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pattern was slightly broadened and the center of the peak was slightly shifted to the low value after the acid treatment (Figure 4B). On the other hand, the alkali-treated HB(77), especially HB(77)-AT(0.2 M), displayed a new weak hysteresis loop at P/P0 of 0.5–0.9, indicating that new mesopores were formed by NaOH treatment (Figure 5A). Correspondingly, the peaks in the pore size distribution pattern were broadened, suggesting the presence of inhomogeneous mesopores (Figure 5B). The isotherms of the alkali-acid-treated HB, especially HB(77)-AT(0.05 M)- NT(1 M), showed increasing step due to multilayer adsorption at P/P0 (>0.5) and slightly enlarged hysteresis loops at P/P0 of 0.5–0.9, indicating that the mesopores were increased by the subsequent HNO3 treatment. A reason may be that amorphous Si and/or Al species formed by alkali treatment were partially removed by the subsequent acid treatment. Correspondingly, broad peaks centered at ca. 3–4 nm in the pore size distribution pattern were also observed for the alkali-acid-treated HB(77) samples (Figure 5B). The textural properties of all HB samples obtained from N2 adsorption isotherms are listed in Tables 1 and 2. Both of the HB(12) and HB(77) had high surface area, micropore volume and external surface area. After HNO3 treatment, the surface area and the micropore volume of acid-treated HB(77) were slightly decreased, while the external surface area was slightly increased (Table 1). Table 1. Physicochemical properties of HB(12), HB(77) and acid-treated HB catalysts. Catalysts HB(12) HB(77) HB(77)-NT(1 M, 1 h) HB(77)-NT(2 M, 1 h) HB(77)-NT(2 M, 16 h) SBET / m2 ̈ g ́1 510 670 650 611 590 Sext d / m2 ̈ g ́1 157 170 176 200 210 Vtotal c / cm3 ̈ g ́1 0.61 0.64 0.63 0.62 0.61 Vmicro d / cm3 ̈ g ́1 0.18 0.22 0.20 0.18 0.17 Vmeso e / cm3 ̈ g ́1 0.43 0.42 0.43 0.44 0.44 Acid Si/Al Amount b/ a mmol ̈g ́1 12 0.76 77 0.16 80 0.16 104 0.12 160 0.07 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. On the other hand, the surface area and micropore volume were decreased after the 0.05 M NaOH treatment, while the external surface area was slightly increased. Note that the total pore volume was slightly decreased, however, the mesopore volume was almost unchanged (Table 2). By increasing the NaOH concentration to 0.1 or 0.2 M, the total volume and mesopore volume increased, meaning that a large amount of mesopores were formed by these treatments. However, the surface area and micropore volume were further decreased, suggesting the severe destruction of structure (Table 2). 82PDF Image | Zeolite Catalysis
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