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Synthesis and Structure of a 22 × 12 × 12 Extra-Large Pore Zeolite ITQ-56 Determined by 3D Electron Diffraction.

ABSTRACT: A multidimensional extra-large pore germanosilicate, denoted ITQ-56, has been synthesized by using modified memantine as an organic structure-directing agent. ITQ-56 crystallizes as plate-like nanocrystals. Its structure was determined by 3D electron diffraction/MicroED. The structure of ITQ-56 contains extra-large 22-ring channels intersecting with straight 12-ring channels. ITQ-56 is the first zeolite with 22-ring pores, which is a result of ordered vacancies of double 4-ring (d4r) units in a fully connected zeolite framework. The framework density is as low as 12.4 T atoms/1000 Å³. The discovery of the ITQ-56 structure not only fills the missing member of extra-large pore zeolite with 22-ring channels but also creates a new approach of making extra-large pore zeolites by introducing ordered vacancies in zeolite frameworks.

SUBMITTER: Kapaca E

PROVIDER: S-EPMC8213054 | biostudies-literature |

REPOSITORIES: biostudies-literature

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Project description:In small-pore zeolite catalysts, where the size of the pores is limited by eight-ring windows, aromatic hydrocarbon pool molecules that are formed inside the zeolite during the Methanol-to-Olefins (MTO) process cannot exit the pores and are retained inside the catalyst. Hydrocarbon species whose size is comparable to the size of the zeolite cage can cause the zeolite lattice to expand during the MTO process. In this work, the formation of retained hydrocarbon pool species during MTO at a reaction temperature of 400 °C was followed using operando UV-vis spectroscopy. During the same experiment, using operando X-ray Diffraction (XRD), the expansion of the zeolite framework was assessed, and the activity of the catalyst was measured using online gas chromatography (GC). Three different small-pore zeolite frameworks, i.e., CHA, DDR, and LEV, were compared. It was shown using operando XRD that the formation of retained aromatic species causes the zeolite lattice of all three frameworks to expand. Because of the differences in the zeolite framework dimensions, the nature of the retained hydrocarbons as measured by operando UV-vis spectroscopy is different for each of the three zeolite frameworks. Consequently, the magnitude and direction of the zeolite lattice expansion as measured by operando XRD also depends on the specific combination of the hydrocarbon species and the zeolite framework. The catalyst with the CHA framework, i.e., H-SSZ-13, showed the biggest expansion: 0.9% in the direction along the c-axis of the zeolite lattice. For all three zeolite frameworks, based on the combination of operando XRD and operando UV-vis spectroscopy, the hydrocarbon species that are likely to cause the expansion of the zeolite cages are presented; methylated naphthalene and pyrene in CHA, 1-methylnaphthalene and phenalene in DDR, and methylated benzene and naphthalene in LEV. Filling of the zeolite cages and, as a consequence, the zeolite lattice expansion causes the deactivation of these small-pore zeolite catalysts during the MTO process.

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Synthesis and Structure of a 22 × 12 × 12 Extra-Large Pore Zeolite ITQ-56 Determined by 3D Electron Diffraction.

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