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respectively. Then 0.08 g NaAlO2 and 8 mL TPAOH (20 wt % in water) were added to this solution under vigorous stirring. Likewise, 0.76 g NaCl were added, prior to a dilution in 30 mL distilled water. Finally, 6 mL TEOS were added dropwise. The solution was allowed to age for 1h at room temperature and then autoclaved at 170 ̋C during 24, 48 or 72 h. 1.2–1.3 g of ZSM-5 zeolites were obtained after Millipore membrane filtration. The zeolite was dried at 120 ̋C overnight and then calcined at 600 ̋C. X-Ray diffraction (XRD) was performed using an Ultima IV diffractometer (Rigaku, Tokyo, Japan, Cu Kα = 0.1542 nm) at a scanning rate of 0.02 s ́1 in 2θ ranges from 5 to 80 ̋. A fixed power source was used (40 kV, 20 mA). The relative crystallinity of ZSM-5 phase was determined by the area of the peaks at 2θ 23.1 ̋ to 24.1 ̋. The crystallinity was arbitrarily set to 100% for pristine reference zeolites (1 and 2) exhibiting the same crystallinity. Scanning electron microscopy (SEM) micrographs were acquired on a FEG 6700F microscope (JEOL, Tokyo, Japan) working at a 9 kV accelerating voltage. X-Ray fluorescence was carried out to estimate the SAR using a Magic X instrument (Phillips, Almalo, The Netherlands). The textural properties were evaluated using n-hexane adsorption as presented elsewhere [38]. ZSM-5 samples were placed in an 85 μL crucible and analyzed by an Iris TG 209 F1 thermal analyzer (Netzsch, Selb, Germany). Firstly, the sample was pre-treated to remove water (this step comprises heating in N2 flow (60 mL ̈ min ́1) from room temperature to 600 ̋C at 10 ̋ ̈ min ́1 plus 30 min kept at final temperature. Secondly, the sample was cooled to 160 ̋C. Finally, n-hexane adsorption was carried out continuously, followed by weight variation, during cooling from 160 ̋C to 40 ̋C at 4 ̋ ̈ min ́1 under a flow of 8% of n-hexane in N2. Silicon-to-aluminum ratios were determined by XRF. The catalytic cracking of n-hexane (99.89% pure, water 0.005 wt % no volatile residue 0.001% wt/wt from (VETEC/ Sigma-Aldrich Chemistry Ltda., St. Louis, MO, USA) was conducted in a high-throughput unit. Eight reactors in parallel (187 mm in length and 6 mm of internal diameter) made of quartz, with the catalyst localized 90 mm below the top of the reactor, were placed in the middle part of an oven (400 mm external diameter). The temperature was measured by means of a thermocouple located in the center of each reactor and differed less than two degrees between the reactors. All experiments were performed at atmospheric pressure in a continuous down flow fixed-bed micro-reactor. Prior to catalyst evaluation, all the materials were simultaneously heated in nitrogen from room temperature to the reaction temperature (500 or 600 ̋C) at 10 ̋/min. Then, nitrogen was fed through a saturator containing n-hexane at 20 ̋C to the reactors. This procedure ensured a 60 mL/min of 11% v/v n-hexane flow in nitrogen. Since the catalysts were evaluated sequentially, the activation time (at the final temperature) is different for each reactor. This difference did not affect activity and selectivity results. A typical run was carried 234PDF Image | Zeolite Catalysis
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