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At least 55 records · Page 3

Selective butene formation in direct ethanol-to-C3+-olefin valorization over Zn-Y/Beta and single-atom alloy composite catalysts using in situ generated hydrogen

The selective production of C3+ olefins from renewable feedstocks, especially via C1 and C2 platform chemicals, is a critical challenge for obtaining economically viable low-carbon middle distillate transportation fuels (i.e., jet and diesel). Here, we report a multifunctional catalyst system composed of Zn-Y/Beta and “single-atom” alloy (SAA) Pt-Cu/Al2O3 which selectively catalyzes ethanol-to-olefins (C3+, ETO) valorization in the absence of cofed hydrogen, forming butenes as the primary olefin products. Beta zeolites containing predominately isolated Zn and Y metal sites catalyze ethanol upgrading steps (588 K, 3.1 kPa ethanol, ambient pressure) regardless of cofed hydrogen partial pressure (0-98.3 kPa H2), forming butadiene as the primary product (60% selectivity at 87% conversion). The Zn-Y/Beta catalyst possesses site-isolated Zn and Y Lewis acid sites (at ~7 wt% Y) and Brønsted acidic Y sites, the latter of which has been previously uncharacterized. A secondary bed of SAA Pt-Cu/Al2O3 selectively hydrogenates butadiene to butene isomers at a consistent reaction temperature using hydrogen generated in situ from ethanol-to-butadiene (ETB) conversion. This unique hydrogenation reactivity at near-stoichiometric hydrogen and butadiene partial pressures is not observed over monometallic Pt or Cu catalysts, highlighting these operating conditions as a critical SAA catalyst application area for conjugated diene selective hydrogenation at high reaction temperatures (>573 K) and low H2/diene ratios (e.g., 1:1). Single-bed steady state selective hydrogenation rates, associated apparent hydrogen and butadiene reaction orders, and DFT calculations of the Horiuti-Polanyi reaction mechanisms indicate that the unique butadiene selective hydrogenation reactivity over SAA Pt-Cu/Al2O3 reflects lower hydrogen scission barriers relative to monometallic Cu surfaces and limited butene binding energies relative to monometallic Pt surfaces. DFT calculations further indicate the preferential desorption of butene isomers over SAA Pt-Cu(111) and Cu(111) surfaces while Pt(111) surface favors subsequent butene hydrogenation reactions to form butane over butene desorption events. Under operating conditions without of hydrogen cofeeding, this combination of Zn-Y/Beta and SAA Pt-Cu catalysts can selectively form butenes (65% butenes, 78% C3+ selectivity at 94% conversion) and avoid butane formation using only in situ generated hydrogen, avoiding costly hydrogen cofeeding requirements that hinder many renewable energy processes.

Cordon, Michael↗

Mechanistic understanding of catalytic conversion of ethanol to 1-butene over 2D-pillared MFI zeolite

Ethanol is an important C2 platform molecule for producing value-added chemicals and distillate hydrocarbon fuels (e.g., jet and diesel). Among these, catalytic upgrading of ethanol to butenes can generate valuable commodity chemicals (e.g., 1-butene) and provide C4 olefin intermediates that can be further upgraded to jet/diesel fuels. 2D zeolites offer hierarchical mesoporous structures, leading to improved mass transport and reduced diffusion length, which can help to address the coking challenges faced by ethanol conversion to hydrocarbons over 3D zeolites. In this study, we investigate the acid-catalyzed conversion of ethanol to 1-butene over the Brønsted acid sites (BAS) in 2D-pillared MFI zeolite (2D-PMFI) using ab initio molecular dynamics (AIMD) simulations, in situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), and calorimetric measurements. A detailed thermodynamic analysis, using quasi-harmonic approximation (QHA), on the Gibbs free energy pathway of ethanol conversion shows that the consideration of entropy is critical to accurately capture the detailed thermodynamic profiles. The formation of bulky ethoxy-ethene complex is found to be a potential rate-determining step (RDS), proceeding via stepwise mechanism. The reactivity of 2D-PMFI can be further tuned by manipulating RDS through a careful control of number of BAS and operating temperatures. The accuracy of computational model is confirmed through the comparison of calculated vibrational density of states (VDOS) against the experimental DRIFTS measurements. Overall, our study provides mechanistic insights into ethanol upgrading over the 2D-PMFI and shows the importance of evaluating entropic effects in such confined system.

