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Heteroatom-Tolerant Delamination of Layered Zeolite Precursor Materials

Ogino, Isao and Eilertsen, Einar A. and Hwang, Son-Jong and Rea, Thomas and Xie, Dan and Ouyang, Xiaoying and Zones, Stacey I. and Katz, Alexander (2013) Heteroatom-Tolerant Delamination of Layered Zeolite Precursor Materials. Chemistry of Materials, 25 (9). pp. 1502-1509. ISSN 0897-4756. doi:10.1021/cm3032785.

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The synthesis of the first delaminated borosilicate layered zeolite precursor is described, along with its aluminosilicate analogue, which consists of Al-containing UCB-3 and B-containing UCB-4 from as-made SSZ-70. In addition, the delamination of PREFER (which is the precursor to ferrierite zeolite) under similar conditions yields delaminated layered zeolite precursors consisting of Al-containing UCB-5 and Ti-containing UCB-6. Multinuclear solid-state NMR spectroscopy (^(11)B and ^(27)Al), diffuse-reflectance UV-vis spectroscopy, and heteroatom/Si ratios measured via elemental analysis are consistent with a lack of heteroatom leaching from the framework following delamination. Such mild delamination conditions are achieved by swelling the zeolite precursor in a fluoride/chloride surfactant mixture in DMF solvent, followed by sonication. Powder X-ray diffraction, argon gas physisorption, and chemisorption of bulky base probes strongly suggest delamination, and demonstrate a 1.5-fold increase in the number density of external acid sites and surface area of calcined UCB-3, relative to calcined Al-SSZ-70. The synthesis of microporous pockets in materials UCB-3–UCB-5 suggests the possibility of interlayer porosity in SSZ-70, which is a layered zeolite precursor material whose structure remains currently unknown. The mildness of the delamination method presented here, as well as the lack of need for acidification in the synthesis procedure, enables the delamination of heteroatom-containing zeolites while preserving the framework integrity of labile heteroatoms, which could otherwise be leached under harsher conditions.

Item Type:Article
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URLURL TypeDescription
Hwang, Son-Jong0000-0002-3210-466X
Xie, Dan0000-0003-2467-976X
Katz, Alexander0000-0003-3487-7049
Additional Information:© 2013 American Chemical Society. Received: October 10, 2012; Revised: February 22, 2013; Published: February 27, 2013. E.E. is grateful to the Norwegian Research Council KOSKII for a fellowship at the University of California, Berkeley. The authors acknowledge Mr. Michael Nigra for DRIFT UV−vis spectra experiments and thank Kelly Harvey for editing coordination. The authors are grateful to the Management and Transfer of Hydrogen via Catalysis Program funded by Chevron Corporation for financial support.
Funding AgencyGrant Number
Norwegian Research Council KOSKIIUNSPECIFIED
Chevron CorporationUNSPECIFIED
Subject Keywords:delamination; exfoliation; layered zeolite precursor; SSZ-70; ferrierite zeolite; MCM-22(P)
Issue or Number:9
Record Number:CaltechAUTHORS:20130715-115713554
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Official Citation:Heteroatom-Tolerant Delamination of Layered Zeolite Precursor Materials Isao Ogino, Einar A. Eilertsen, Son-Jong Hwang, Thomas Rea, Dan Xie, Xiaoying Ouyang, Stacey I. Zones, and Alexander Katz Chemistry of Materials 2013 25 (9), 1502-1509
Usage Policy:No commercial reproduction, distribution, display or performance rights in this work are provided.
ID Code:39365
Deposited On:15 Jul 2013 21:37
Last Modified:09 Nov 2021 23:44

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