Transesterification of diethyl malonate with n-butanol over HPWA/MCM-41 molecular sieves
- 341 Downloads
Mesoporous Si-MCM-41 and Al-MCM-41 (Si/Al = 100) materials were synthesized via a hydrothermal method. Three different ratios (10, 20 and 30 wt%) of heteropoly tungstic acid (HPWA) was loaded on Si-MCM-41 by wet impregnation techniques. The characteristic structural features of the prepared materials were studied by various physico-chemical techniques such as X-ray diffraction (XRD), Nitrogen physisorption (BET), temperature programmed desorption of ammonia (TPD) and transmission electron microscopy (TEM). Transesterification of diethyl malonate (DEM) with n-butanol under autogeneous conditions in a temperature range from 50 to 125 °C was selected as the test reaction for the as synthesized materials. The reactants were fed with various mole ratios in order to determine the optimal feed composition leading to maximum yields of transesterified products. The results indicated that the conversion of diethylmalonate depends on the HPWA concentration on the support, temperature, reaction time and mole ratio of the reactants. Further, the catalytic efficiency of HPWA/MCM-41 was compared with that of Al-MCM-41. The solid acid HPWA/MCM-41 catalysts have several advantages in comparison to conventional mineral acid catalysts which are heterogeneous, eco-friendly, highly active and selective in the formation of transesters.
KeywordsHPWA/MCM-41 Transesterification Dietyl malonate n-Butanol
The authors gratefully acknowledge Council of Scientific & Industrial Research (CSIR), New Delhi, India for the financial support. The Bio4Energy programme is acknowledged.
- 4.M. Canakci, V.J. Gerpen, Trans. ASAE 46, 945 (2003)Google Scholar
- 8.A. Demirbas, Energ. Convers. Manage. 50, 923 (2009)Google Scholar
- 9.H. Yazawa, K. Tanaka, K. Kariyone, Tetrahedron Lett. (1974) 3995Google Scholar
- 10.E.C. Blossey, L.M. Turner, D.C. Neckers, Tetrahedron Lett. (1973) 1823Google Scholar
- 15.B.S. Balaji, M. Sasidharan, R. Kumar, B. Chanda, J. Chem. Soc.,Chem. Commun. (1996) 707Google Scholar
- 16.I.V. Kozhevnikov, Catalysts for Fine Chemicals, vol. 2: Catalysis by Polyoxometalates, Wiley, Chichester, England, 2002Google Scholar
- 19.J.B. Moffat, Metal–Oxygen Clusters: The Surface and Catalytic Properties of Heteropoly Oxometalates, Kluwer, New York, 2001Google Scholar
- 22.S. Tural, Turk. J. Chem. 32, 169 (2008)Google Scholar
- 24.H. Iskra, M. Weber, F. Bauer, C. Tice, E. Fiolitakis, Jpn. Kokai Tokkyo Koho JP 2001233823 (2001)Google Scholar