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3.2. Catalyst Preparation and Characterization The desilicated HZSM-5 sample was prepared by heating the parent HZSM-5 (SiO2/Al2O3 of 57) in a 0.5 M NaOH solution (10 mL per gram of zeolite) at 333 K under stirring for 60 min. Pt/HZSM-5 was prepared by impregnating HZSM-5 zeolite with aqueous solutions of H2PtCl6 ̈ 6H2O. The prepared sample was dried at 393 K for 12 h, and then calcined at 773 K for 4 h in air. After calcination, catalysts were ground to a fine powder and pressed into pellets. These pellets were then crushed and sieved to give particles sized 250–400 μm (40–60 mesh). Ni/HZSM-5 and Pt/HBeta were prepared as the same method as Pt/HZSM-5. In this paper, the HZSM-5 (SiO2/Al2O3 of 25, 57 and 107), desilicated HZSM-5 and HBeta (SiO2/Al2O3 of 25) zeolites were denoted as Z-25, Z-57, Z-107, Z-57D, and B-25, respectively. The BET (Brunauer-Emmett-Teller) surface area and pore volume of catalysts were determined by using N2 isothermal (77 K) adsorption on Micromeritics Tristar 3000 physisorption analyzer (Atlanta, GA, USA). The SiO2/Al2O3 ratio of the fresh catalysts was determined using an X-ray Fluorescence spectrometer (Philips Magix PW 2403 XRF, Amsterdam, Holland). NH3-temperature programmed desorption (NH3-TPD) and CO pulse chemisorptions were performed on an Altamira-300 temperature programming unit equipped with a thermal conductivity detector (TCD). The chemical composition, textural properties, calculated dispersion, and NH3 uptake of the parent and desilicated materials are exhibited in Table 5. The coke deposited on the spent catalysts was quantified by thermogravimetry (TGA-Q500, TA, New Castle, DE, USA). The TG experiments were carried out by raising the sample temperature from room temperature up to 1073 K at a rate of 10 K/min in a mixture flow of N2 balance gas (40 mL/min) and air sample gas (40 mL/min). Table 5. Chemical composition, textural properties, NH3 uptake, and calculated dispersion of the catalysts. a Metal Catalysts Content, wt. % Pt/Z-25 1.0 Pt/Z-57 0.6 Pt/Z-57 1.0 Pt/Z-57D 1.0 Pt/Z-107 1.0 Ni/Z-107 10.0 Pt/B-25 1.0 b SiO2 /Al2 O3 29.2 - 50.6 38.6 100.4 - 21.6 c SBET, 2 m /g 334 368 400 342 342 264 503 d V , 3 o e Vm, 3 NH3 Uptake (μmol/g) 959.2 627.6 717.6 513.0 413.8 472.3 938.8 f Calculated Dispersion, % 14.1 13.7 10.4 17.2 18.0 0.6 7.0 cm /g cm /g 0.11 0.11 0.12 0.10 0.11 0.10 0.18 0.10 0.04 0.08 0.12 0.10 0.05 0.18 a Metal content calculated based on the wet impregnating procedure; b The SiO2/Al2O3 ratio was measured by XRF; c SBET is the specific surface area analyzing according to Brunauer-Emmett-Teller method; d Vo is the micropore volume and calculated from the desorption branch of the N2 isotherm; e Vm is the meso-and macropore volumes and calculated from the desorption branch of the N2 isotherm; f Calculated dispersion was measured by CO pulse chemisorption. 219PDF Image | Zeolite Catalysis
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