IM-17: a new zeolitic material, synthesis and structure elucidation from electron diffraction ADT data and Rietveld analysis

Lorgouilloux, Yannick; Dodin, Mathias; Mugnaioli, Enrico; Marichal, Claire; Caullet, Philippe; Bats, Nicolas; Kolb, Ute; Paillaud, Jean-Louis

doi:10.1039/c4ra01383b

Cited by 48 publications

(34 citation statements)

References 68 publications

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“…A related framework type, IWR also possesses the same 3D 12×10×10‐ring channel system as that of CON . Later on, a series of interesting zeolites (such as ITG , *‐ITN and MSE ) with interconnected large and medium pores have been synthesized . However, the 3D channel systems of these framework types are all 12×10×10‐ring, and zeolites with more open 3D interconnected 12×12×10‐ring channels have not yet been reported.…”

Section: Figurementioning

confidence: 99%

“…[10] Later on, as eries of interesting zeolites( such as ITG, *-ITN and MSE)w ith interconnected large andm edium pores have been synthesized. [7,[11][12][13][14][15] However,t he 3D channel systems of these framework types are all 12 10 10-ring, and zeolites with more open 3D interconnected 12 12 10-ring channels have not yet been reported.…”

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confidence: 99%

“…Elemental analysis and 13 Cs olid-state MAS NMR spectroscopy of as-made SCM-15d emonstrate that the OSDA molecules remain intact within the framework structure ( Table S1, Figure S2). Besides, the 13 Cl iquid NMR spectra of protonated OSDA molecules in solution with different pH values coupled with the pH value ( % 8-9) of the starting gel reveal that the OSDA molecules in the structure of SCM-15 are mainly monoprotonated and charge-balanced by F À ions ( Figure S2). T he 19 F MAS NMR spectrum of as-made SCM-15i ndicatest he F À ions are located in the small d4r units, since two resonanceb ands centereda tÀ7.7 and À18.9 ppm are present in the spectrum ( Figure S3).…”

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confidence: 99%

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Synthesis and Structure Determination of SCM‐15: A 3D Large Pore Zeolite with Interconnected Straight 12×12×10‐Ring Channels

Luo

Smeets

Wang

et al. 2019

Chemistry A European J

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A new germanosilicate zeolite named SCM‐15 (Sinopec Composite Material No. 15), the first zeolite containing a 3‐dimensional (3D) channel system with interconnected 12‐, 12‐, and 10‐ring channels (pore sizes: 6.1×7.2, 6.1×7.4, and 5.2×5.9 Å), has been synthesized using neutral 4‐pyrrolidinopyridine as organic structure‐directing agents (OSDAs). Its structure has been determined by combining single‐crystal electron diffraction (SCED) and synchrotron powder X‐ray diffraction (SPXD) data. The unique open framework structure of SCM‐15 is related to that of FOS‐5 (BEC), ITQ‐7 (ISV), PKU‐16 (POS), ITQ‐26 (IWS), ITQ‐21, Beta polymorph B, and SU‐78B, since all these framework structures can be constructed from similar chains which are connected through shared 4‐ring or double 4‐ring (d4r) units. Based on this relation, six topologically reasonable 3D large or extra‐large pore hypothetical zeolites are predicted.

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Section: Figurementioning

confidence: 99%

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confidence: 99%

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Synthesis and Structure Determination of SCM‐15: A 3D Large Pore Zeolite with Interconnected Straight 12×12×10‐Ring Channels

Luo

Smeets

Wang

et al. 2019

Chemistry A European J

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“…[10] Germanosilicate UTL is an ideal ADOR starting point because of its chemical composition and because of the stability of the layered units that are formed on disassembly.H erein we report the synthesis of an ew zeolite,w hich we name IPC-12, using the ADOR transformation of ag ermanosilicate parent zeolite with the UOV topology. [11] We have previously predicted that UOV would be agood target, [12] but since it has pores in three dimensions, rather than only in two as is the case for UTL,w ecould not rule out the possibility that the layers (which are porous) would be less stable than in UTL.Indesigning this successful procedure,p articular attention has to be given to the factors controlling the ADOR process,such as appropriate chemical and structural properties of the parent material, optimized conditions for disassembly and reassembly of formed intermediates.…”

