The
Malaysian Journal of Analytical Sciences Vol 11 No 1 (2007): 117 – 123
BIFUNCTIONAL Nb/Ti-MCM-41 CATALYST IN OXIDATIVE
ACIDIC REACTION OF CYCLOHEXENE TO DIOL
Zainab Ramli, Mazidah Abdul Shukor and Didik
Prasetyoko
Dept. of
Chemistry, Faculty of Science, Universiti Teknologi Malaysia,
81310 UTM Skudai,
Johor D.T.
Abstract
Bifunctional
oxidative and acidic catalyst was prepared by incorporating titanium ion (Ti4+)
and niobic acid in mesoporous molecular sieves MCM-41 structure. The catalyst
is active both in oxidation, and acid-catalyzed reaction of olefin to diol. Nb/Ti-MCM-41
catalyst was prepared by first synthesizing Ti-MCM-41 by hydrothermal method,
followed by subsequent impregnation of
niobic acid (Nb) into Ti-MCM-41 at various %wt Nb loading. The framework
structure of Ti-MCM-41 collapsed after incorporation of Nb but the tetrahedral form of Ti4+ still
maintained with octahedral
Nb species . Both Brønsted and
Lewis acid sites
are present in
all Nb/Ti-MCM-41 samples. The formation of cyclohexanediol in the epoxidation of
cyclohexene proved the bifunctional
oxidative and acidic catalyst
through the formation of cyclohexane oxide. The yield increased with the
increase amount of the Brønsted acid sites provided by niobium species .
Keywords:
bifunctional catalyst, Nb/TiMCM-41, oxidative-acidic, diol
References
1. Nowak, I. Ziolek, M. 2005. “Effect of
Texture and Structure on the Catalytic Activity of Mesoporous Niobosilicates
for the Oxidation of Cyclohexene”. Micropor. Mesopor. Mater. 78. 281-288.
2. Nowak, I. Kilos, B. Ziolek, M.
Lewandowska, A. 2003. “Epoxidation of Cyclohexenon Nb-containing Meso and Macroporous
Maetrials”. Catal. Today. 78. 487-498.
3. Didik
Prasetyoko, Salasiah Endud,
Zainab Ramli and
Hadi Nur 2005.
“Enhancement of Catalytic
Activity of
Titanosilicalite-1 – Sulfated
Zirconia Combination Towards
Epoxidation of 1-Octene
with Aqueous Hydrogen Peroxide”. Reaction Kinetics and
Catalysis Letters. 86(1): 83-89,
4. Hadi Nur, Didik Prasetyoko, Salasiah
Endud, and Zainab Ramli. 2004. “Sulfation: a Simple Method to Enhance the Catalytic
Activity of TS-1 in Epoxidation of 1-Octene with Aqueous Hydrogen Peroxide”.
Catalysis Communications. 5: 725-728,.
5. Didik
Prasetyoko, Zainab Ramli,
Salasiah Endud, and
Hadi Nur. 2005.
“Structural and Superacidity
Study of Bifunctional Catalyst,
Sulfated-Titanium/TS-1”. Malaysian Journal of Chemistry. 7(1): 011-018.
6. D. Prasetyoko. Zainab Ramli.
Salasiah Endud. H.
Nur. 2005. “Preparation and
Characterization of Bifunctional Oxidative
and Acidic Catalysts Nb2O5/TS-1 for Synthesis of Diols”. Mater. Chem. Phys .
93. 443-449.
7. Blasco, T. Corma, A. Navarro, M.T.
Pèrez Pariente, J. 1995. “Synthesis, Characterization, and Catalytic Activity
of Ti-MCM-41 Structures”. J. Catal. 156. 65-74.
8 Zecchina, A. Bordiga, S. Spoto,
Lamberti, C, Ricchiardi, G.., Scarano, D., Petrini, G. Leofanti, G. Mantegazza, M. 1996. Structural
chara cterization of Ti
centres in Ti-silicalite and
reaction mechanism in
cyclohexanone ammoximation. Catal Today. 32: 97-106
9. Yu,
Jiangqiang. Feng, Zhaochi.
Xu, Lei. Li,
Meijun. Xin, Qin.
Liu, Zhongmin. Li, Can.
2001. “Ti-MCM-41 Synthesized
from Colloidal Silica and Titanium Trichloride: Synthesis, Characterization and
Catalysis”. Chem. Mater . 13. 994-998.