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Room-temperature interaction of n-hexane with ZSM-5 zeolites

Microcalorimetric and temperature-programmed desorption studies

Journal of Thermal Analysis and Calorimetry
Authors: V. Rac, Vesna Rakić, S Gajinov, Vera Dondur, and Aline Auroux

Abstract  

In this work, room temperature interaction of n-hexane with HZSM-5 (Si/Al=20) and ion-exchanged samples containing one (CuZSM-5, FeZSM-5 and MnZSM-5) or two transition-metal cations (Fe,CuZSM-5; Cu,MnZSM-5 and Fe,MnZSM-5) was studied by microcalorimetry and TPD methods. Both differential heats and the amounts of n-hexane adsorbed per one unit cell were quantitatively determined. Higher heats of adsorption and higher amounts of adsorbed gas were found for ion-exchanged samples than for HZSM-5. The experiments of n-hexane adsorption on hydrated samples were also performed. The amounts of n-hexane adsorbed on hydrated ZSM-5 were lower in comparison with dehydrated samples, while the energies of interaction were similar.

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Abstract  

In the present study, we performed an investigation of phase transformation of zeolite Na-GIS in temperature interval from room temperature up to 1300C. The collapse of S4R and S8R (secondary building units in zeolite Na-GIS) and the forming of pure sodium nepheline phase, consists of S6R, was examined. During the thermal transformation of Na-GIS zeolite symmetry of rings was changed and their deformation increases. The irregularity of rings causes the appearance of defect modes in the IR spectra of amorphous precursors. Investigated phases were characterized by XRPD, IR, NMR and DSC methods. A semiempirical method AM1 was used for calculation of vibrational spectrum of nepheline.

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Abstract  

Temperature-programmed desorption coupled with mass spectrometer as a detector (TPD), IR and 13C NMR measurements are used to study the adsorption of n-hexane on hydrated HZSM-5 and NH4ZSM-5 zeolites. The 13C NMR measurements show that n-hexane can access the pore structure of ZSM-5 zeolites previously saturated with water. TPD spectra of n-hexane are monitored in the temperature region 50–300C, in the case of fully or partially hydrated samples; two-stage desorption of n-hexane is found. Simultaneous desorption of water and n-hexane in the same temperature region are found, in all investigated samples.

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