Ethanol conversion, 2D-pillared zeolite, MFI, Anha↗

Tuning the zeolite acidity enables selectivity control by suppressing ketene formation in lignin catalytic pyrolysis

Unveiling catalytic mechanisms at a molecular level aids rational catalyst design and selectivity control for process optimization. In this study, we find that the Brønsted acid site density of the zeolite catalyst efficiently controls the guaiacol catalytic pyrolysis mechanism. Guaiacol demethylation to catechol initiates the reaction, as evidenced by the detected methyl radicals. The mechanism branches to form either fulvenone (c-C 5 H 4 = C = O), a reactive ketene intermediate, by catechol dehydration, or phenol by acid-catalyzed dehydroxylation. At high Brønsted acid site density, fulvenone formation is inhibited due to surface coordination configuration of its precursor, catechol. By quantifying reactive intermediates and products utilizing operando photoelectron photoion coincidence spectroscopy, we find evidence that ketene suppression is responsible for the fivefold phenol selectivity increase. Complementary fulvenone reaction pathway calculations, along with 29 Si NMR-MAS spectroscopy results corroborate the mechanism. The proposed, flexible operando approach is applicable to a broad variety of heterogeneous catalytic reactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Deeper Understanding of Mononuclear Manganese(IV)–Oxo Binding Brønsted and Lewis Acids and the Manganese(IV)–Hydroxide Complex

Binding of Lewis acidic metal ions and Brønsted acid at the metal–oxo group of high-valent metal–oxo complexes enhances their reactivities significantly in oxidation reactions. However, such a binding of Lewis acids and proton at the metal–oxo group has been questioned in several cases and remains to be clarified. In this work, we report the synthesis, characterization, and reactivity studies of a mononuclear manganese(IV)–oxo complex binding triflic acid, {[(dpaq)Mn IV (O)]–HOTf} + (1–HOTf). First, 1–HOTf was synthesized and characterized using various spectroscopic techniques, including resonance Raman (rRaman) and X-ray absorption spectroscopy/extended X-ray absorption fine structure. In particular, in rRaman experiments, we observed a linear correlation between the Mn–O stretching frequencies of 1–HOTf (e.g., ν Mn–O at ~793 cm –1 ) and 1–M n+ (Mn + = Ca 2+ , Zn 2+ , Lu 3+ , Al 3+ , or Sc 3+ ) and the Lewis acidities of H + and M n+ ions, suggesting that H+ and Mn+ bind at the metal–oxo moiety of [(dpaq)Mn IV (O)] + . Interestingly, a single-crystal structure of 1–HOTf was obtained by X-ray diffraction analysis, but the structure was not an expected Mn(IV)–oxo complex but a Mn(IV)–hydroxide complex, [(dpaq)Mn IV (OH)](OTf) 2 (4), with a Mn–O bond distance of 1.8043(19) Å and a Mn–O stretch at 660 cm –1 . More interestingly, 4 reverted to 1–HOTf upon dissolution, demonstrating that 1–HOTf and 4 are interconvertible depending on the physical states, such as 1–HOTf in solution and 4 in isolated solid. The reactivity of 1–HOTf was investigated in hydrogen atom transfer (HAT) and oxygen atom transfer (OAT) reactions and then compared with those of 1–Mn+ complexes; an interesting correlation between the Mn–O stretching frequencies of 1–HOTf and 1–M n+ and their reactivities in the OAT and HAT reactions is reported for the first time in this study.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Protonation Dynamics of Confined Ethanol–Water Mixtures in H-ZSM-5 from Machine Learning-Driven Metadynamics

