Influence of Preparation Parameters on Characteristics of Zirconia-Pillared Clay using Ultrasonic Technique and its Catalytic Performance in Phenol Hydroxylation Reaction

Shobhana Vaman Awate; Suresh Babasaheb Waghmode; Kashinath Rangu Patil; Mangala Shripad Agashe; Praphulla Narahar Joshi

Korean Journal of Chemical Engineering, Vol.18, No.2, 257-262, March, 2001

Shobhana Vaman Awate, Suresh Babasaheb Waghmode, Kashinath Rangu Patil, Mangala Shripad Agashe, and Praphulla Narahar Joshi^†

Catalysis Division, National Chemical Laboratory, Pune 411 008, India

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Ultrasonication method was employed for preparation of zirconia-pillared montmorillonite (Zr-PILC) by using polyhydroxy zirconium cation. The influences of various preparation parameters such as pH, concentration of pillaring agent, aging period on physico-chemical properties of Zr-PILCs are reported. The characterization was done by using different characterizing tools such as powder X-ray diffraction (XRD), thermal analysis (TG/DTA), Fourier transform infrared spectroscopy (FTIR), X-ray photo-electron spectroscopy (XPS), X-ray fluorescence spectroscopy (XRF) and surface area measurements. Effective pillaring was obtained in the pH range 2.0-2.8 at reduced preparation time by using ultrasonication. Ultrasonication, especially at higher pH and concentration of pillaring agent with no aging after ultrasonic agitation of the clay slurry was found to increase zirconium content and specific BET surface area leaving no scope for remarkable increase in d001 spacing. The presence of -OH groups attached to Zr has been revealed by pyridine-adsorbed FTIR, TG/DTA and XPS techniques. The acidic character, ease of accessibility and good dispersion of active sites in Zr-PILC were found to be controlling factors for the challenging activity in hydroxylation reaction of phenol. Probably, this first report on the use of Zr-PILC in hydroxylation of phenol and its preparation by employing ultrasonication technique may attract great attention in the catalysis area of academic and industrial importance.

Keywords:Montmorillonite;Ultrasonication;Zr-Pillared Clay;Hydroxylation of Phenol;Zr-PILC

[References]

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Bartley GJJ, Catal. Today, 2, 233 (1988)
Borade RB, Adnot A, Kalliaguine S, J. Catal., 126, 26 (1990)
Burch R, Warburton CI, J. Catal., 97, 503 (1986)
Clearfield A, Inorg. Chem., 3(1), 146 (1964)
Dongare MK, Singh P, Moghe PP, Ratnasamy P, Zeolites, 11, 690 (1991)
Farfan-Torres EM, Sham E, Grange P, Catal. Today, 15, 515 (1992)
Germain A, Allian M, Figueras F, Catal. Today, 32(1-4), 145 (1996)
Moreno S, Kou RS, Molina R, Poncelet G, J. Catal., 182(1), 174 (1999)
Morterra C, Cerrato G, Langmuir, 6, 1810 (1990)
Notari B, Grobet PJ, Mortier WJ, Vansant EF, Schulz-Ekloff G, Stud. Surf. Sci. Catal., 37, 413 (1989)
Pinnavaia TJ, Tzou M, Landau SD, J. Am. Chem. Soc., 107, 2783 (1985)
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Suzuki K, Horio M, Masuda H, Mori T, Bull. Chem. Soc. Jpn., 64, 732 (1991)
Toranzo R, Vicente MA, Banares-Munoz MA, Gandia LM, Gil A, Microporous Mesoporous Mater., 173, 173 (1998)
Tuel A, Gontier S, Teissier R, Chem. Commun., 651 (1996)
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Zurita PJM, Mireya VG, Goldwasser MR, Rojas D, Garcia JJ, J. Mol. Catal. A-Chem., 107, 175 (1996)

[Referenced By]

[1] Allian M, Germain A, Cseri T, Figueras F, "Heterogeneous Catalysis and Fine Chemicals III," eds., Guisnet, M et al., Elsevier Science Publishers B.V., 455 (1993)

[2] Bartley GJJ, Catal. Today, 2, 233 (1988)

[3] Borade RB, Adnot A, Kalliaguine S, J. Catal., 126, 26 (1990)

[4] Burch R, Warburton CI, J. Catal., 97, 503 (1986)

[5] Clearfield A, Inorg. Chem., 3(1), 146 (1964)

[6] Dongare MK, Singh P, Moghe PP, Ratnasamy P, Zeolites, 11, 690 (1991)

[7] Farfan-Torres EM, Sham E, Grange P, Catal. Today, 15, 515 (1992)

[8] Germain A, Allian M, Figueras F, Catal. Today, 32(1-4), 145 (1996)

[9] Moreno S, Kou RS, Molina R, Poncelet G, J. Catal., 182(1), 174 (1999)

[10] Morterra C, Cerrato G, Langmuir, 6, 1810 (1990)

[11] Notari B, Grobet PJ, Mortier WJ, Vansant EF, Schulz-Ekloff G, Stud. Surf. Sci. Catal., 37, 413 (1989)

[12] Pinnavaia TJ, Tzou M, Landau SD, J. Am. Chem. Soc., 107, 2783 (1985)

[13] Pinnavaia TJ, Tzou MS, Landau SD, Raythatha RH, J. Mol. Catal., 27, 195 (1984)

[14] Suzuki K, Horio M, Masuda H, Mori T, Bull. Chem. Soc. Jpn., 64, 732 (1991)

[15] Toranzo R, Vicente MA, Banares-Munoz MA, Gandia LM, Gil A, Microporous Mesoporous Mater., 173, 173 (1998)

[16] Tuel A, Gontier S, Teissier R, Chem. Commun., 651 (1996)

[17] Vaughan DEW, Lussier RJ, Magee JS, U.S. Patent 4,176,090 (1979)

[18] Wagner CD, Riggs WM, Davis LE, Molder JF, Mullenberg GE, "Handbook of X-ray Photoelectron Spectroscopy," eds. Perkin-Elmer Corporation (1978)

[19] Zurita PJM, Mireya VG, Goldwasser MR, Rojas D, Garcia JJ, J. Mol. Catal. A-Chem., 107, 175 (1996)