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Preparation of Fe2O3 Supported γ-alumina Catalyst by Hydrothermal Method

수열법에 의한 Fe2O3 담지 감마알루미나 촉매제조

  • 박병기 (충남대학교 재료공학과) ;
  • 이정민 (한국화학연구원 화학공정연구센터) ;
  • 서동수 (충남대학교 재료공학과)
  • Published : 2003.07.01

Abstract

The cylindrical ${\gamma}$-alumina pellets were prepared using amorphous alumina and pore generating agent. Its were immersed in aqueous solution of the mixture of Fe(NO$_3$)$_3$.9$H_2O$ and $CH_3$COOH, Fe(NO$_3$)$_3$.9$H_2O$ and $CH_3$COOH and HNO$_3$, and Fe(NO$_3$)$_3$.9$H_2O$ and HNO$_3$. The pellets thus were hydrothermally treated at 20$0^{\circ}C$ for 3 h in autoclave, and were investigated morphologies and changes of crystal pore characteristics, $N_2$ adsorption and desorption isotherms, active sites and mechanical strength etc. According to the preparation method, acicular platelet pseudo-boehmite crystals of 0.1~0.3 ${\mu}{\textrm}{m}$ size were transformed into acicular pseudo-boehmite cristals of 0.5~2 ${\mu}{\textrm}{m}$ size having the same crystal structure. When ${\gamma}$-alumina pellets were immersed in aqueous solution of the mixture of Fe(NO$_3$)$_3$.9$H_2O$ and $CH_3$COOH and then were hydrothermally treated, pore volume between 100 $\AA$ and 1000 $\AA$ was increased from 0.34 ㏄/g to 0.86 ㏄/g, and the gap of $N_2$ adsorption and desorption hysteresis loop was decreased due to increasement of pore size. New active site that could adsorb the C-H functional group was created on the catalist. Also, mechanical strength of catalyst was increased from 1.06 ㎫ to 1.36 ㎫.

비정질알루미나와 기공형성제를 물과 혼합하여 원통형으로 성형하고 수화, 건조 및 소성하여 ${\gamma}$-alumina pellet을 제조하였다. 이를 Fe(NO$_3$)$_3$.9$H_2O$$CH_3$COOH, HNO$_3$ 또는 $CH_3$COOH와 HNO$_3$의 혼합용액에 침척시켜 20$0^{\circ}C$ 온도로 3시간 수열처리 한 다음 결정의 형태 및 변화, 기공특성, $N_2$ 흡/탈착특성, 산점변화 및 기계적 강도 등을 조사하였다. 제조방법에 따라서 0.1~0.3 $mu extrm{m}$ 크기의 작은 결정이 0.5~2 $\mu\textrm{m}$ 길이의 큰 침상결정으로 형태가 변했고, 결정구조는 의사베마이트 또는 ${\gamma}$-alumina 구조를 나타냈다. ${\gamma}$-alumina pellet에 Fe(NO$_3$)$_3$.9$H_2O$$CH_3$COOH 용액을 침적시켜 수열처리 했을 때 촉매와 반응물간의 물질전달이 용이한 100~1000 $\AA$ 사이의 기공부피가 0.34 ㏄/g에서 0.86 ㏄/g으로 크게 증가하였다. 기공크기의 증가로 인해 질소 흡.탈착이 원활히 이루어짐을 알 수 있었으며, C-H 그룹의 관능기를 흡착할 수 있는 새로운 활성점이 형성되었다. 또한 촉매의 기계적 강도도 1.06 ㎫에서 1.36 ㎫로 증가하였다.

Keywords

References

  1. Appl. Ind. Cataly. v.3 Aluminas for Catalysts-their Preparation and Properties P.K.Oberlander
  2. Catalysis and Automotive Pollution Control Alumina Carriers for Automototive Pollution Control P.Nortier;M.Soustelle;A.Crucq(ed.);A.Frennet(ed.)
  3. Key Eng. Mater. v.115 Critical Factors in the Production of Sol-gel Derived Porous Alumina R.B.Bagwell;G.L.Messing https://doi.org/10.4028/www.scientific.net/KEM.115.45
  4. Encyclopedia of Chem. Tech. (4th ed.) v.2 Aluminum Oxide (Hydrate) C.Misra
  5. Ullmann's Encyclopedia of Industrial Chemistry (5th ed.) v.A1 Aluminum Oxide L.K.Hudson;C.Misra;K.Wefers
  6. Physical and Chemical Aspects of Adsorbents and Catalysts v.4 Active Alumina B.C.Lippens;J.J.Steggerda
  7. Alumina Chemicals (2nd ed.) Activated Alumina Desiccants R.D.Woosley;L.D.Hert(ed.)
  8. J. Kor. Ceram. Soc. v.32 no.9 Formation Mechanism of Amorphous Alumina by Rapid Calcination of Gibbsite S.Y.Kim;Y.S.Kim
  9. J. Kor. Ceram. Soc. v.33 no.1 Properties of Amorphous Alumina as Precusor of Catalyst Support S.Y.Kim;Y.S.Kim
  10. J. Coll. Interface. Sci. v.150 no.1 Properties of Activated Alumaina Obtained by Flash Calcination of Gibbsite N.Jovanovic;T.Novakovic;J.Janackovic;A. Terlecki-Baricevic https://doi.org/10.1016/0021-9797(92)90265-N
  11. J. Mat. Sci. v.28 Morphological and Phase Changes of Transition Aluminas During their Rehydration Z.J.Galas;S.Janiak;W.Mista;J.Wrzyszca;M.Zawadzki https://doi.org/10.1007/BF00367564
  12. Ind. End. Chem. Res. v.28 Granulation and Rehydration of Rehydratable Alumina Powders C.C.Huang;H.O.Kono https://doi.org/10.1021/ie00091a005
  13. Appl/Cataly. A:General. v.101 Effect of Acidic and Basic Vapors on Pore Size Distribution of Alumina under Hydrothermal Conditions M. Absi-Halabi;A. Stanislaus;Al-Zaid https://doi.org/10.1016/0926-860X(93)80142-D
  14. J. Kor. Ceram. Soc. v.35 no.10 The Rehy-dration Properties of Amorphous Alumina Power in Low Water/Alumina Ratio B.K.Park;J.K.Suh;J.M.Lee;D.S.Suhr
  15. J. Kor. Ceram. Soc. v.39 no.3 Preparation of High-capacity Ceramic Catalytic Support from Gibbsite B.K.Park;J.K.Suh;J.M.Lee;D.S.Suhr; https://doi.org/10.4191/KCERS.2002.39.3.245
  16. J. Kor. Ceram. Soc. v.39 no.3 Preparation of Zirconia Nanocrystalline Powder by the Hydrothermal Treatment at Low Temperature H.J.Noh;J.K.Lee;D.S.Seo;K.H.Hwang https://doi.org/10.4191/KCERS.2002.39.3.308
  17. J. Kor. Ceram. Soc. v.39 no.10 J.Y.Yun;H.D.Kim;C.H.Park Fabrication of Double-layered Porous Materials https://doi.org/10.4191/KCERS.2002.39.10.919