
  16. K. H. Lee and B. H. Ha, 'Preparation and Characteristic for $\gamma$-Alumina,' J. Kor. Ins. Chem. Eng., 34 [1] 28-35 (1996)
  17. J. A. Gadsden, 'In Frared Specpra of Minerals and Related Inorganic Compounds,' Batte Rworths, Reading, Mass. (1975)
  18. U. Y. Hwang, S. W. Lee, H. S. Park, K. K. Koo, S. J. Yoo, H. S. Yoon, and Y. R. Kim, 'Synthesis of Porous $Al_2O_3$ Particles by Sol-Gel Method,' J. Kor. Chem. Eng., 39 [2] 199-205 (2001)
  19. B. K. Park, J. K. Suh, J. M. Lee, and D. S. Suhr, 'Preparation of High-Capacity Ceramic Catalytic Support from Gibbsite,' J. Kor. Ceram. Soc., 39 [3] 245-51 (2002) https://doi.org/10.4191/KCERS.2002.39.3.245
  20. J. T. Kim, M. C. Kim, and W. H. Nam, 'Characterization of OH Groups on Alumina by Infrared Spectroscopy,' J. Kor. Chem. Eng., 25 [3] 229-36 (1987)
  21. Z. J. Galas, S. Janiak, W. Mista, J. Wrzyszcz, and M. Zawadzki, 'Morphological and Phase Changes of Transition Aluminas During their Rehydration,' J. Mat. Sci., 28 2075-78 (1993) https://doi.org/10.1007/BF00367564