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the O–H stretching modes in Si–O–H and/or O–H groups on the surface of the zeolite catalysts [22]. The broad weak band around 3475 cm−1 was assigned to the stretching vibration of the O–H bond in silanol groups (Si–O–H) but could be due to the adsorbed water (H–O–H) molecules on the surface of silica. The band at 3142 cm−1 was assigned to the stretching vibration of the hydroxyl (O–H) group of water molecules and amines (N–H) present in the pores of the zeolites [22]; bands at 1639 cm−1 ChemEngineering 2019, 3, 35 6 of 11 were attributed to the O–H bending vibration of water molecules [23]. The band at 1400 cm−1 in untreated zeolite may be affected by characteristics peak of NH4+ and a similar band has been observed for treated zeolites after the ion exchange process [24]. Bands at 1227 and within the range It can be seen from the isotherm in Figure 3a(iv,v) that there were two steps with increased volume of 1070 to 1150 cm−1 were referred to the external asymmetric stretch and the internal asymmetric which occurred at the P/Po values of 0.2 and 0.4. Figure 3b(ii,iv,v) show that ZSM-5-C has an average posrteresticzhe of Tca–.O1–4T.9, rnemspewcthivereelya.sTZhSeMb-a5n-dT atn7d93ZcSmM-5c-oCrTrehspavonedcead.11to.1thaendex1te5r.2nanlmsyamvmereatgriecpstorreetch ChemEngineering 2019, 3, x FOR PEER REVIEW −1 6 of 11 −1 sizoefs,Tr–eOsp–eTc,tiavnedly.thTahteamt 4e5s5opcmorouwsasstrduucetutroetihsepTre–sOenbtetnhdro(uwgheoruetTth=eSzieorlitAelc)awtahliycsht aisntdypfoicramllsyafor higthleTyh5ien‐ftsoeulrdprfearncinetgrasarteoinaf,ghpaiognrhdelyusnisziifelosicr, emaonupdsorpmoouarsteenrveioatwlus,omrwke.hs Iefnroecraosanltltrhuaesntft, rtaehameteisdwotoahrnekdrmvtriboearf atethideonuzenaotrloeituaetnecdatz5ae5loy0lsitctsem−1 wcaet(radeloydustebtilesertmryipningicesad)liosufcsmihnaigrcarNoctp2eoraridsotsuiocsrompftaiMotenFr‐Iid‐atelyspoherapzvteinoglnitheisisgo[ht2h5ae]dr.msosr.pFtiognuraet l3oaw(i)reillautisvtreaptersestshuereusn. treated ZSM‐5 exhibits Type I adsorption isotherm, while Figure 3a(iii) ZSM‐5‐Na displays Type IV ads(oar)ption isotherm with a hysteresis loop type H3 of pl(abt)e‐like particles, which gives rise to the slit‐ shaped pores. A hysteresis loop was seen during the desorption measurements in the case of ZSM‐5‐ Na, strongly suggesting the formation of mesoporous ZSM‐5 in comparison to the other materials reported mesoporous materials [26]. Furthermore, the synthesized ZSM‐5‐T can be classified as Type IV with a hysteresis loop type H2 that is associated with a capillary condensation in the bottle‐pore shape. On the other hand, the synthesized catalysts ZSM5‐CT and ZSM‐5‐C were found to be Type VI with a hysteresis loop type H2. The Type VI isotherm is associated with multilayer adsorption isotherms. It can be seen from the isotherm in Figure 3a(iv and v) that there were two steps with increased volume which occurred at the 𝑃/𝑃o values of 0.2 and 0.4. Figure 3b(ii, iv and v) show that ZSM‐5‐C has an average pore size of ca. 14.9 nm whe40r0e0as Z35S00M‐53‐0T00 and250Z0 SM2‐0500‐CT15h00ave 1c0a00.11.1500and 4000 3500 3000 2500 2000 1500 1000 500 15.2 nm average pore sizes, respectively. The mesoporous structure is present throughout the zeolite Wavenumbers (cm-1) Wavenumbers (cm-1) catalyst and forms a highly interpenetrating and uniform porous network. In contrast, the isotherm Figure 2. FT‐IR spectra for untreated and treated zeolite catalysts before (a) and after ion exchange Figure 2. FT-IR spectra for untreated and treated zeolite catalysts before (a) and after ion exchange (b). of the untreated zeolite catalyst is typical of microporous materials having high adsorption at low Wh(ebr)e. WZShMer-e5ZisSiMn ‐b5laisckin, ZbSlaMck-5,-ZNSaMis‐5i‐nNraedis, ZinSMred-5,-ZCSiMs i‐n5‐gCreiesnin, ZgSrMee-n5,-ZTSisMi‐n5b‐Tluies,iannbdluZeS,Man-d5-CZSTM‐ relative5p‐CreTssisuirnesp.urple. is in purple. 