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At least 55 records · Page 3

Ethylene Dehydroaromatization over Ga‐ZSM‐5 Catalysts: Nature and Role of Gallium Speciation

Abstract Bifunctional catalysis in zeolites possessing both Brønsted and Lewis acid sites offers unique opportunities to tailor shape selectivity and enhance catalyst performance. Here, we examine the impact of framework and extra‐framework gallium species on enriched aromatics production in zeolite ZSM‐5. We compare three distinct methods of preparing Ga‐ZSM‐5 and reveal direct (single step) synthesis leads to optimal catalysts compared to post‐synthesis methods. Using a combination of state‐of‐the‐art characterization, catalyst testing, and density functional theory calculations, we show that Ga Lewis acid sites strongly favor aromatization. Our findings also suggest Ga(framework)–Ga(extra‐framework) pairings, which can only be achieved in materials prepared by direct synthesis, are the most energetically favorable sites for reaction pathways leading to aromatics. Calculated acid site exchange energies between extra‐framework Ga at framework sites comprised of either Al or Ga reveal a site‐specific preference for stabilizing Lewis acids, which is qualitatively consistent with experimental measurements. These findings indicate the possibility of tailoring Lewis acid siting by the placement of Ga heteroatoms at distinct tetrahedral sites in the zeolite framework, which can have a marked impact on catalyst performance relative to conventional H‐ZSM‐5.

Zhou, Yunwen↗

Energetic decomposition yields efficient bimetallic Cu MOF-derived catalysts

Metal–organic frameworks (MOFs) have recently emerged as efficient self-sacrificial templates to fabricate porous carbon-supported metal nanoparticles (NPs). Due to observed increased activity, catalysts containing bimetallic NPs represent an active frontier for heterogeneous catalyst development. A strategy to synthesize active catalysts with highly dispersed bimetallic metal/metal oxides within a porous carbon matrix via rapid MOF decomposition using dopants is presented in this paper. A 2,4,6-trinitrotoluene (TNT) additive enhances the rapid thermolysis of the metal-doped Cu-based MOFs to minimize particle aggregation. Catalyst characterization reveals that a secondary metal increases dispersion of both metals over the carbon composite support. The catalyst preparation method influences both the metal particle size and oxidation state. Catalytic performance shows increased rates for 4-nitrophenol reduction even with <1 wt% of added secondary metal. Among the synthesized catalysts, the Ni–CuO@C bimetallic catalyst exhibits outstanding activity. This synthetic strategy is useful for creating highly efficient, robust, non-noble metal catalysts for development of sustainable chemical processes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

CH 4 steam reforming on Pt + Pd/Al 2 O 3 monolith: impact of Mn 0.5 Fe 2.5 O 4 spinel addition

The performance of Pt + Pd/Al 2 O 3 monolith catalysts was analyzed under a feed (H 2 + CO + CH 4 + NO + O 2 + H 2 O + CO 2 ) simulating the exhaust gas of stoichiometric natural gas vehicles (NGVs). The flow reactor results show enhanced low temperature (<400 °C) CH 4 oxidation activity under cyclic lean/rich feed modulation and with Mn 0.5 Fe 2.5 O 4 (MFO) spinel addition to the platinum group metal (PGM) catalyst. In the absence of the MFO spinel, the PGM catalyst can achieve full CH 4 conversion, but the presence of spinel in the catalyst limits the high temperature (>500 °C) CH 4 conversion. The depletion of gas phase O 2 , as indicated by the detection of products CO and H 2 in the reactor effluent at higher temperature and CH 4 conversion, portends the emergence of steam reforming of CH 4 (SRM). To investigate the cause of the detrimental impact of spinel under the high temperature, net rich regime, we show through a combination of SRM experiments and post-reaction catalyst characterization that SRM is negatively impacted by the accumulation of Mn and Fe spinel species on the PGM catalyst. This is due to the migration of the base metal species and potential encapsulation and blockage of PGM active sites. The latter is supported by density functional theory (DFT) calculations that indicate favorable metal oxide decoration of active Pt step sites. Lastly, a zoned catalyst design is developed that mitigates the detrimental metals migration while exploiting the methane conversion enhancement afforded by spinel oxides under oxygen rich conditions.

