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ChemEngineering 2019, 3, 35 7 of 11 Table 3. N2 adsorption-desorption isotherms of untreated and treated zeolites. ChemEngineering 2019, 3, x FOR PEER REVIEW Catalysts SBET * Vp ** t-Plot Values External Surface 7 of 11 The particle size and morphologies of treated and untreated zeolite catalysts were observed by Micropore Area (m2·g−1) SEM as shown in Figure 4. It can be observed from the SEM images that very tiny particle with unclear (m2 ·g−1 ) (mL·g−1 ) ZSM-5 279 ± 1.6 0.18 1.7 ± 0.1 55 0.13 Dp *** (nm) V (cm3·g−1) ZSM-5-Na 328 ± 1.2 0.26 3.7 ± 0.1 65 0.08 shapes, within a few nm size ranges, agglomerate with each other to form irregular clusters with ZSM-5-T 390 ± 1.9 0.23 11.1 ± 0.1 60 0.12 different morphologies. In order to observe the clear morphologies and confirm the mesoporosity of ZSM-5-C 395 ± 2.5 0.37 14.9 ± 0.1 300 0.06 the zeolite catalyst, a high‐resolution transmission electron microscopy analysis must be performed. ZSM5-CT 419 ± 2.0 0.34 15.2 ± 0.1 200 0.08 The results indicate that most of the crystals keep their shapes after treatments. However−,1some * SBET: BET surface area estimated using 0.05–0.3 relative pressure range; ** Vp: total pore volume (mL·g ) surfawceasrocaulcguhlantedssawt Pa/sPob=se0r.9v9e;d**i*nDtph:emSEeaMn pimoreagsiezse.(Tnhme)sestriemsauteltdsbmyautscihngwtehellBwJHithmtohdelrefrsoumltsNo2fthe desorption isotherm. literature [27]. 500 nm 500 nm 500 nm 500 nm 500 nm Figure 4. SEM images for (a) ZSM-5, (b) ZSM-5-Na, (c) ZSM-5-C, (d) ZSM-5-T and (e) ZSM-5-CT. Figure 4. SEM images for (a) ZSM‐5, (b) ZSM‐5‐Na, (c) ZSM‐5‐C, (d) ZSM‐5‐T and (e) ZSM‐5‐CT. 3.2. Catalytic Performance 3.2. Catalytic Performance The reaction of anisole and propionic anhydride was conducted with untreated zeolite (parent The reaction of anisole and propionic anhydride was conducted with untreated zeolite (parent ZSM-5) and treated zeolite catalysts (ZSM-5-Na, ZSM-5-T, ZSM-5-C, and ZSM-5-CT) as shown in ZSM‐5) and treated zeolite catalysts (ZSM‐5‐Na, ZSM‐5‐T, ZSM‐5‐C, and ZSM‐5‐CT) as shown in Scheme 1. The main product obtained in this acylation reaction was p-methoxypropiophenone. Scheme 1. The main product obtained in this acylation reaction was p‐methoxypropiophenone. It was It was found that the untreated zeolite and treated zeolites showed selective characteristic towards found that the untreated zeolite and treated zeolites showed selective characteristic towards para para orientation isomer instead of other orientation (ortho and meta) isomers because of its smaller orientation isomer instead of other orientation (ortho and meta) isomers because of its smaller molecular sizes in comparison to its counterpart ortho or meta position isomers. This agrees with other molecular sizes in comparison to its counterpart ortho or meta position isomers. This agrees with reported studies on the selectivity of zeolite catalysts towards the para position for many instances of other reported studies on the selectivity of zeolite catalysts towards the para position for many aromatic acylation [28,29]. The anisole conversion was found to be 40, 56, 76, 88, and 90%, with the instances of aromatic acylation [28,29]. The anisole conversion was found to be 40, 56, 76, 88, and 90%, product selectivity toward p-methoxypropiophenone being 60, 66, 83, 94 and 96%, respectively. This with the product selectivity toward p‐methoxypropiophenone being 60, 66, 83, 94 and 96%, revealed that the amount of anisole conversion increases with the increasing BET surface area and respectively. This revealed that the amount of anisole conversion increases with the increasing BET surface area and average pore size. In addition, the surface acidity of the zeolite catalysts may have an important role in anisole’s high conversion with more selectivity towards the product. Figure 5 shows two resulting peaks that correlated to the two different types of active acid sites. The high‐ temperature peak was attributed to the desorption of ammonia from strong Brønsted and Lewis acidic sites [30]. Furthermore, the low‐temperature peak was attributed to ammonia weakly held orPDF Image | Synthesis of Uniform Mesoporous Zeolite ZSM-5 Catalyst
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