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Alkylation of p-cresol with tert-butanol catalyzed by heteropoly acid supported on zirconia catalyst
Authors:Biju M. Devassy   G. V. Shanbhag   F. Lefebvre  S. B. Halligudi  
Affiliation:

a Inorganic Chemistry and Catalysis Division, National Chemical Laboratory, Pune 411 008, India

b Laboratorie de Chemie Organometallique de Surface, UMR CNRS-CPE 9986, 43 Bd du 11 November 1918, 69616, Villeurbanne Cedex, France

Abstract:Butylation of p-cresol by tert-butanol was catalyzed by 12-tungstophosphoric acid supported on zirconia (TPA/ZrO2) under flow conditions. Catalysts prepared with different TPA loading (5–30 wt.%) were calcined at 1023 K and acidity was estimated by temperature programmed desorption (TPD) of NH3. Fifteen percent TPA/ZrO2 showed the highest acidity and found to be the most active catalyst in butylation of p-cresol. The effects of temperature, space velocity (LHSV) and molar ratio of the reactants on the conversion of p-cresol and products selectivities were optimized and the optimum reaction conditions evaluated were 403 K, tert-butanol/p-cresol (Bu/Cr) molar ratio 3 and LHSV 4 h−1. Under the optimized conditions, conversion of p-cresol was found to be 61 mol% with product selectivity for 2-tert-butyl-p-cresol (TBC) 81.4%, 2,6-di-tert-butyl-p-cresol (DTBC) 18.1% and tert-butyl-p-tolyl ether (ether) 0.5%. Study of time on stream (TOS) performed as a function of time for 100 h showed that the loss in activity in terms of conversion of p-cresol was 6%.
Keywords:Heteropoly acid   p-Cresol   tert-Butanol   2-tert-Butyl-p-cresol   2,6-Di-tert-butyl-p-cresol   Alkylation
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