03 NATURAL GAS↗

Biofuel production from palm oil deoxygenation using nickel-molybdenum on zirconia catalyst using glycerol as a hydrogen donor

The growing demand for renewable energy has generated interest in biofuels as alternatives to fossil fuels. Second-generation biofuels, derived from deoxygenating fats and oils, have garnered a higher level of interest from industry and academia due to their potential for direct replacement of diesel and jet fuels. Palm oil, mostly cultivated in Thailand and composed of C16 and C18 fatty acids, is a primary feedstock sought for biofuel production. Palm oil deoxygenation contains several pathways that may or may not require hydrogen gas. This study aimed to produce biofuels in different fuel ranges, such as gasoline, jet fuel, and diesel, through palm oil deoxygenation using glycerol as a hydrogen source. Glycerol, a low-value byproduct, was used as a hydrogen donor, whereas nickel-molybdenum-supported catalysts were chosen for their high efficiency in deoxygenation and cost-effectiveness. The study investigated the impact of reaction time, temperature, and catalyst activation method on palm oil deoxygenation. Catalyst characterization methods, including XRD, SEM, TEM, XPS, FTIR, TGA, and nitrogen-sorption, were employed to understand the role of catalysts’ activity during palm oil upgrading. Findings indicated that alkane hydrocarbons are the major components in liquid products. The presence of excess hydrogen in post reaction gaseous phase proves the hydrogen donation capability of glycerol. Increased reaction time and temperature facilitated the removal of oxygen from palm oil. Nickel-molybdenum on zirconia activated by sulfidation demonstrated higher stability than by reduction activation.

09 BIOMASS FUELS↗

Ensembles of Metastable States Govern Heterogeneous Catalysis on Dynamic Interfaces

Heterogeneous catalysis is at the heart of chemical industry. Being able to tune and design efficient catalysts for processes of interest is of an utmost importance, and for this, the molecular-level understanding of heterogeneous catalysts is the first step, and indeed a prime focus of the modern catalysis research. For a long time, a single most thermodynamically stable structure of the catalytic interface attained in reaction conditions had been envisioned as the reactive phase. However, some catalytic interfaces continue to undergo structural dynamics in the steady state, triggered by high temperatures, pressures, and binding and changing reagents. Among particularly dynamic interfaces are such widely-used catalysts as crystalline and amorphous surfaced supporting (sub-)nano metallic clusters. Recently, it became clear that this dynamic fluxionality causes the supported clusters to populate many distinct structural and stoichiometric states in catalytic conditions. Hence, the catalytic interface should be viewed as an evolving statistical ensemble of many (not one) structures. As such, every member in the ensemble contributes to the properties of the catalyst differently, and in proportion to its probability to be populated. This new notion flips the established paradigm and calls for new theory, modeling approaches, operando measurements, and updated design strategies. The statistical ensemble nature of surface-supported sub-nano cluster catalysts can be exemplified by oxide-supported and adsorbate-covered Pt, Pd, Cu, CuPd clusters, catalytic toward oxidative and non-oxidative dehydrogenation. They have access to a variety of 3D and quasi-2D shapes. The compositions of their thermal ensembles are dependent on the cluster size, leading to size-specific catalytic activities and the famous “every atom counts” phenomenon. The support and adsorbates affect catalyst structures, and state of the reacting species causes the ensemble to change in every reaction intermediate. The most stable member of the ensemble dominates the thermodynamic properties of the corresponding intermediate, whereas the kinetics can be determined by more active but less populated metastable catalyst states, and that suggests that many earlier studies might have overlooked the actual active sites. Both effects depend on the relative time-scales of catalyst restructuring and reaction dynamics. The catalyst may routinely operate off-equilibrium. Ensemble phenomena lead to surprising exceptions from established rules of catalysis, such as scaling relations, and Arrhenius behavior. Catalyst deactivation is also an ensemble property, and its extent of mitigation can be predicted through the new paradigm. These findings were enabled by advances in theory, such as global optimization and subsequent utilization of multiple local minima, and pathways sampling, as well as operando catalyst characterization. The fact that the per-site and per-species resolution is needed for the description and predicting of catalyst properties gives theory the central role in catalysis research, as most experiments provide ensemble-average information and cannot detect the crucial minority species that may be responsible for the catalytic activity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Reactive Separations of CO/CO 2 mixtures over Ru–Co Single Atom Alloys

