Synthesis of a Sulfate Enclathrated Zeolite with Intermediate Framework Structure between Sodalite and Cancrinite

Publikation: Beitrag in FachzeitschriftArtikelForschungPeer-Review

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  • Josef Christian Buhl

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OriginalspracheEnglisch
Seiten (von - bis)1030-1036
Seitenumfang7
FachzeitschriftZeitschrift fur Anorganische und Allgemeine Chemie
Jahrgang643
Ausgabenummer15
PublikationsstatusVeröffentlicht - 17 Juli 2017

Abstract

A sulfate enclathrated microporous zeolite of composition Na7.4[SiAlO4]6(SO4)0.7(H2O)4.8 with intermediate framework structure (INT) between the well known zeolites sodalite (SOD) and cancrinite (CAN) can be prepared by the autothermal synthesis, a method first demonstrated in reference. The product (abbreviated as “SO4-INT”) was characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX-analysis), Fourier transform infrared spectroscopy (FT-IR) and thermogravimetry (TG). SO4-INT was found to crystallize as spheres with 1–6 μm in diameter with a rough surface. Sometimes the spheres are agglutinated to each other by a few amount of amorphous material within the sample. The thermal behavior of the new phase was further studied. At elevated temperature (1000 °C) a transformation of SO4-INT into a large amount of nosean was observed beside some parts of nepheline, formed by crystallization of the amorphous byproduct. The nosean phase was found to be stable up to 1250 °C, before the onset of a total destruction by melting during further heating. Finally a re-crystallization of the melt during cooling yielded carnegieite as the final product (low form at room temperature). This unusual thermal behavior of SO4-INT is discussed in terms of structural interactions of the sulfate guests inside the aluminosilicate host-framework and in comparison with literature data of the intermediate phases CO3-INT, as well as NO3-INT.

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Synthesis of a Sulfate Enclathrated Zeolite with Intermediate Framework Structure between Sodalite and Cancrinite. / Buhl, Josef Christian.
in: Zeitschrift fur Anorganische und Allgemeine Chemie, Jahrgang 643, Nr. 15, 17.07.2017, S. 1030-1036.

Publikation: Beitrag in FachzeitschriftArtikelForschungPeer-Review

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abstract = "A sulfate enclathrated microporous zeolite of composition Na7.4[SiAlO4]6(SO4)0.7(H2O)4.8 with intermediate framework structure (INT) between the well known zeolites sodalite (SOD) and cancrinite (CAN) can be prepared by the autothermal synthesis, a method first demonstrated in reference. The product (abbreviated as “SO4-INT”) was characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX-analysis), Fourier transform infrared spectroscopy (FT-IR) and thermogravimetry (TG). SO4-INT was found to crystallize as spheres with 1–6 μm in diameter with a rough surface. Sometimes the spheres are agglutinated to each other by a few amount of amorphous material within the sample. The thermal behavior of the new phase was further studied. At elevated temperature (1000 °C) a transformation of SO4-INT into a large amount of nosean was observed beside some parts of nepheline, formed by crystallization of the amorphous byproduct. The nosean phase was found to be stable up to 1250 °C, before the onset of a total destruction by melting during further heating. Finally a re-crystallization of the melt during cooling yielded carnegieite as the final product (low form at room temperature). This unusual thermal behavior of SO4-INT is discussed in terms of structural interactions of the sulfate guests inside the aluminosilicate host-framework and in comparison with literature data of the intermediate phases CO3-INT, as well as NO3-INT.",
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T1 - Synthesis of a Sulfate Enclathrated Zeolite with Intermediate Framework Structure between Sodalite and Cancrinite

AU - Buhl, Josef Christian

PY - 2017/7/17

Y1 - 2017/7/17

N2 - A sulfate enclathrated microporous zeolite of composition Na7.4[SiAlO4]6(SO4)0.7(H2O)4.8 with intermediate framework structure (INT) between the well known zeolites sodalite (SOD) and cancrinite (CAN) can be prepared by the autothermal synthesis, a method first demonstrated in reference. The product (abbreviated as “SO4-INT”) was characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX-analysis), Fourier transform infrared spectroscopy (FT-IR) and thermogravimetry (TG). SO4-INT was found to crystallize as spheres with 1–6 μm in diameter with a rough surface. Sometimes the spheres are agglutinated to each other by a few amount of amorphous material within the sample. The thermal behavior of the new phase was further studied. At elevated temperature (1000 °C) a transformation of SO4-INT into a large amount of nosean was observed beside some parts of nepheline, formed by crystallization of the amorphous byproduct. The nosean phase was found to be stable up to 1250 °C, before the onset of a total destruction by melting during further heating. Finally a re-crystallization of the melt during cooling yielded carnegieite as the final product (low form at room temperature). This unusual thermal behavior of SO4-INT is discussed in terms of structural interactions of the sulfate guests inside the aluminosilicate host-framework and in comparison with literature data of the intermediate phases CO3-INT, as well as NO3-INT.

AB - A sulfate enclathrated microporous zeolite of composition Na7.4[SiAlO4]6(SO4)0.7(H2O)4.8 with intermediate framework structure (INT) between the well known zeolites sodalite (SOD) and cancrinite (CAN) can be prepared by the autothermal synthesis, a method first demonstrated in reference. The product (abbreviated as “SO4-INT”) was characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX-analysis), Fourier transform infrared spectroscopy (FT-IR) and thermogravimetry (TG). SO4-INT was found to crystallize as spheres with 1–6 μm in diameter with a rough surface. Sometimes the spheres are agglutinated to each other by a few amount of amorphous material within the sample. The thermal behavior of the new phase was further studied. At elevated temperature (1000 °C) a transformation of SO4-INT into a large amount of nosean was observed beside some parts of nepheline, formed by crystallization of the amorphous byproduct. The nosean phase was found to be stable up to 1250 °C, before the onset of a total destruction by melting during further heating. Finally a re-crystallization of the melt during cooling yielded carnegieite as the final product (low form at room temperature). This unusual thermal behavior of SO4-INT is discussed in terms of structural interactions of the sulfate guests inside the aluminosilicate host-framework and in comparison with literature data of the intermediate phases CO3-INT, as well as NO3-INT.

KW - Microporous solids

KW - Structural intermediates of SOD and CAN

KW - Sulfate enclathrated zeolites

KW - Thermal stability

KW - Zeolites

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JO - Zeitschrift fur Anorganische und Allgemeine Chemie

JF - Zeitschrift fur Anorganische und Allgemeine Chemie

SN - 0044-2313

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