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confidence: 99%

Expansion of the ADOR Strategy for the Synthesis of Zeolites: The Synthesis of IPC‐12 from Zeolite UOV

et al. 2017

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The assembly-disassembly-organization-reassembly (ADOR) process has been used to disassemble ap arent zeolite with the UOV structure type and then reassemble the resulting layers into anovel structure,IPC-12. The structure of the material has previously been predicted computationally and confirmed in our experiments using X-ray diffraction and atomic resolution STEM-HAADF electron microscopy. This is the first successful application of the ADOR process to amaterial with porous layers.For more than 60 years,z eolites have been almost exclusively prepared via hydrothermal, [1] solvothermal, [2] and ionothermal [3] synthesis techniques.T he recently discovered ADOR (assembly-disassembly-organization-reassembly) strategy [4] is an alternative way to prepare new zeolite structures.T he method consists of the chemically selective disassembly of aparent zeolite into its constituent layers.This is followed by organization of these units into as uitable relative orientation and the reassembly of the units into new materials.C ontrolled disassembly of the parent zeolite is possible when there is aw eakness engineered into the structure during the initial synthesis.[5] In general, this involves the regioselective substitution of silicon for germanium, which is much more hydrolytically sensitive than the silicon species,a llowing selective dissolution of the germanium out of the material.TheA DOR process is fundamentally different from hydrothermal synthesis in that the final framework-forming step is an irreversible condensation at high temperature (500-700 8 8C) rather than areversible crystallization step.This leads to new zeolites that have unusual properties that include the possibility of preparing isoreticular families of materials with continuously controllable porosity.[6] Of potential great importance is the possibility of preparing materials that do not obey the energy-density rules [7] associated with hydrothermal synthesis,l eading to new zeolites that in the past would have been thought unfeasible synthetic targets.[8] An important point to note is that the reassembly process is very easy to model, leading to final products that are computationally predictable, [9] something that is very difficult in hydrothermal synthesis.One crucial issue of the ADOR approach not yet demonstrated is its general applicability.U pt on ow,t he ADOR approach to new materials has concentrated on the use of zeolite UTL as the parent material, although other parent zeolites,s uch as IWW have been successfully disassembled.[10] Germanosilicate UTL is an ideal ADOR starting point because of its chemical composition and because of the stability of the layered units that are formed on disassembly.H erein we report the synthesis of an ew zeolite,w hich we name IPC-12, using the ADOR transformation of ag ermanosilicate parent zeolite with the UOV topology.[11] We have previously predicted that UOV would be agood target, [12] but since it has pores in three dimensions, rather than only in two as is the case for UTL,w ecould not...

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“…The key feature of the parent zeolites is the presence of a chemical 'weakness' in a specific structural site. 5 Zeolites that have silica-rich layers linked by germanium-rich cubic units, termed double four rings (d4rs), such as those with the UTL, 6,7 IWW 8,9 and UOV 10,11 topologies, are particularly suitable for the process. The d4r units each comprise eight tetrahedra and contain approximately 50% Ge and 50% Si.…”

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In situ solid-state NMR and XRD studies of the ADOR process and the unusual structure of zeolite IPC-6

et al. 2017

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The Assembly-Disassembly-Organisation-Reassembly (ADOR) mechanism is a recent method for preparing inorganic framework materials and, in particular, zeolites. This flexible approach has enabled the synthesis of isoreticular families of zeolites with unprecedented continuous control over porosity, and the design and preparation of materials that would have been difficult -or even impossible -to obtain using traditional hydrothermal techniques. Applying the ADOR process to a parent zeolite with the UTL framework topology, for example, has led to six previously unknown zeolites (named IPC-n with n = 2, 4, 6, 7, 9 and 10). To realize the full potential of the ADOR method, however, a further understanding of the complex mechanism at play is needed. Here, we probe the disassembly, organisation and reassembly steps of the ADOR process through a combination of in situ solid-state nuclear magnetic resonance (NMR) spectroscopy and powder Xray diffraction (PXRD) experiments. We further use the insight gained to explain the formation of the intriguing structure of zeolite IPC-6.The recently-discovered ADOR process 1-4 has proved to be effective for the preparation of new silicate and aluminosilicate zeolites, providing routes to 'unfeasible' synthesis targets with novel structural features 3 and to families of isoreticular solids whose pore size can be precisely controlled over the whole range of zeolite porosity, from small pore all the way up to extra-large pore materials. 1,4 The process comprises four distinct steps. The assembly (A) process involves the preparation of a parent zeolite with suitable chemical and topological properties for

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IM-17: a new zeolitic material, synthesis and structure elucidation from electron diffraction ADT data and Rietveld analysis

Cited by 48 publications

References 68 publications

Synthesis and Structure Determination of SCM‐15: A 3D Large Pore Zeolite with Interconnected Straight 12×12×10‐Ring Channels

Synthesis and Structure Determination of SCM‐15: A 3D Large Pore Zeolite with Interconnected Straight 12×12×10‐Ring Channels

Expansion of the ADOR Strategy for the Synthesis of Zeolites: The Synthesis of IPC‐12 from Zeolite UOV

In situ solid-state NMR and XRD studies of the ADOR process and the unusual structure of zeolite IPC-6

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