Zeolites are indispensable heterogeneous catalysts in industrial chemical processes, valued for their strong Brønsted acidity, well-defined microporous frameworks, and tunable pore structures. Their catalytic activity arises primarily from Brønsted acid sites (BAS), typically present as bridging hydroxyl groups (Si–OH–Al). Under aqueous reaction conditions, these protons interact dynamically with water and alcohol molecules, leading to complex solvation and protonation behavior within confined pores. In this study, we investigate the protonation equilibrium occurring between ethanol and water at the BAS of acidic zeolites under varying hydration levels, i.e., C2H5OH–(H2O)n, n=1–4. Local structure was analyzed through an adaptive-learning global optimization algorithm, while enhanced sampling molecular dynamics simulations with Well-Tempered Metadynamics (WMetaD) and machine learning interatomic potentials (MLPs) provide free-energy surfaces (FES) at variable hydration levels. The results reveal a strong dependence of proton localization on the degree of hydration. At low hydration (1 water molecule), the proton resides predominantly on ethanol; with 2 water molecules, it shifts toward water, and at higher hydration (3 or more water molecules), it becomes extensively delocalized over the water cluster. These findings underscore the critical role of solvation in modulating acid site behavior and suggest that a minimum of three water molecules is necessary to fully stabilize the proton on water within the zeolite framework. This solvation threshold has significant implications for catalytic processes, particularly in biomass conversion reactions where alcohol protonation is a key step in dehydration mechanisms.

machine learning↗

Single-Walled Zeolitic Nanotube–Poly(oxazoline) Nanocomposites as Heterogeneous Catalysts for Acid–Base Cascade Reactions

Zeolites with a unique, 1-dimensional form factor were recently discovered − zeolite nanotubes (ZNTs). Here we describe the synthesis and characterization of NaH-ZNTpoly( oxazoline) composites targeting liquid-phase acid−base cascade catalysis. NaH-ZNT, a one-dimensional zeolite analogue with mesoporosity (3−4 nm) associated with nanotubes and inherent Brønsted acid sites associated with the microporous zeolite domains, is functionalized with poly(oxazoline)-based triblock copolymers with varying molecular weights (3−17 kDa). The composites are characterized using N2 sorption, STEM, FTIR, and elemental analysis, confirming successful grafting and preservation of the zeolite nanotube structure. The composites’ catalytic performance is evaluated through separate acid and base reactions, followed by a combined cascade of a deacetalization−Knoevenagel condensation for the synthesis of chalcone compounds. High initial reaction rates are demonstrated, but modest overall cascade product formation rates are observed, attributed to interactions between Brønsted acid sites and base amine groups that occur in the polymer-grafted systems. Physical mixtures of NaH-ZNT-SH and poly(oxazoline)s, lacking covalent linkages between ZNT and the polymer, support this supposition. This work demonstrates the potential of NaH-ZNT-poly(oxazoline) composites for liquid-phase cascade catalysis for synthesizing compounds of potential medicinal interest, highlighting the benefits of the grafting-to approach as well as the need for further optimization of the catalytic performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Electrochemically tunable proton-coupled electron transfer in Pd-catalyzed benzaldehyde hydrogenation

Acid-functionalization of carbon support allows enhancing the electrocatalytic activity of Pd to hydrogenate benzaldehyde to benzyl alcohol in proportion to the concentration of Brønsted acid sites. The hydrogenation rate is not enhanced when H2 is used. The rate enhancement is attributed to differences in the hydrogenation mechanism between the electrochemical and the H2 induced hydrogenations, in particular to the participation of hydronium ions formed at Brønsted acid sites at the perimeter of metal particles in proton coupled electron transfer.

Koh, Katherine↗

A molecular mediator for reductive concerted proton-electron transfers via electrocatalysis

Electrocatalytic approaches to the activation of unsaturated substrates via reductive concerted proton-electron transfer (CPET) must overcome competing, often kinetically dominant hydrogen evolution. We introduce the design of a molecular mediator for electrochemically triggered reductive CPET through the synthetic integration of a Brønsted acid and a redox mediator. Cathodic reduction at the cobaltocenium redox mediator substantially weakens the homolytic nitrogen-hydrogen bond strength of a Brønsted acidic anilinium tethered to one of the cyclopentadienyl rings. The electrochemically generated molecular mediator is demonstrated to transform a model substrate, acetophenone, to its corresponding neutral α-radical via a rate-determining CPET.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Selective catalytic reduction of NOx with NH 3 over Ce-Mn oxide and Cu-SSZ-13 composite catalysts – Low temperature enhancement

