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hydrolysed into p-HBP. The direct reaction between phenol and BA is also carried out, using BF3 as a Lewis-type catalyst [19]. 2. ResultsandDiscussion 2.1. Characterization of H-Beta Zeolites Table 2 summarizes the main characteristics of the four H-beta zeolites used: the Si/Al ratio (as stated by the supplier), the overall amount of ammonia desorbed (as determined by NH3-Thermal-Programmed -Desorption TPD), and main morphological features. As can be seen, the number of acid sites was not exactly in line with that expected based on the Si/Al ratio; in fact, sample HB-75 had a smaller number of acid sites than HB-150, while the opposite would normally be expected. This seems to be attributable to an overestimation of the number of acid sites in HB-150. Table 2. Main characteristics of the H-beta (HB) and H-Y (HY) zeolites used as catalysts for phenol benzoylation. Si/Al, Overall Atomic Amount of NH3 Ratio Desorbed (mmole NH3/g) 13 0.39 38 0.24 75 0.11 150 0.17 Micropore Volume and Area (cm3/g, m2/g) 0.13, 384 0.15, 421 0.15, 429 0.16, 458 Mesopore Total Total Volume Pore Surface (cm3/g) Volume Area (cm3/g) (m2/g) 0.55 0.70 575 0.94 1.10 636 0.99 1.16 645 0.17 0.38 641 Crystallite Size (nm; from XRD) 18 16 16 27 Nd In regard to the strength of these sites, Figure 1 plots the relative concentration of the Lewis and Brønsted sites, as determined by means of FTIR spectra after pyridine adsorption, taking as reference bands those falling at 1455 and 1545 cm−1, respectively, and using the formula reported in the literature [101]. As can be seen, the sample with the greater Al content showed the higher fraction of strong Lewis sites, which is an expected result based on the fact that the latter is attributable to extra-framework Al species. The strength and relative amount of these Lewis sites decreased when the Si/Al ratio was increased. Conversely, the zeolite with the stronger Brønsted sites was sample H-beta (HB)-150. We also determined the degree of hydrophilicity of samples by means of H2O-TPD; Figure 2 shows that, as expected, the increased Si/Al ratio led to samples with a lower affinity for water; however, the molar ratio between adsorbed H2O Sample HB-13 HB-38 HB-75 HB-150 HY-3 3 1.0* HY-7 7.5 0.1 * HY-100 100 <0.1 * Nd Nd Nd 584 Nd Nd Nd 550* Nd Nd Nd Nd 814 Nd Nd: not determined; * as from the TOSOH website. 121PDF Image | Zeolite Catalysis
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