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ChemEngineering 2019, 3, 35 3 of 11 water followed by vacuum filtration. Afterward, the collected wet sample was oven-dried at 80 ◦C overnight. This sample was then calcined up to 550 ◦C with a 1 ◦C·min−1 heating rate and oxygen as a purge gas followed by maintaining the temperature of 550 ◦C for a period of 6 h to allow the removal of the remaining surfactant template. The same procedure was repeated for other surfactant templates (CTAB and mixed CTAB and TPAOH) and alkaline solution (NaOH) treatments. Finally, the dried catalysts were labeled, as listed in Table 1. Table 1. Zeolite catalyst coding. Catalysts Untreated zeolite catalyst Treated zeolite with NaOH Treated zeolite with CTAB Treated zeolite with TPAOH Treated zeolite with mixed CTAB and TPAOH 2.3. Characterization Methods 2.3.1. X-Ray Diffraction (XRD) Label Code ZSM-5 ZSM-5-Na ZSM-5-C ZSM-5-T ZSM-5-CT The crystal structure of all prepared zeolite catalysts was identified at room temperature by XRD (Siemens D5000 diffractometer, Siemens AG, Munich, Germany) using Bragg-Brentano geometry, λ = 0.1541 nm CuKα radiation at 40 kV, and a current of 30 mA. Each powder catalyst was loaded onto the sample holder and scanned at 2θ angle range from 5–50◦ with a 0.05◦ angular step size [18]. The average crystallite size of zeolite catalysts was calculated according to the Debye-Scherrer’s formula (see Equation (1)) [19] while the crystallinity was calculated [20] using Equation (2). Crystallite size (D) = kλ/βcos θ (1) where k is a shape factor of the particles (k = 0.9), λ is a wavelength of the CuKα radiation, θ is the incident angle of the X-rays, and β is the full width at half maxima of the diffraction peaks (FWHM). Crystallinity%= ΣIntensityofpeaksofcatalyst ×100 (2) ΣIntensity of peaks of standard 2.3.2. Fourier Transform Infrared (FT-IR) Spectroscopy The functional groups present in the untreated zeolite (parent ZSM-5) and treated zeolite catalysts were examined by FT-IR spectrometer (Perkin Elmer Spectrum One, PerkinElmer, Waltham, MA, USA) at room temperature. At least 36 scans were conducted using an average infrared signal with a resolution of 4 cm−1 within the range of 400–4000 cm−1 and the final output was in transmittance%. The samples were made ready by mixing 5 mg of each zeolite catalyst on 200 mg of KBr pressed into a disk for FT-IR measurement. 2.3.3. Nitrogen Porosimetry The surface area of untreated and treated ZSM-5 catalysts was obtained according to the Brunauer-Emmer-Teller (BET) method using multipoint N2 adsorption-desorption at 77.3 K employing Micromeritics (3FLEX surface characterization) analyzer (Micromeritics Instrument Corporation, Norcross, GA, USA). All catalysts had been pre-treated at 350 ◦C for 4 h under a vacuum to dehydrate the catalysts prior to analysis. In order to calculate the BET surface area, the N2 adsorption isotherms (∆Gads. = RT(lnPads. − lnPo)) data over the relative pressure range of 0.05–0.3 were used for all catalyst samples. However, desorption isotherms (∆Gdes. = RT(lnPdes. − lnPo)) were used to calculate the average pore size and total pore volume for all samples using the Barrett-Joyner-Halenda (BJH) method. Since Pdes. < Pads. it follows that ∆Gdes. < ∆Gads.. Hence, the desorption value of relativePDF Image | Synthesis of Uniform Mesoporous Zeolite ZSM-5 Catalyst
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