Fuel, Vol.182, 373-381, 2016
Microwave-dried alpha-Fe2O3 as a highly efficient catalyst for ortho-methylation of phenol with methanol
A novel alpha-Fe2O3 catalyst for the ortho-methylation of phenol with methanol was synthesized by a combination of co-precipitation and microwave drying technologies. The resultant catalyst was characterized by XRD, BET surface area, XPS, TEM, TG-DTG, and NH3-TPD. As compared with air oven dried alpha-Fe2O3 catalyst, the microwave dried one demonstrated larger specific surface area, bigger pore volume, as well as more acidity, and hence exhibited superior catalytic property for the ortho-methylation of phenol with methanol. Under the reaction conditions of 623 K, WHSV 0.8 h(-1), and n(phenol):n(methanol):n(water) = 1:2:0.5, the conversion of phenol on microwave dried alpha-Fe2O3 was 67.0%, 21 percentage points higher than that of oven dried catalyst, the selectivity of o-cresol was 88.5%, and total ortho-selectivity of o-cresol and 2,6-xylenol was nearly constant as 99.7%, that is, almost all methyl group in methanol was guided to ortho-C site of OH group in phenol. The microwave dried alpha-Fe2O3 catalyst could be synthesized with good repeatability, and conveniently reactivated. The catalyst still remained high catalytic activity after continuous 2000 h operation at the temperature from 623 K to 653 K. (C) 2016 Elsevier Ltd. All rights reserved.