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Obviously, the HB(12) had the highest acid amount among all the HB samples. In addition, the l-peak and h-peak were seriously overlapped for the HB(12), however, they can be easily separated for the HB(77) (Figure 6). This fact suggests that the HB(12) had a wider distribution of acid strength than the HB(77). As shown in Figure 6B and Table 1, the acid amount was decreased after the HNO3 treatment, indicating dealumination occurred during the acid treatment. Moreover, the acid amount was gradually decreased along with the HNO3 concentration or treatment time. On the other hand, as shown in Figure 7A and Table 2, the acid amount was also decreased after NaOH treatment, indicating dealumination occurred accompanied with desilication during the alkali treatment procedure. Note that the amount of acid of HB(77)-AT(0.2 M) was slightly higher than that of HB(77)-AT(0.1 M) (Figure 7A, Table 2). This may be due to the increase in the LAS generated by the higher concentrated NaOH treatment (see in Section 2.1.6). In addition, the acid amount was further decreased after 0.05 M NaOH treatment followed by HNO3 treatment (Figure 7B, Table 2), suggesting further dealumination. 2.1.6. Pyridine Adsorption FT-IR To clarify the acidic properties in detail, the pyridine adsorption FT-IR spectra of the HB(12), HB(77) and post-treated HB samples were measured. In the region of hydroxyl stretching vibration (Figure 8A), the HB(12) exhibited three main bands at 3781, 3741 and 3603 cm ́1, which are attributed to AlOH hydroxyls, isolated external silanols and structural Si(Al)OH hydroxyls, respectively [29]. The HB(77) exhibited two main bands at 3730 and 3603 cm ́1, which are attributed to isolated internal silanols and structural Si(Al)OH hydroxyls, respectively [29]. After HNO3 treatment, the band at 3603 cm ́1 decreased in intensity, however, the band at 3730 cm ́1 increased. Additionally, HB(77)-NT(2 M, 16 h) showed a broad band at 3700–3500 cm ́1 ascribed to hydrogen-bonded hydroxyl groups [29]. These facts suggest that the silanols were increased by the dealumination with HNO3 treatment. On the other hand, the band at 3603 cm ́1 was slightly decreased in intensity after NaOH treatment (Figure 9A), indicating that the dealumination occurred accompanied by desilication during the alkali treatment. However, the band at 3741 cm ́1 increased in intensity after NaOH treatment. The increase in the isolated external silanols was consistent with the increase in the external surface area after alkali treatment (Table 2). In addition, the band at 3603 cm ́1 further decreased in intensity after 0.05 M NaOH treatment followed by 0.2 M HNO3 treatment, meaning that further dealumination occurred. Note that the band at 3730 cm ́1 decreased in intensity for HB(77)-AT(0.05 M)-NT(2 M). This may be related to the repair of the defect sites by the amorphous Si and/Al species generated by the alkali treatment in the acidic medium [30]. It can also be explained for the increases in its crystallinity, 85PDF Image | Zeolite Catalysis
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