Pressure-induced water intrusion in FER-type zeolites and the influence of extraframework species on structural deformations

Arletti, Rossella; Vezzalini, Giovanna; Quartieri, Simona; Renzo, Francesco Di; Dmitriev, Vladimir

doi:10.1016/j.micromeso.2014.02.036

Cited by 26 publications

(42 citation statements)

References 47 publications

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“…The low difference in weight loss between the two samples (0.4 wt.%), confirms that the creation of defect sites (silanol groups) after intrusion-extrusion experiment, if any, is very low. Such a result was confirmed by 29 Si and 1 H- 29 Si CP MAS NMR experiments (see Figures S1 and S2). The textural properties of the different Si-FER samples were determined from N 2 adsorption-desorption measurements.…”

Section: Tg Analysis and N 2 Adsorption-desorption Measurementssupporting

confidence: 68%

“…The starting atomic coordinates were taken from the structural model [29] and the intruded extraframework species were located after the inspection of the Fourier Difference Observed and calculated profiles are reported in Figure 1, details of the structural refinements are reported in Table S1. The refined cell parameters as a function of pressure are reported in Table 1.…”

Section: Sgmentioning

confidence: 99%

“…In the last decades a number of studies have been devoted to the structural investigation of zeolite-water systems, in particular in relation of the so-called "pressure induced hydration" [4,5,28,29]. Arletti et al [29] studied the P-induced penetration of aqueous/alcohol (m.e.w.)…”

Section: Introductionmentioning

confidence: 99%

“…Arletti et al [29] studied the P-induced penetration of aqueous/alcohol (m.e.w.) mixture (16 methanol: 3 ethanol: 1 water) in the channel of an all-silica ferrierite (Si-FER) (FER Framework type [30]) by in situ high pressure (HP) X-ray powder diffraction (XRPD).…”

Section: Introductionmentioning

confidence: 99%

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Intrusion-extrusion experiments of MgCl2 aqueous solution in pure silica ferrierite: Evidence of the nature of intruded liquid by in situ high pressure synchrotron X-ray powder diffraction

Arletti

Ronchi

Quartieri

et al. 2016

Microporous and Mesoporous Materials

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Intrusion-extrusion experiments of MgCl2 aqueous solution in pure silica ferrierite: Evidence of the nature of intruded liquid by in situ high pressure synchrotron X-ray powder diffraction / Arletti, Rossella; Ronchi, Laura; Quartieri, Simona; Vezzalini, Giovanna; Ryzhikov, Andrey; Nouali, Habiba; Daou, T. Jean; Patarin, Joël. ABSTRACTExperimental intrusion-extrusion isotherms of MgCl 2 21H 2 O solution were recorded at room temperature on pure silica FER-type zeolite (Si-FER). The intrusion occurs at 195 MPa and the phenomenon is completely reversible with a slight hysteresis. The "Si-FER -MgCl 2 aqueous solution" system behaves like a spring. The material was deeply characterized before and after intrusion-extrusion experiments and no significant changes were observed. The unit cell parameters were refined -on the basis of the in situ synchrotron X-ray powder diffraction data -up to 1.47 GPa and then at P amb upon pressure release. The Rietveld refinement of the data collected at 0.28 GPa (280 MPa), a pressure close to the intrusion value, shows that both ions and water molecules present in the MgCl 2 aqueous solution were intruded in the porosities. However, the solvation degree of the intruded ions differs from the initial solution, revealing a partial desolvation of both magnesium and chloride ions. As a whole, the nature and amount of the intruded species correspond to a MgCl 2 10H 2 O composition. Moreover, at a higher pressure (0.68 GPa), a phase transition from the orthorhombic Pmnn to the monoclinic P2 1 /n s.g. is observed in Si-FER. At 1.47 GPa, the zeolite maintains this monoclinic symmetry, while another phase transition, to the monoclinic P2 1 s.g., is argued from the analysis of the pattern of the sample compressed to 2.6 GPa and then collected upon pressure release to ambient conditions. KEYWORDS.FER-type zeolite, pure silica ferrierite, intrusion-extrusion experiments, in-situ high pressure synchrotron XRPD experiments, structural refinement.