Reactive separations of CO/CO 2 mixtures are a promising pathway to lower the energy requirement of CO 2 hydrogenation to chemicals and fuels, with applications in the U.S. Navy’s seawater-to-fuel process. With the CO/CO 2 feedstock, a challenge is activating CO to produce heavier hydrocarbons while preventing CO 2 methanation, requiring low-temperature Fischer-Tropsch synthesis (FTS) catalysts. In this work, we demonstrate that a Ru–Co single atom alloy (SAA) catalyst produces C 5+ hydrocarbons at a rate of 11.7 μmol/s/g-cobalt (hexane basis) in a 50/50 CO/CO 2 stream with ≤1% CO 2 conversion. The reaction operates at a relatively low temperature (200 °C) and high gas hourly space velocity (GHSV: 84,000 mL/g/h) that is compatible with the upstream reverse water-gas shift reaction. Detailed experiments, catalyst characterizations, and density functional theory (DFT) calculations have been conducted to understand the active phase, the role of the Ru dopant, and catalyst restructuring that occurs at elevated temperatures (>200 °C). Ru dopants are found to promote the reduction of Co species, enabling catalytic activity for CO hydrogenation without pre-reduction, but may not enhance the FTS activity or desired C 5+ hydrocarbon selectivity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Hydrogenolysis of Poly(Ethylene–co–Vinyl Alcohol) and Related Polymer Blends over Ruthenium Heterogeneous Catalysts

The hydrogenolysis of polymers is emerging as a promising approach to deconstruct plastic waste into valuable chemicals. Yet, the complexity of plastic waste, including multilayer packaging, is a significant barrier to handling realistic waste streams. Herein, we reveal fundamental insights into a new chemical route for transforming a previously unaddressed fraction of plastic waste – poly(ethylene–co­­–vinyl alcohol) (EVOH) and related polymer blends – into alkane products. Additionally, we report that Ru/ZrO2 is active for the concurrent hydrogenolysis, hydrogenation, and hydrodeoxygenation of EVOH and its thermal degradation products into alkanes (C1–C35) and water. Detailed reaction data, product analysis, and catalyst characterization reveal that the in–situ thermal degradation of EVOH forms aromatic intermediates that are detrimental to catalytic activity. Increased hydrogen pressure promotes hydrogenation of these aromatics, preventing catalyst deactivation and improving alkane product yields. Calculated apparent rates of C–C scission reveal that the hydrogenolysis of EVOH is slower than low–density polyethylene. We apply these findings to achieve hydrogenolysis of EVOH/polyethylene blends and elucidate the sensitivity of hydrogenolysis catalysts to such blends. Overall, we demonstrate progress towards efficient catalytic processes for the hydroconversion of waste multilayer film plastic packaging into valuable products.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Selective Hydrogenation of Biomass-Derived 2(5H)-Furanone to γ-Butyrolactone over Ni-Based Bimetallic Catalysts

2(5H)-Furanone was selectively hydrogenated to γ-butyrolactone (GBL) over Ni-based bimetallic catalysts, Ni-M/SiO2 (M = Fe, Co, Cu, and Zn). Catalyst characterization showed that the metal dispersion and reducibility were changed after introducing a second metal, while the physical morphology was nearly unchanged. The most active and selective bimetallic catalyst was found to be Ni–Fe/SiO2. The reaction rate constant over the 4 wt %Ni–1 wt %Fe/SiO2 bimetallic catalyst was 0.06 min–1, doubling that over 5 wt %Ni/SiO2, and the selectivity to GBL increased slightly from 86.1 to 89.5%. The Fe/(Ni+Fe) weight ratio was changed to optimize the promoting effect of Fe. The Ni–Fe bimetallic effect was further investigated using temperature-programmed desorption experiments on single crystal model surfaces with different Fe/Ni(111) structures, revealing that the enhanced catalyst activity was mainly contributed by the formation of the Ni–Fe surface alloy.

