Improving Stability of Zeolites in Aqueous Phase via Selective Removal of Structural Defects

Missing silicon–oxygen bonds in zeolites are shown to be the cause for structural instability of zeolites in hot liquid water. Their selective removal drastically improved their structural stability as demonstrated using zeolite beta as example. The defects in the siloxy bonds were capped by reactio...

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Published inJournal of the American Chemical Society Vol. 138; no. 13; pp. 4408 - 4415
Main Authors Prodinger, Sebastian, Derewinski, Miroslaw A, Vjunov, Aleksei, Burton, Sarah D, Arslan, Ilke, Lercher, Johannes A
Format Journal Article
LanguageEnglish
Published United States American Chemical Society 06.04.2016
American Chemical Society (ACS)
Subjects
Environmental Molecular Sciences Laboratory
hydrothermal zeolite stability
nuclear magnetic resonance spectroscopy
sieves
silanol defects
silylation
sorption
sorption isotherms
X-ray diffraction
zeolites
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Abstract Missing silicon–oxygen bonds in zeolites are shown to be the cause for structural instability of zeolites in hot liquid water. Their selective removal drastically improved their structural stability as demonstrated using zeolite beta as example. The defects in the siloxy bonds were capped by reaction with trimethylchlorosilane, and Si–O–Si bonds were eventually formed. Hydrolysis of Si–O–Si bonds of the parent materials and dissolution of silica–oxygen tetrahedra in water causing a decrease in sorption capacity by reprecipitation of dissolved silica and pore blocking was largely mitigated by the treatment. The stability of the modified molecular sieves was monitored by 29Si-MAS NMR, transmission electron micrographs, X-ray diffraction, and adsorption isotherms. The microporosity, sorption capacity, and long-range order of the stabilized material were fully retained even after prolonged exposure to hot liquid water.
AbstractList This work reports significant improvement in the hydrothermal stability of a well-characterized BEA zeolite via the selective removal of structural defects. Recent work suggests that the presence of silanol defects destabilizes the framework integrity of most zeolites and makes them susceptible to hydrolysis of the siloxy bonds by hot liquid water. The described approach allows for a key removal of silanols as shown with 29Si-MAS-NMR. Subsequently, the material stability in hot liquid water, measured by retention of its crystallinity with X-ray diffraction (XRD), is found to be superior to defective zeolites. In addition, N2-sorption measurements (BET) and transmission electron microscopy (TEM) show the formation of different types of mesoporosity for water-treated stabilized and unmodified materials. While the sorption capacity for untreated materials drops, related to re-precipitation of dissolved silica and pore blocking, the stabilized material retains its microporosity and improves its overall sorption capacity. The authors would like to thank B. W. Arey (PNNL) for HIM measurements and I. Arslan for TEM imaging. This work was supported by the U. S. Department of Energy (DOE), Office of Science, Office of Basic Energy Sciences, Division of Chemical Sciences, Geosciences & Biosciences. SP and MD acknowledge support by the Materials Synthesis and Simulation Across Scales (MS3 Initiative) conducted under Laboratory Directed Research & Development Program at PNNL.
Missing silicon-oxygen bonds in zeolites are shown to be the cause for structural instability of zeolites in hot liquid water. Their selective removal drastically improved their structural stability as demonstrated using zeolite beta as example. The defects in the siloxy bonds were capped by reaction with trimethylchlorosilane, and Si-O-Si bonds were eventually formed. Hydrolysis of Si-O-Si bonds of the parent materials and dissolution of silica-oxygen tetrahedra in water causing a decrease in sorption capacity by reprecipitation of dissolved silica and pore blocking was largely mitigated by the treatment. The stability of the modified molecular sieves was monitored by (29)Si-MAS NMR, transmission electron micrographs, X-ray diffraction, and adsorption isotherms. The microporosity, sorption capacity, and long-range order of the stabilized material were fully retained even after prolonged exposure to hot liquid water.
Missing silicon–oxygen bonds in zeolites are shown to be the cause for structural instability of zeolites in hot liquid water. Their selective removal drastically improved their structural stability as demonstrated using zeolite beta as example. The defects in the siloxy bonds were capped by reaction with trimethylchlorosilane, and Si–O–Si bonds were eventually formed. Hydrolysis of Si–O–Si bonds of the parent materials and dissolution of silica–oxygen tetrahedra in water causing a decrease in sorption capacity by reprecipitation of dissolved silica and pore blocking was largely mitigated by the treatment. The stability of the modified molecular sieves was monitored by 29Si-MAS NMR, transmission electron micrographs, X-ray diffraction, and adsorption isotherms. The microporosity, sorption capacity, and long-range order of the stabilized material were fully retained even after prolonged exposure to hot liquid water.