A composite catalyst comprised of ceria-manganese oxide and Cu-SSZ-13 components represents a potential solution for improving selective catalytic reduction (SCR) of NOx by ammonia. Here, clarity is provided to the pathway of promotion on these catalysts at low temperatures (< 200 °C), and it is shown that improved performance comes solely from interaction of the oxide phase with Brønsted acid bound NH 3 . We demonstrate that at low temperatures, the catalytic components interact via oxide-derived nitrites/nitrite-precursors (e.g., HONO, N 2 O 3 ) reacting with Brønsted acid bound NH3 from the zeolite. Then, only at elevated temperatures is the influence of the oxide phase on Cu redox in the Cu-SSZ-13 observed. Furthermore, we show how the oxide component has the great potential to circumvent NH 4 NO 3 inhibition on Cu-SSZ-13 in the composite catalysts at low temperatures by bypassing the formation of nitrates from NO 2 disproportionation, thus providing a practical solution to improving low temperature SCR reactivity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The role of the metal core in the performance of WO x inverse catalysts

In this study, metal-metal oxide inverse catalysts are valuable in diverse applications but selecting pairs is challenging. Here we investigate the role of metal cores (Pt, Ru, Rh, Pd, Ni) in the formation and dynamics of Brønsted acid sites on WO x overlayer on carbon. By in situ/ex situ characterizations, probe chemistry kinetics, and DFT calculations, we demonstrate that metals with varying work functions promote the WO x dispersion, enhancing the Brønsted acidity than the 3D crystallites on carbon at submonolayer coverages by tuning the oxidation state of WO x . The metal core impacts the water splitting and hydroxylation of WO x . Water splitting on Ru-WO x is thermodynamically favorable compared to Ni-WO x and increases the dehydration rate on the former, leading to an activity enhancement by increasing the H 2 pulsing frequency. This study provides insights into optimizing inverse catalysts.

36 MATERIALS SCIENCE↗

Tailoring Lewis/Brønsted acid properties of MOF nodes via hydrothermal and solvothermal synthesis: simple approach with exceptional catalytic implications

The Lewis/Brønsted catalytic properties of the Metal–Organic Framework (MOF) nodes can be tuned by simply controlling the solvent employed in the synthetic procedure. In this work, we demonstrate that Hf-MOF-808 can be prepared from a material with a higher amount of Brønsted acid sites, via modulated hydrothermal synthesis, to a material with a higher proportion of unsaturated Hf Lewis acid sites, via modulated solvothermal synthesis. The Lewis/Brønsted acid properties of the resultant metallic clusters have been studied by different characterization techniques, including XAS, FTIR and NMR spectroscopies, combined with a DFT study. The different nature of the Hf-MOF-808 materials allows their application as selective catalysts in different target reactions requiring Lewis, Brønsted or Lewis– Brønsted acid pairs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Dual Chemical Looping/Catalytic Process for Alkylation of Benzene With Ethane and Propane Yielding Ethylbenzene and Cumene Over Copper‐Containing Mordenite

Given the sustained demand for alkylated aromatics and the strained olefin market, there is an urgent need to develop efficient one‐step processes for the direct alkylation of aromatics using alkanes instead of olefins. Such technologies offer greater energy efficiency and sustainability by eliminating the need for separate, energy‐intensive alkane dehydrogenation steps. In this work, we report a dual chemical looping / catalytic process that couples alkane dehydrogenation with aromatic alkylation over a copper‐containing mordenite yielding up to 25% of alkylated aromatics with >97% selectivity per cycle. In situ MAS NMR and FTIR spectroscopies combined with DFT calculations showed that the alkylation of benzene with alkanes proceeds via a π‐bounded Cu(I)‐olefin intermediate, which subsequently interacts with benzene, catalyzed by Brønsted acid sites, leading to alkylated products that readily desorb from the active material into the gas phase. DFT calculations show that alkylation mediated solely by Cu(I) has prohibitively high barriers (>1.8 eV), whereas a bi‐functional pathway involving both Cu(I) and Brønsted acid sites can proceed with significantly lower barrier (0.8 eV) through a concerted C–C bond formation and proton transfer step.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Tuning the reactivity of carbon surfaces with oxygen-containing functional groups