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Section: Tg Analysis and N 2 Adsorption-desorption Measurementssupporting

confidence: 68%

Section: Sgmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Intrusion-extrusion experiments of MgCl2 aqueous solution in pure silica ferrierite: Evidence of the nature of intruded liquid by in situ high pressure synchrotron X-ray powder diffraction

Arletti

Ronchi

Quartieri

et al. 2016

Microporous and Mesoporous Materials

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“…Phase transitions even in a low P regime is not uncommon; in fact they have also been reported for the high-silica zeolites silicalite-1 9,15,67 and Si-FER. 68 These studies demonstrate that high-silica zeolites, when compressed in nonpenetrating PTM, undergo marked framework deformations as a consequence of the lack of the extra-framework species, which cannot contribute to the stiffening of the structure. Thus it is not surprising that these zeolites accommodate HP induced distortions by changing their symmetry.…”

Section: Structural Deformations Induced By Non-penetrating Ptmmentioning

confidence: 89%

Pressure-induced penetration of guest molecules in high-silica zeolites: the case of mordenite

Arletti

Leardini

Vezzalini

et al. 2015

Phys. Chem. Chem. Phys.

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A synthetic high-silica mordenite (HS-MOR) has been compressed in both non-penetrating (silicone oil, s.o.) and penetrating [methanol : ethanol : water (16 : 3 : 1) (m.e.w.), water : ethanol (3 : 1) (w.e.), and ethylene glycol (e.gl.)] pressure transmitting media (PTM). In situ high-pressure (HP) synchrotron X-ray powder diffraction (XRPD) experiments allowed the unit cell parameters to be followed up to 1.6, 1.8, 8.4, and 6.7 GPa in s.o., w.e., m.e.w., and e.gl., respectively. Moreover, e.gl. was also used as a PTM in in situ HP Raman and ex situ IR experiments. The structural refinement of HS-MOR compressed in e.gl.at 0.1 GPa -the lowest investigated pressure -revealed the presence of 3.5 ethylene glycol molecules per unit cell. The infrared spectrum of the recovered sample, after compression to 1 GPa, is consistent with the insertion of ethylene glycol molecules in the pores. XRPD and Raman spectroscopy experiments performed under pressure indicated the insertion of a small number of guest molecules. Ethylene glycol is partially retained inside mordenite upon pressure release. A symmetry lowering was observed in s.o. above 0.8 GPa, while above 1.6 GPa the patterns indicated a rapid loss of long range order. From ambient pressure (P amb ) to 1.6 GPa, a high cell volume contraction (DV = À9.5%) was determined. The patterns collected with penetrating PTM suggested the penetration of guest molecules into the porous host matrix, starting from a very low P regime. The entrapment of PTM molecules inside micropores contributes to the stiffening of the structure and, as a consequence, to the decrease of the compressibility with respect to that measured in s.o. From the structural point of view, HS-MOR reacts to compression and to the penetration of different guest species with appropriate framework deformations. Interestingly, ethylene glycol is partially retained inside mordenite upon pressure release, which is of importance for potential application of this composite material.

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Irreversible Conversion of a Water–Ethanol Solution into an Organized Two‐Dimensional Network of Alternating Supramolecular Units in a Hydrophobic Zeolite under Pressure

et al. 2017

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Turning disorderi nto organization is ak ey issue in science.B ym aking use of X-rayp owder diffraction and modeling studies,w es how herein that high pressures in combination with the shape and space constraints of the hydrophobic all-silica zeolite ferrierite separate an ethanolwater liquid mixture into ethanol dimer wires and water tetramer squares.T he confined supramolecular blocks alternate in ab inary two-dimensional (2D) architecture that remains stable upon complete pressure release.T hese results support the combined use of high pressures and porous networks as av iable strategy for driving the organization of molecules or nano-objects towards complex, pre-defined patterns relevant for the realization of novel functional nanocomposites.Supportinginformation and the ORCID identification number(s) for the author(s) of this article can be found under: http://dx.

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Pressure-induced water intrusion in FER-type zeolites and the influence of extraframework species on structural deformations

Cited by 26 publications

References 47 publications

Intrusion-extrusion experiments of MgCl2 aqueous solution in pure silica ferrierite: Evidence of the nature of intruded liquid by in situ high pressure synchrotron X-ray powder diffraction

Intrusion-extrusion experiments of MgCl2 aqueous solution in pure silica ferrierite: Evidence of the nature of intruded liquid by in situ high pressure synchrotron X-ray powder diffraction

Pressure-induced penetration of guest molecules in high-silica zeolites: the case of mordenite

Irreversible Conversion of a Water–Ethanol Solution into an Organized Two‐Dimensional Network of Alternating Supramolecular Units in a Hydrophobic Zeolite under Pressure

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