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Table 2. Physicochemical properties of HB(77), alkali-treated and alkali-acid- treated catalysts. Catalysts HB(77) HB(77)-AT(0.05 M) HB(77)-AT(0.1 M) HB(77)-AT(0.2 M) HB(77)-AT(0.05 M)-NT(0.2 M) HB(77)-AT(0.05 M)-NT(1 M) HB(77)-AT(0.05 M)-NT(2 M) Si/Al a 77 71 51 52 137 116 105 S / BET m2 ̈ g ́1 670 446 360 376 354 374 376 S d / ext m2 ̈ g ́1 170 212 259 300 214 220 210 V c / total cm3 ̈ g ́1 0.64 0.55 0.74 0.77 0.57 0.61 0.56 V d / micro cm3 ̈ g ́1 0.22 0.12 0.05 0.04 0.06 0.07 0.08 Vmeso e / cm3 ̈ g ́1 0.42 0.43 0.69 0.73 0.51 0.54 0.48 Acid Amount b/ mmol ̈ g ́1 0.16 0.14 0.13 0.14 0.08 0.07 0.06 Textual Properties a Molar ratio determined by ICP; b Determined by NH3-TPD; c Total volume for pores below p/p0 = 0.99; d Calculated by t-plot method; e Vmeso = Vtotal ́ Vmicro. The surface area and micropore volume were further decreased after 0.05 M NaOH treatment followed by 0.2 M HNO3 treatment. The possible reason for the decreases is that the framework of zeolite became unstable by alkali treatment, and it would be easily destroyed by the subsequent acid treatment. However, the total volume remained and the mesopore volume slightly increased. 2.1.4. Elemental Analysis As shown in Table 1, the Si/Al ratio of the acid-treated HB(77) samples was gradually increased with an increase in the HNO3 concentration or treatment time. The bulk Si/Al ratio of 160 was achieved by 2 M HNO3 treatment for 16 h. These facts suggest that the direct acid treatment is an efficient dealumination method for Beta zeolite. This may be due to the presence of stacking defects and three dimensional 12-MR channels, which are beneficial to the removal of Al atoms from the framework and/or extra-framework [13]. On the other hand, as shown in Table 2, the Si/Al ratio was slightly decreased to 71 after 0.05 M NaOH treatment. By increasing the NaOH concentration to 0.1 or 0.2 M, the Si/Al ratio was decreased to ca. 50, meaning that the extraction of Si atom was more easily than Al atoms, especially during the higher concentrated NaOH treatment. Note that the Si/Al ratio was drastically increased to 137 after 0.05 M NaOH treatment followed by 0.2 M HNO3 treatment. This result was different from the facts that the Si/Al ratio was slightly increased after the direct HNO3 treatment (Si/Al = 80 for HB(77)-NT(1 M)). Thus, it can be concluded that the alkali treatment even under mild conditions (i.e., 0.05 M NaOH treatment at room temperature for 0.5 h) would lead to the formation of many stacking defects or 83PDF Image | Zeolite Catalysis
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