240 (v) 0.25 0.20 0.15 0.10 0.05 0.00 3.7 (b) (i) (ii) (iii) (vi) (v) 30 40 220 200 180 160 140 120 100 80 60 (a) (iv) (iii) (ii) (i) 0.0 0.2 0.4 0.6 0.8 1.0 1.7 11.1 10 15.2 20 14.9 Quantity adsorbed (cm3/g STP) %Transmittance Pore volume (cm3/g *nm) % Transmittance 3636 3475 3142 1639 1400 1227 1070 793 550 445 3636 3475 3142 1693 1400 1227 1070 793 550 455 Relative pressure (P/P) Figure 3. (a) N2 adsorption-desorption isotherm and (b) average pore size distribution. (i) ZSM-5, (ii) ZSM-5-T, (iii) ZSM-5-Na, (iv) ZSM-5-CT, and (v) ZSM-5-C. Figure 3. (a) N2 adsorption‐desorption isotherm and (b) average pore size distribution. (i) ZSM‐5, (ii) ZSM‐5‐T, (iii) ZSM‐5‐Na, (iv) ZSM‐5‐CT, and (v) ZSM‐5‐C. Table 3 summarizes the BET surface area, average pore size, and total pore volumes result for the treated and untreated zeolite catalysts. It is obvious that the surface area, pore sizes, and volumes of all Table 3 summarizes the BET surface area, average pore size, and total pore volumes result for the treated zeolite catalysts were significantly increased as compared to those of the untreated zeolite the treated and untreated zeolite catalysts. It is obvious that the surface area, pore sizes, and volumes catalyst. This is very important for the enhanced catalytic activity of synthesized catalysts. The highest of all the treated zeolite catalysts were significantly increased as compared to those of the untreated surface area of 419 ± 2.0 m2·g−1 was received for synthesised ZSM5-CT catalyst whereas the lowest zeolite catalyst. This is very important for the enhanced catalytic activity of synthesized catalysts. The surfaceareaof279±1.6m2·g−1wa2s−f1oundfortheuntreatedzeolite. highest surface area of 419 ± 2.0 m ∙g was received for synthesised ZSM5‐CT catalyst whereas the The particle size and morphol2og−i1es of treated and untreated zeolite catalysts were observed by SEM lowest surface area of 279 ± 1.6 m ∙g was found for the untreated zeolite. as shown in Figure 4. It can be observed from the SEM images that very tiny particle with unclear shapes, within a few nm size ranges, agglomerate with each other to form irregular clusters with different Table 3. N2 adsorption‐desorption isotherms of untreated and treated zeolites. morphologies. In order to observe the clear morphologies and confirm the mesoporosity of the zeolite SBET * Vp ** Dp *** t‐plot Values catalCysat,aalyhstisgh-resolution transmission electron microscopy analysis must be performed. The results 0 (m2∙g−1) (mL∙g−1) (nm) External Surface Area (m2∙g−1) VMicropore (cm3∙g−1) indicate that most of the crystals keep their shapes after treatments. However, some surface roughness ZSM‐5 279 ± 1.6 0.18 1.7 ± 0.1 55 0.13 was observed in the SEM images. These results match well with the results of the literature [27]. ZSM‐5‐Na ZSM‐5‐T ZSM‐5‐C ZSM5‐CT * SBET: BET surface area estimated using 0.05–0.3 relative pressure range; ** Vp: total pore volume (mL∙g−1) was calculated at 𝑃/𝑃o = 0.99; *** Dp: mean pore size (nm) estimated by using the BJH model from N2 desorption isotherm. 328 ± 1.2 390 ± 1.9 395 ± 2.5 419 ± 2.0 0.26 3.7 ± 0.1 0.23 11.1 ± 0.1 0.37 14.9 ± 0.1 0.34 15.2 ± 0.1 65 0.08 Pore diameter (nm) 60 0.12 300 0.06 200 0.08PDF Image | Synthesis of Uniform Mesoporous Zeolite ZSM-5 Catalyst
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