Missing silicon-oxygen bonds in zeolites are shown to be the cause for structural instability of zeolites in hot liquid water. Their selective removal drastically improved their structural stability as demonstrated using zeolite beta as example. The defects in the siloxy bonds were capped by reaction with trimethylchlorosilane, and Si-O-Si bonds were eventually formed. Hydrolysis of Si-O-Si bonds of the parent materials and dissolution of silica-oxygen tetrahedra in water causing a decrease in sorption capacity by reprecipitation of dissolved silica and pore blocking was largely mitigated by the treatment. The stability of the modified molecular sieves was monitored by (29)Si-MAS NMR, transmission electron micrographs, X-ray diffraction, and adsorption isotherms. The microporosity, sorption capacity, and long-range order of the stabilized material were fully retained even after prolonged exposure to hot liquid water.Missing silicon-oxygen bonds in zeolites are shown to be the cause for structural instability of zeolites in hot liquid water. Their selective removal drastically improved their structural stability as demonstrated using zeolite beta as example. The defects in the siloxy bonds were capped by reaction with trimethylchlorosilane, and Si-O-Si bonds were eventually formed. Hydrolysis of Si-O-Si bonds of the parent materials and dissolution of silica-oxygen tetrahedra in water causing a decrease in sorption capacity by reprecipitation of dissolved silica and pore blocking was largely mitigated by the treatment. The stability of the modified molecular sieves was monitored by (29)Si-MAS NMR, transmission electron micrographs, X-ray diffraction, and adsorption isotherms. The microporosity, sorption capacity, and long-range order of the stabilized material were fully retained even after prolonged exposure to hot liquid water.
Missing silicon–oxygen bonds in zeolites are shown to be the cause for structural instability of zeolites in hot liquid water. Their selective removal drastically improved their structural stability as demonstrated using zeolite beta as example. The defects in the siloxy bonds were capped by reaction with trimethylchlorosilane, and Si–O–Si bonds were eventually formed. Hydrolysis of Si–O–Si bonds of the parent materials and dissolution of silica–oxygen tetrahedra in water causing a decrease in sorption capacity by reprecipitation of dissolved silica and pore blocking was largely mitigated by the treatment. The stability of the modified molecular sieves was monitored by ²⁹Si-MAS NMR, transmission electron micrographs, X-ray diffraction, and adsorption isotherms. The microporosity, sorption capacity, and long-range order of the stabilized material were fully retained even after prolonged exposure to hot liquid water.
Author Lercher, Johannes A
Burton, Sarah D
Arslan, Ilke
Prodinger, Sebastian
Vjunov, Aleksei
Derewinski, Miroslaw A
AuthorAffiliation TU München
Institute for Integrated Catalysis
Department of Chemistry and Catalysis Research Institute
Pacific Northwest National Laboratory
AuthorAffiliation_xml – name: Institute for Integrated Catalysis
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  givenname: Aleksei
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BackLink https://www.ncbi.nlm.nih.gov/pubmed/26972547$$D View this record in MEDLINE/PubMed
https://www.osti.gov/biblio/1254581$$D View this record in Osti.gov
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Snippet Missing silicon–oxygen bonds in zeolites are shown to be the cause for structural instability of zeolites in hot liquid water. Their selective removal...
Missing silicon-oxygen bonds in zeolites are shown to be the cause for structural instability of zeolites in hot liquid water. Their selective removal...
This work reports significant improvement in the hydrothermal stability of a well-characterized BEA zeolite via the selective removal of structural defects....
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SubjectTerms Environmental Molecular Sciences Laboratory
hydrothermal zeolite stability
nuclear magnetic resonance spectroscopy
sieves
silanol defects
silylation
sorption
sorption isotherms
X-ray diffraction
zeolites
Title Improving Stability of Zeolites in Aqueous Phase via Selective Removal of Structural Defects
URI http://dx.doi.org/10.1021/jacs.5b12785
https://www.ncbi.nlm.nih.gov/pubmed/26972547
https://www.proquest.com/docview/1779881209
https://www.proquest.com/docview/2000378441
https://www.osti.gov/biblio/1254581
Volume 138
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