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ChemEngineering 2019, 3, 35 5 of 11 decreasing the ratio of Si/Al appearing at 2θ from 5 to 20◦. Table 2 presents the crystallite size and amount of crystallinity for the treated and untreated zeolite catalysts. 5 of 11 ChemEngineering 2019, 3, x FOR PEER REVIEW [e] [d] [c] [b] [a] 10 20 30 40 50 / o Figure 1. XRD patterns for (a) ZSM‐5, (b) ZSM‐5‐Na, (c) ZSM‐5‐C, (d) ZSM‐5‐T and (e) ZSM‐5‐CT. Figure 1. XRD patterns for (a) ZSM-5, (b) ZSM-5-Na, (c) ZSM-5-C, (d) ZSM-5-T and (e) ZSM-5-CT. Table 2. The crystallite size and crystallinity of treated and untreated zeolite catalysts. Table 2. The crystallite size and crystallinity of treated and untreated zeolite catalysts. Catalysts Crystallite Size (nm) Crystallinity (%) Catalysts Crystallite Size (nm) Crystallinity (%) ZSM‐5 22 100 ZSM-5 ZSZMSM‐5-‐5N-Naa 22 100 ZSZMSM‐5-‐5C-C ZSM-5-T 21 21 8866 9933 ZSM‐5‐T 20 93 ZSM-5-CT 20 93 21 95 ZSM‐5‐CT Figure 2a,b presents the FT‐IR spectra before and after ion exchange, respectively, for all 21 95 Figure 2a,b presents the FT-IR spectra before and after ion exchange, respectively, for all untreated −1 −1 untreated and treated zeolite catalysts. The absorption band located at 3636 cm was attributed to and treated zeolite catalysts. The absorption band located at 3636 cm was attributed to the O–H tshtreeOtc–hHingstmreotcdheisnignmSio–dOe–sHinaSnid–/Oo–r HO–aHndg/rooruOp–s Hongtrhoeuspusrofancethoef stuherfzaecoeloitfetchaetazleyosltiste[2c2a]t.aTlyhsetsb[r2o2a]d. −1 −1 Twheabkrboanddwaeraokubnadn3d4a7r5ocumnd 34w7a5scamssigwnaesdatsosigthnedsttroettcheinsgtrevticbhriantgiovniborfathioenOo–fHthbeoOn–dHinbosinladnionl sgilraonuoplsg(rSoi–uOps–H(S)i–bOut–cHo)ubldutbceoduulde tboetdhueeadtosothrbeeadwsoartbeerd(Hw–aOte–rH(H) m–Ool–eHcu)lmesoolenctuhlesuornfathce osuf srfilaicea. −1 The band at 3142 cm was−1assigned to the stretching vibration of the hydroxyl (O–H) group of of silica. The band at 3142 cm was assigned to the stretching vibration of the hydroxyl (O–H) group −1 water molecules and amines (N–H) present in the pores of the zeolites [22]; bands at 1639 cm wer−e1 of water molecules and amines (N–H) present in the pores of the zeolites [22]; bands at 1639 cm −1 attributed to the O–H bending vibration of water molecules [23]. The band at 1400 cm in untre−a1ted were attributed to the O–H bending vibration of water molecules [23]. The band at 1400 cm in zeolite may be affected by characteristics peak of NH + and a simi+lar band has been observed for untreated zeolite may be affected by characteristics p4 eak of NH4 and a similar band has been treated zeolites after the ion exchange process [24]. Bands at 1227 and within the range of 1070 to observed for treated zeolites after the ion exchange process [24]. Bands at 1227 and within the range 1150 cm−1 were re−f1erred to the external asymmetric stretch and the internal asymmetric stretch of of 1070 to 1150 cm were referred to the external asymmetric stretch and the internal asymmetric −1 T–O–T, respectively. The band at 793 cm correspo−1nded to the external symmetric stretch of T–O–T, stretch of T–O–T, respectively. The band at 793 cm corresponded to the external symmetric stretch and that at 455 cm−1 was due to the T–O bend (where T = Si or Al) which is typically for the 5-fold of T–O–T, and that at 455 cm−1 was due to the T–O bend (where T = Si or Al) which is typically for rings of highly siliceous materials, whereas the framework vibration around 550 cm−1 (double rings) the 5‐fold rings of highly siliceous materials, whereas the framework vibration around 550 cm−1 is characteristic of MFI-type zeolites [25]. (double rings) is characteristic of MFI‐type zeolites [25]. The surface area, pore sizes, and pore volumes for all untreated and treated zeolite catalysts were determined using N adsorption-desorption isotherms. Figure 3a(i) illustrates the untreated (a) 2 (b) ZSM-5 exhibits Type I adsorption isotherm, while Figure 3a(iii) ZSM-5-Na displays Type IV adsorption isotherm with a hysteresis loop type H3 of plate-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. %Transmittance % Transmittance 3636 3475 3142 1639 1400 1227 1070 793 550 445 3636 3475 3142 1693 1400 1227 1070 793 550 455 Intensity / a.u. 4000 3500 3000 2500 2000 Wavenumbers (cm-1) 1500 1000 500 4000 3500 3000 2500 2000 1500 1000 500 Wavenumbers (cm-1) Figure 2. FT‐IR spectra for untreated and treated zeolite catalysts before (a) and after ion exchange (b). Where ZSM‐5 is in black, ZSM‐5‐Na is in red, ZSM‐5‐C is in green, ZSM‐5‐T is in blue, and ZSM‐ 5‐CT is in purple.PDF Image | Synthesis of Uniform Mesoporous Zeolite ZSM-5 Catalyst
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