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3.3. Experiment Procedure Experiments were carried out in a continuous-flow tubular fixed-bed reactor made of stainless steel (i.d. = 10 mm, l = 1000 mm), which was described in detail elsewhere [45]. In a typical run, 3 g of catalyst diluted with SiC was packed into the stainless steel reactor, and then reduced at 723 K for 4 h in a flow of H2 (120 mL/min) controlled by a mass flow controller. Reactants (m-cresol or a mixture of m-cresol (p-cresol or guaiacol) with methanol, W/Fm ́cresol = 75 gcat ̈ h/molm ́cresol) were feed through a HPLC pump. The pressure of H2 was 2 MPa and the molar ratio of H2/reagent kept constant at five. The catalyst bed temperature was measured by a K-type thermocouple and maintained using a tube furnace equipped with a temperature controller. The reaction temperature arrived at a heating rate of 5 K/min from room temperature and in this study it changed from 573 K to 723 K. A water-cooled condenser was used to separate condensable from volatile products. The gas product stream was collected in a gas bag. The liquid product was sampled for analysis with an off-line GC. Each experiment was repeated three times, and the results were deviated ca. 4%. A Bruker 456-GC (Karlsruhe, Germany) equipped with BR-5ms column (30 m ˆ 0.25 mm ˆ 0.25 μm) and a flame ionization detector (FID) was used to quantify the liquid products. The GC oven temperature was programmed as follow: maintained 318 K for 2 min, and ramped from 318 K to 523 K with a heating rate of 10 K/min, and finally kept 523 K for 5 min. Standards of known concentration containing observed reactants and products, i.e., a mixture of m-cresol, cylclohexane, toluene, p-xylene, phenol, and 2,4-dimethyl phenol, were used to calibrate the conversion and yield from FID area. Identification of products was carried out by liquid product injections to an Agilent 7890A gas chromatograph (GC) equipped with HP-5ms column (30 m ˆ 0.25 mm ˆ 0.25 μm) and a 5975C mass selective detector (MSD), with temperature starting at 323 K for 5 min, and then 5 K/min up to 443 K and, lastly, dwelling at 443 K for 2 min. Each sample was analyzed at least twice, and the deviation error of analysis was about ̆1%. The W/F (catalyst weight/molar feed flow rate) values reported were found by dividing the total weight of catalyst in the reactor bed by the molar flow rate of m-cresol (or other kinds of lignin-based phenols) injected during a given experiment. Product selectivity is defined as the mass fraction of the material in the total product. 4. Conclusions A novel method of high-selectively catalytic hydrodeoxygenation and methylation of lignin-based phenols into xylenes was explored over a series of Pt/HZSM-5 under H2. A maximum p-/m-xylene selectivity of 33.5% was obtained at the m-cresol/methanol molar ratio of 1/8, which was two times as much as that without methanol. The improved p-/m-xylene selectivity with methanol was 220PDF Image | Zeolite Catalysis
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