Drastic change of the intrusion–extrusion behavior of electrolyte solutions in pure silica *BEA-type zeolite

Ryzhikov, Andrey; Khay, Ismail; Nouali, Habiba; Daou, T. Jean; Patarin, Joël

doi:10.1039/c4cp01862a

Cited by 39 publications

(73 citation statements)

References 30 publications

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“…Such a behavior, which was already observed for the *BEA-type zeosil reveals an alteration of the MFI nanosheets after intrusion of water. 50 This result is in agreement with the NMR results (see below), where a higher number of defect sites was found for the water intruded−extruded nanosheet sample.…”

Section: ■ Experimental Sectionsupporting

confidence: 92%

Influence of the Particle Sizes on the Energetic Performances of MFI-Type Zeolites

et al. 2015

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Nanoporous materials have an important role in addressing some of the major energy and environmental-related problems facing society. Herein, four MFI-type zeosils with crystallite size ranging from nanometer to micrometer were synthesized (nanosheets, nanocrystals, honeycombs, and big crystals) in order to establish a relation between the crystal size of these zeosils and their energetic performances under high-pressure intrusion−extrusion experiments (mechanical energy storage). The intrusion−extrusion behavior of water and concentrated LiCl aqueous solution (20 M) in these four zeosils was evaluated at room temperature. Whatever the crystal size, the "Silicalite-1-water" systems displayed a spring behavior, whereas "Silicalite-1-LiCl aqueous solution" systems moved slightly toward a shock-absorber behavior with an increase in the intrusion and extrusion pressures (273−285 MPa) compared to "Silicalite-1-water" systems (88−96 MPa). Therefore, in the case of the LiCl aqueous solution (20 M), the energetic performance was tripled. Compared to the big crystal sample, both the honeycomb and the nanocrystal samples showed a slight decrease of the intrusion and extrusion pressures. A decrease of the intrusion and extrusion volumes was observed in the case of nanocrystal sample compared to both big crystal and honeycomb samples, which is attributed to the noncrystallized silica regions infused within the nanocrystals. Contrary to these three samples, liquid intrusion occurred at atmospheric pressure for the nanosheet sample, which is likely due to both the presence of a high number of surface defects and the low thickness of the zeolite nanosheets (2 nm). Solid-state NMR spectroscopy and thermogravimetric analyses provided evidence on the presence of local defects on the nonintruded samples and the breaking of some siloxane bridges after the intrusion−extrusion step. ■ INTRODUCTIONZeolites have an important role in addressing some of the major problems facing society in the twenty-first century, such as energy storage, water and air decontamination, therapeutics (i.e., drug delivery, etc.), and catalysis. 1−11 The size of the zeolite pores and their accessibility can directly affect their performance in a particular application. 3 For example, zeolites are used as acid catalysts or molecular adsorbents, but their micropores impose severe diffusion limitations. 3,10,11 To address such issues, great effort is being expended in preparing new zeolites with larger micropores or to improve the diffusion inside existing zeolites. 12 This improvement can be achieved by creating additional porosity in the microporous materials, or by inhibiting their growth beyond a nanometer-scale. 13,14 Several methods were developed to obtain zeolite nanocrystals, 15 but they were opposed to limitations such as slow reaction kinetics, low yields, or nanocrystal agglomeration, which restricted their use at the industrial scale. A considerable number of works have been done to introduce mesopores into zeolite 16,17 by using postsynthetic demet...

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Section: ■ Experimental Sectionsupporting

confidence: 92%

Influence of the Particle Sizes on the Energetic Performances of MFI-Type Zeolites

et al. 2015

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“…The topology of the porous material used is expected to have an impact on the pressure hysteresis as well. From the analysis of reported data on microporous HLSs in terms of dimensionality of the pores (Table and Figure ) it is evident that a potential candidate should not have a cagelike structure, as was often stressed in the works of Patarin and co‐workers . On the other hand, it should be highly stable to resist the concomitant effects of pressure and temperature in intrusion/extrusion cycles, which may strongly affect the structure of the porous material .…”

Section: Characteristics Of Microporous Hlss[a]mentioning

confidence: 96%

A Highly Stable Nonhysteretic {Cu₂(tebpz) MOF+water} Molecular Spring

Grosu

Peng

et al. 2016

ChemPhysChem

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A molecular spring formed by a hydrophobic metal-organic framework Cu (tebpz) (tebpz=3,3',5,5'-tetraethyl-4,4'-bipyrazolate) and water is presented. This nanoporous heterogeneous lyophobic system (HLS) has exceptional properties compared to numerous reported systems of such type in terms of stability, efficiency, and operating pressure. Mechanical and thermal energetic characteristics as well as stability of the system are discussed and compared in detail with those of other previously reported HLS.

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“…Whereas, using concentrated LiCl aqueous solution (15-20 M) as non-wetting liquid, the system displays a shock-absorber behavior and, during the decompression step, the liquid is completely expelled from the porous solid [19]. It was supposed that this behavior change was related to a change of the nature of the intruded liquid from water, to solvated ions from highly concentrated LiCl aqueous solutions.…”

Section: Introductionmentioning

confidence: 99%

“…The intrusion of highly concentrated electrolyte solutions can also change the behavior of the "zeosil-aqueous solution" system. It was the case, for instance, for the LTA-and *BEA-type zeosil [27,19].…”

Section: Introductionmentioning

confidence: 99%

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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Drastic change of the intrusion–extrusion behavior of electrolyte solutions in pure silica *BEA-type zeolite

Cited by 39 publications

References 30 publications

Influence of the Particle Sizes on the Energetic Performances of MFI-Type Zeolites

Influence of the Particle Sizes on the Energetic Performances of MFI-Type Zeolites

A Highly Stable Nonhysteretic {Cu₂(tebpz) MOF+water} Molecular Spring

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

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Drastic change of the intrusion–extrusion behavior of electrolyte solutions in pure silica *BEA-type zeolite

Cited by 39 publications

References 30 publications

Influence of the Particle Sizes on the Energetic Performances of MFI-Type Zeolites

Influence of the Particle Sizes on the Energetic Performances of MFI-Type Zeolites

A Highly Stable Nonhysteretic {Cu2(tebpz) MOF+water} Molecular Spring

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

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A Highly Stable Nonhysteretic {Cu₂(tebpz) MOF+water} Molecular Spring