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Zeolite Catalysis

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Zeolite Catalysis ( zeolite-catalysis )

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3. ExperimentalSection 3.1. Catalyst Preparation The representative nano-ZSM-5/SBA-15 analog composite, pre-crystallized for 24 h (denoted as ZSC-24), was prepared according to the synthesis procedure as reported in the previous work [14]. Briefly, the zeolite seed solution was pre-crystallized for 24 h to partially form nano-ZSM-5 crystals and then added to the surfactant solution to convert unreacted precursors into an ordered mesoporous SBA-15 analog. Finally, the resulting nano-ZSM-5/SBA-15 analog composite (ZSC-24) was activated by protonation. For comparison, Al-SBA-15 was prepared under the same conditions as for synthesis of ZSC-24, but using conventional silica-based precursors instead of pre-formed seeds. Additionally, commercial H-ZSM-5 (Zeocat PZ-2/25, ZeoChem AG, Uetikon am See, Switzerland) was used to provide a benchmark. All catalyst samples used in this study were fresh since they provide a better understanding of structure, property, and function relationships. 3.2. Catalyst and Feedstock Characterization The nitrogen physisorption studies were carried out at −196 ◦C with an ASAP 2010 apparatus (Micromeritics GmbH, Aachen, Germany). The temperature-programmed desorption of ammonia (NH3-TPD) measurements using TCD detector (TCD, GOW-MAC Instrument Co., Bethlehem, PA, USA) were performed in a homemade set-up using a quartz tube reactor in the range of 100–550 ◦C. The Al and Si contents were determined by inductively coupled plasma atomic emission spectroscopy (ICP-AES; 715-ES, Varian, Inc., Palo Alto, PA, USA) and atomic absorption spectroscopy (AAS; Analyst 300, PerkinElmer, Inc., Waltham, MA, USA), respectively. More details of these characterization methods and experiment parameters are described elsewhere [14,20]. The fatty acid compositions of technical grade triolein (obtained from Santa Cruz Biotechnology, Inc, Heidelberg, Germany) and waste cooking oil (collected from a local restaurant) were analyzed on a gas chromatography-mass spectrometry combination (GC-MS; QP2010S, Shimadzu Europa GmbH, Duisburg, Germany). For this purpose, a derivatization was carried out with trimethylsulfonium hydroxide solution (0.25 M in methanol, Fluka, Sigma-Aldrich Chemie GmbH, Taufkirchen, Germany) to transform triglycerides completely into methyl esters. The C, H, N elemental analysis of triolein and WCO was performed on a TruSpec CHNS Micro analyser (Leco Instrumente GmbH, Mönchengladbach, Germany). 3.3. Catalyst Tests The fixed bed microactivity test equipment (MAT) is widely used for studying catalytic cracking at the laboratory scale. However, the traditional MAT unit provides 201

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