Oxygen-containing carbons are promising supports and metal-free catalysts for many reactions. However, distinguishing the role of various oxygen functional groups and quantifying and tuning each functionality is still difficult. Here we investigate the role of Brønsted acidic oxygen-containing functional groups by synthesizing a diverse library of materials. By combining acid-catalyzed elimination probe chemistry, comprehensive surface characterizations, 15N isotopically labeled acetonitrile adsorption coupled with magic-angle spinning nuclear magnetic resonance, machine learning, and density-functional theory calculations, we demonstrate that phenolic is the main acid site in gas-phase chemistries and unexpectedly carboxylic groups are much less acidic than phenolic groups in the graphitized mesoporous carbon due to electron density delocalization induced by the aromatic rings of graphitic carbon. The methodology can identify acidic sites in oxygenated carbon materials in solid acid catalyst-driven chemistry.

Zhou, Jiahua↗

Measurement and Modeling of the effects of exhaust composition and hydrothermal aging on the ammonia storage capacity of a commercial Cu-SSZ-13 catalyst

Copper exchanged chabazites are among the state-of-the-art catalyst materials being studied for selective catalytic reduction of NOx, however, there is still a need to understand how these materials store ammonia after aging. In this work, studies are performed to assess the ammonia storage capacity of Cu-SSZ-13 as a function of concentration, temperature, and extent of hydrothermal aging. Ammonia binds at three difference sites: (i) a Cu site bound at 1 framework Al (Z 1 Cu site), (ii) a Cu site bound at 2 framework Al (Z 2 Cu site), and (iii) a Brønsted acid site (ZH site). Results show that a 3-site model can accurately capture ammonia storage across all conditions. Impacts for hydrothermal aging are considered via 3 aging reactions that change the site densities of each identified adsorption site. Model assessment shows that during aging there is a significant loss in Brønsted acid sites.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Powders and pellets – Extrusion engineering for a Cu/BEA syngas-to-hydrocarbons catalyst

Converting high-performing powder catalysts from the laboratory reactor scale into effective extruded catalysts at the industrial scale remains a hurdle for advancing sustainable catalytic processes, such as the conversion of biogenic syngas into high octane gasoline. Recently, a process-intensified syngas-to-hydrocarbons (STH) reaction in a single reactor under relatively mild conditions (220–250 ºC, 0.75–2.0 MPa) was reported, enabled by the development of a dimethyl ether (DME) homologation catalyst, Cu-modified H-BEA (Cu/BEA) zeolite. In this study, we explore approaches for synthesizing engineered Cu/BEA catalysts for use in the STH reaction to retain the high performance observed with the powder catalyst. We demonstrate that changes to the order of manufacturing steps (i.e., Cu deposition, alumina binder addition, and extrusion) result in observable changes to key active sites (Brønsted acid sites and zeolitic Cu + species), and ultimately, catalyst performance. When the Cu precursor was added directly to BEA before extrusion, both types of active sites were stabilized, preserving the activity of the powder catalyst. However, when the Cu precursor was added after extrusion, the resulting Cu species were mobile, destabilizing Brønsted acid sites and leading to near-zero activity.

09 BIOMASS FUELS↗

Interplay between copper redox and transfer and support acidity and topology in low temperature NH 3 -SCR

Low-temperature standard NH 3 -SCR over copper-exchanged zeolite catalysts occurs on NH 3 -solvated Cu-ion active sites in a quasi-homogeneous manner. As key kinetically relevant reaction steps, the reaction intermediate Cu II (NH 3 ) 4 ion hydrolyzes to Cu II (OH)(NH 3 ) 3 ion to gain redox activity. The Cu II (OH)(NH 3 ) 3 ion also transfers between neighboring zeolite cages to form highly reactive reaction intermediates. Via operando electron paramagnetic resonance spectroscopy and SCR kinetic measurements and density functional theory calculations, we demonstrate here that such kinetically relevant steps become energetically more difficult with lower support Brønsted acid strength and density. Consequently, Cu/LTA displays lower Cu atomic efficiency than Cu/CHA and Cu/AEI, which can also be rationalized by considering differences in their support topology. By carrying out hydrothermal aging to eliminate support Brønsted acid sites, both Cu II (NH 3 ) 4 ion hydrolysis and Cu II (OH)(NH 3 ) 3 ion migration are hindered, leading to a marked decrease in Cu atomic efficiency for all catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