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

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 N...

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Published inNew journal of chemistry Vol. 40; no. 5; pp. 4319 - 4324
Main Authors Yuan, Ruting, Claes, Nathalie, Verheyen, Elke, Tuel, Alain, Bals, Sara, Breynaert, Eric, Martens, Johan A., Kirschhock, Christine E. A.
Format Journal Article
LanguageEnglish
Published 2016
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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 GeO 2 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.
AbstractList 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 GeO 2 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.
Author Verheyen, Elke
Tuel, Alain
Breynaert, Eric
Martens, Johan A.
Kirschhock, Christine E. A.
Claes, Nathalie
Yuan, Ruting
Bals, Sara
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  surname: Claes
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  givenname: Christine E. A.
  surname: Kirschhock
  fullname: Kirschhock, Christine E. A.
  organization: Centre for Surface Chemistry and Catalysis, KU Leuven, 3001 Heverlee, Belgium
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