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Issue 5, 2016
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Synthesis of an IWW-type germanosilicate zeolite using 5-azonia-spiro[4,4]nonane as a structure directing agent

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Abstract

An IWW-type zeolite with a Si/Ge ratio of 4.9 is obtained using 5-azonia-spiro[4,4]nonane as a template in fluoride-free medium under hydrothermal conditions at 175 °C. In an otherwise identical synthesis, using related 5-azonia-spiro[4,5]decane as a structure directing agent, a mixture of IWW and NON zeolite types was formed. In the absence of GeO2 from the reactant mixture, pure NON formed. The IWW zeolite was characterized by XRD, SEM, and HRTEM. The IWW zeolite displayed a unique morphology and could be calcined at 600 °C without the loss of crystallinity. The Si/Ge ratio of the IWW zeolite was increased by postsynthesis modification. Part of germanium could be eliminated from the as-synthesized IWW zeolite by acid leaching using 6 M HCl solution. Also the calcined material could be degermanated. Here the presence of a silicon source in the acidic leaching solution minimized structural damage. In this way the Si/Ge ratio of the IWW zeolite was increased from 4.9 up to 10.

Graphical abstract: Synthesis of an IWW-type germanosilicate zeolite using 5-azonia-spiro[4,4]nonane as a structure directing agent

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Article information


Submitted
04 Nov 2015
Accepted
18 Feb 2016
First published
19 Feb 2016

New J. Chem., 2016,40, 4319-4324
Article type
Paper
Author version available

Synthesis of an IWW-type germanosilicate zeolite using 5-azonia-spiro[4,4]nonane as a structure directing agent

R. Yuan, N. Claes, E. Verheyen, A. Tuel, S. Bals, E. Breynaert, J. A. Martens and C. E. A. Kirschhock, New J. Chem., 2016, 40, 4319
DOI: 10.1039/C5NJ03094C

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