티타니움이 치환된 Silicalite(TS-1)의 제조 및 특성분석

홍은화; 김영남; 정재빈; 이재성; 정종식; 김영걸

HWAHAK KONGHAK, Vol.36, No.6, 908-912, December, 1998

Export Citation

티타니움이 치환된 Silicalite(TS-1)의 제조 및 특성분석

Synthesis and Characterization of Titanium Silicalite-1(TS-1)

홍은화, 김영남, 정재빈, 이재성, 정종식, 김영걸

초록

과산화수소를 이용한 탄화수소의 선택적인 산화반응에 유용한 촉매인 Titanium Silicalite-1(TS-1)의 제조와 특성분석에 관하여 XRD, FT-IR, Raman, TGA, SEM등을 이용하여 연주하였다. XRD를 이용하여 MFI구조의 생성을 확인하였으며, FT-IR은 MFI의 구조 생성과 아울러 그 격자내에 T가 치환되었음을 확인시켜 주었다. Ti의 양이 2.0 atomic %가 넘을 때는 부산물로서 anatase형의 TiO₂가 생성됨을 Raman분광법으로써 확인하였다. 생성된 TS-1은 650℃까지는 열적으로 안정하여 0.25 μm정도의 균일한 입자크기를 가진 원통형 형상을 보였다. 합성과정 중 MFI구조는 170℃의 결정화 과정에서 형성되며 Ti가 silicalite격자내로 치환되는 시기는 550℃의 소성단계였다.

Synthesis and characterization of titanium silicalite-1(TS-1) have been studied by using XRD, FT-IR, Raman, TGA and SEM. The MFI structure of the prepared sample was confirmed by XRD and the results of FT-IR provided evidence of MFI structure and the substitution of Ti into silicalite lattice. When Ti content exceeded 2 atomic %, some Ti formed anatase TiO₂ particles which was characterized by Raman spectroscopy. The product TS-1 was thermally stable up to 650℃ and formed cylinderical particles of uniform size of ca. 0.25 μm. The MFI structure was formed during crystallization step at 170℃ and Ti substitution into silicalite lattice occurred during calcination step at 550℃.

Keywords:Titanium Silicalite-1(TS-1);Characterization;MFI Structure

[References]

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[1] Notari B, "Structure-Activity and Selectivity Relationships in Heterogeneous Catalysis," Elsevier, p. 243 (1991)

[2] Notari B, Catal. Today, 18, 163 (1993)

[3] Thangaraj A, Kumar R, Mirajkar SP, Ratnasamy P, J. Catal., 130, 1 (1991)

[4] Astorino E, Peri JB, Willey RJ, Busca G, J. Catal., 157(2), 482 (1995)

[5] Keshavaraja A, Ramaswamy V, Soni HS, Ramaswamy AV, Ratnasamy P, J. Catal., 157(2), 501 (1995)

[6] Taramasso M, Perego G, Notari B, U.S. Patent, 4,410,501 (1983)

[7] Duprey E, Beaunier P, Springuelhuet MA, Bozonverduraz E, Fraissard J, Manoli JM, Bregeault JM, J. Catal., 165(1), 22 (1997)

[8] Rhee CH, Lee JS, Catal. Today, 38(2), 213 (1997)

[9] Notari B, Adv. Catal., 41, 253 (1996)

[10] Uguina MA, Serrano DP, Ovejero G, Vangrieken R, Camacho M, Appl. Catal. A: Gen., 124(2), 391 (1995)