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ChemEngineering 2019, 3, 35 4 of 11 pressure corresponds to the more stable adsorbate condition and that is why desorption isotherms should be used for pore size analysis [21]. 2.3.4. Morphology The sizes and morphological features of the zeolite catalysts were examined employing a field emission scanning electron microscope (FE-SEM, ZEISS SIGMA, Zaventem, Belgium). A few particles of each untreated and treated ZSM-5 catalyst were separately dispersed in acetone then one drop of the suspended catalyst was put on a sample holder and coated with Pt before analysis to remove the charging effect from the electron beam. 2.3.5. Surface Acidity The temperature programmed desorption-ammonia (NH3-TPD) analysis was conducted by a Micromeritics Auto Chem II analyzer (TPD/TPR, Micromeritics, Norcross, GA, USA) using a thermal conductivity detector (TCD, Thermo Scientific, Mainz, Germany). The zeolite catalyst (0.04 g) was heated to 560 ◦C under helium purge gas at 30 mL·min−1 before carrying out the measurement. The sample was first cooled down to 180 ◦C, and then the ammonia adsorption was conducted for 30 min using an ammonia flow rate of 30 mL·min−1. The catalyst was purged with helium (30 mL·min−1) for 90 min to eliminate un-reacted ammonia on the surface of the catalyst before NH3-TPD measurements. The NH3-TPD measurements of the catalysts were performed by increasing the temperature from 180 to 550 ◦C at 15 ◦C·min−1 heating rate under 30 mL·min−1 of helium purge gas. Once the temperature reached 550 ◦C, the catalyst was held for 30 min. 2.4. Synthesis of p-Methoxypropiophenone “Friedel-Crafts Acylation” Ion exchange for all treated zeolite catalysts was performed before their catalytic performances as follows: 1.0 g of each modified zeolite catalysts was separately stirred in 20 mL of 1.0 M NH4NO3 aqueous solution at 60 ◦C for 6 h. These catalysts were then filtered, washed few times using deionized water, and oven-dried at 60 ◦C overnight followed by calcination at 500 ◦C for 3 h to obtain the final H+ type ZSM-5 (or NH4-ZSM-5). Then, 0.5 g of untreated NH4-ZSM-5 and the treated catalyst was activated at a temperature of 500 ◦C for 3 h in the air before the reaction. 30 mmol of anisole and 30 mmol of propionic anhydride were gently stirred under N2 gas for 10 min. The obtained solution was then poured to a 100 mL batch glass vessel reactor containing the activated catalyst. Afterward, the solution was heated at the temperature of 100 ◦C under reflux and a N2 atmosphere, and vigorously stirred for 24 h. The final product was separated from the catalyst particles by centrifugation for 15 min, and a few mL of the product was then analyzed by off-line GC-MS (gas chromatography equipped with a mass spectroscopy) as follows: Initially, 1.0 μL of the catalyst was injected into the GC at 50 ◦C for 1 min before increasing the temperature to 200 ◦C at 8 ◦C·min−1 rate, after which the temperature was maintained for 35 min. The same procedure was repeated for catalytic reactions performance at different temperatures and all other treated zeolite catalyst with ZSM-5-Na, ZSM-5-C, ZSM-5-T, and ZSM-5-CT. The separated spent catalyst particles were washed repeatedly with deionized water and then calcined for 3 h at 500 ◦C for further investigations in order to assess the catalyst lifetime. The detailed investigations will be reported in the future studies. 3. Results and Discussion 3.1. Zeolite Catalyst Characterizations XRD was used to analyze the crystal structures of untreated and treated zeolite catalysts. The diffraction patterns of all treated zeolite catalysts were similar compared to the untreated zeolite (parent ZSM-5), and all diffraction peaks matched with that of H-ZSM-5 (JCPDS 44-0003). However, the peak intensities of treated zeolite catalysts were slightly reduced, though without any destruction in the framework. Figure 1 shows that some silicon atoms were removed from the framework byPDF Image | Synthesis of Uniform Mesoporous Zeolite ZSM-5 Catalyst
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