Deactivation of Sn-Beta zeolites caused by structural transformation of hydrophobic to hydrophilic micropores during aqueous-phase glucose isomerization

Cordon, Michael J.; Hall, Jacklyn N.; Harris, James W.; Bates, Jason S.; Hwang, Son-Jong; Gounder, Rajamani

doi:10.1039/c8cy02589d

Title: Deactivation of Sn-Beta zeolites caused by structural transformation of hydrophobic to hydrophilic micropores during aqueous-phase glucose isomerization

Journal Article · Tue Mar 05 00:00:00 EST 2019 · Catalysis Science and Technology

DOI:https://doi.org/10.1039/c8cy02589d· OSTI ID:1505311

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Purdue Univ., West Lafayette, IN (United States)
California Inst. of Technology (CalTech), Pasadena, CA (United States)

The structural changes underlying the deactivation of Sn-Beta zeolites under aqueous-phase reaction conditions at elevated temperatures (373 K) are investigated using spectroscopic characterization and site titration techniques together with turnover rates for glucose isomerization, a well-understood probe reaction for which changes in measured rates can be ascribed to specific changes in catalyst structure. In the case of hydrophobic, low-defect Sn-Beta zeolites (Sn-Beta-F), treatment in hot liquid water (373 K) for short times (<1 h) prior to reaction causes glucose–fructose isomerization turnover rates (per open Sn site, 373 K) to increase, while longer-term exposure (>3 h) to hot liquid water causes turnover rates to decrease and approach values characteristic of hydrophilic, defect-rich Sn-Beta zeolites (Sn-Beta-OH). However, turnover rates on hydrophilic Sn-Beta-OH zeolites are insensitive to the duration of hot liquid water exposure prior to reaction. Activation and deactivation phenomena on Sn-Beta-F zeolites occur concomitantly with the formation of silanol defects (by ~2–10×) with increasing durations (0–24 h) of hot water treatment, despite negligible differences in open and closed Sn site speciation as quantified ex situ by CD₃CN IR spectra. Mechanistic interpretations of these phenomena suggest that silanol groups present at low densities serve as binding sites for water molecules and clusters, which confer enthalpic stability to kinetically-relevant hydride-shift transition states and increase turnover rates, while silanol groups present in higher densities stabilize extended hydrogen-bonded water networks, which entropically destabilize kinetically-relevant transition states and decrease turnover rates. Intraporous voids within hydrophobic Sn-Beta-F zeolites become increasingly hydrophilic as silanol groups are formed by hydrolysis of framework siloxane bridges with increasing durations of water treatment, thereby decreasing aqueous-phase glucose isomerization turnover rates (per open Sn site). These findings imply design strategies that suppress framework hydrolysis would attenuate the deactivation of Lewis acid zeolites in aqueous media.

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Research Organization:: Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

Sponsoring Organization:: USDOE Office of Science (SC); National Science Foundation (NSF)

Grant/Contract Number:: AC05-00OR22725

OSTI ID:: 1505311

Journal Information:: Catalysis Science and Technology, Vol. 9, Issue 7; ISSN 2044-4753

Publisher:: Royal Society of ChemistryCopyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 35 works

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