Synthesis and characterization of mesoporous Si-MCM-41 materials and their application as solid acid catalysts in some esterification reactions

• Published in: Bulletin of materials science Vol. 37; no. 3; pp. 609 - 615
• Main Authors: Parangi, Tarun F, Patel, Rajesh M, Chudasama, Uma V
• Format: Journal Article
• Language: English
• Published: India Springer India 01.05.2014; Springer Nature B.V
• Subjects: Acetates; Aluminum; Ammonia; Catalysis; Catalysts; Chemical analysis; Chemistry and Materials Science; Emission analysis; Engineering; Esterification; Ethyl acetate; High temperature; Inductively coupled plasma; Materials Science; Pore size; Pore size distribution; Reagents; Room temperature; Silicon; Sol-gel processes; Spectroscopy; Surface area; Surface stability; Thermal stability; solid acid catalyst; Mesoporous material; heteropoly acid anchored onto MCM-41; esterification; Al-MCM-41; Si-MCM-41
• ISSN: 0250-4707; 0973-7669
• DOI: 10.1007/s12034-014-0709-7

Mesoporous MCM-41 has been synthesized by sol–gel method at room temperature possessing good thermal stability, high surface area as well as retention of surface area at high temperature. The MCM-41 neutral framework has been modified and put to practical use by incorporating Al 3+ in the siliceous MCM-41 framework and supporting 12-TPA (12-tungstophosphoric acid) onto MCM-41 by process of anchoring and calcination to induce Brønsted acidity in MCM-41 to yield Al-MCM-41 and 12TPA-MCM-41, respectively. The synthesized materials have been characterized for elemental analysis by ICP-AES, XRD, SEM, TEM, EDX, FT–IR and TGA. Surface area has been determined by BET method and pore size and pore size distribution determined by BJH method. Surface acidity has been evaluated by NH 3 -TPD method. The potential use of Al-MCM-41 and 12TPA-MCM-41 as solid acid catalysts has been explored and compared by studying esterification as a model reaction wherein monoesters such as ethyl acetate (EA), propyl acetate (PA), butyl acetate (BA) and benzyl acetate (BzA) have been synthesized, optimizing several parameters such as catalyst amount, reaction time, reaction temperature and mole ratio of reagents.