bio-inspired↗

Evolution of size-selected Pt cluster catalysts on prototypical oxide supports

The current quest for new pathways into sustainable, efficient and durable energy conversion technologies makes the used for a fundamental understanding of the atomic-scale phenomena underlying catalytic processes ever more pressing. In this context, characterizing catalyst particles in situ provides valuable information about the evolution of their composition, structure, oxidation state and charge state during an ongoing process. To disentangle the influence of individual parameters – temperature, pressure, gas composition, cluster size, as well as support acidity, redox state and defect density – it is crucial to control them precisely and separately in experiments. At the example of size-selected Pt n clusters – i.e. sub-nm particles defined to the exact number of atoms – on flat oxide supports, we follow their rich evolution phenomena via (synchrotron-based) X-ray photoelectron spectroscopy (XPS) and scanning tunnelling microscopy (STM) during temperature ramps and in various gas environments. Here, we present our experience with these highly defined, yet complicated-to-create samples in ultra-high vacuum (UHV) and at mbar pressures. We discuss their stability during transport to synchrotrons and under reaction conditions on three prototypical oxide supports and show the various phenomena that can be disentangled. Ptn clusters on the non-reducible silicon dioxide, SiO 2 , remain size-selected and show remarkable stability. Doping strongly influences the size-dependent binding energy shifts and changes the Pt response to oxidative and reaction conditions, which we attribute to different cluster geometries: p-type doping leads to wetting, enhanced sinter resistance and a diminished response to oxidative environments, compared to clusters on n-type doped samples. We compare the system with our previous findings of a similar change in dimensionality for Pt 20 clusters on the reducible ceria, CeO 2 (111), support, induced by modulation of its O vacancy density. The Pt n /CeO 2 system is particularly interesting for strategies to stabilize and redisperse Pt clusters dynamically. Finally, we study the evolution of Pt n clusters on another reducible oxide support, magnetite, Fe 3 O 4 (001), in 0.1 mbar alternating redox conditions at RT and elevated temperature. In analogy to findings previously reported for Pt/TiO 2 (110), the clusters either become encapsulated by a thin oxide film via strong metal–support interaction (SMSI) or deeply buried in the magnetite. Overall, our approach of following the evolution of size-selected clusters on oxide supports leads to fundamental atomic-scale insights on nano-scale catalyst materials, on our path to sustainable, dynamic and self-repairing catalysts.

Falling, Lorenz J. [Technical Univ. of Munich (Ger↗

Surface Science Studies of Selective Fischer-Tropsch Chemistry on Cobalt Carbide Surfaces

Advances in catalysis science are critical to the progress of the United States. Catalysis is employed, in one way or another, in the production of almost every chemical and product manufactured. The catalysis research that we undertook here, regarding the role of specific facets of cobalt carbide in the Fischer-Tropsch production of low molecular weight olefins (FTO), is motivated by the work of many previous investigators. In particular two research groups from China had discovered FTO catalysts that work very selectively for low molecular weight olefins coupled with low production of methane. These are potentially very important findings that could find significant industrial utility if improvements can be discovered. With the research undertaken here we chose to focus on one of these studies and especially the Co 2 C surfaces that they implicate as being responsible for this exciting FTO catalysis with low production of methane. In this study, Zhong and co-workers investigated cobalt-manganese oxide catalysts for the Fischer-Tropsch to Olefins process. After reaching steady-state their catalyst showed a good selectivity to light olefins and low selectivity to methane with a carbon monoxide conversion of 31.8% at one atmosphere (with a H 2 /CO ratio of two and a temperature of 250°C). Lower H 2 /CO ratios and lower pressures increased the olefin production. Their catalyst characterization studies indicated that cobalt carbide quadrangular nanoprisms with preferentially exposed (101) and (020) facets were important in favoring lower olefin production and inhibiting methane formation. The authors stated that these cobalt carbide nanoprisms are a promising new catalyst system for directly converting synthesis gas to lower olefins. Motivated by the studies of Zhong and co-workers, our goal with the research here was to contribute to a better understanding of catalysis science through the study of surface chemical reactions related to the Fischer-Tropsch to Olefins reaction on specific facets of planar model cobalt carbide catalysts in ultrahigh vacuum.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

New Approaches to Improved PEM Fuel Cell Catalyst Layers

Polymer-electrolyte membrane (PEM) fuel-cells are one of the most promising energy conversion technologies for renewable clean energy applications. A major challenge preventing their widespread commercialization is achieving high performance with lowloadings of platinum group metal (PGM) catalysts. One of the factors driving performance limitations in the cell is the mass transport losses within the cathode catalyst layers due to sluggish oxygen-reduction reactions occurring at the platinum-ionomer interface, which is believed to be linked to reduced transport of ions and oxygen. A viable solution to reduce the transport resistances in the catalyst layers is to create new ionomers that can provide good ion and oxygen transport needed to accomplish high-performing fuel cell catalysts. Characterization of transport properties of ionomers for various molecular architectures is the key step, in the effort to create and identify the optimized polymer structure with improved transport. Using this approach, Tetramer Technologies and LBNL propose improved fuel-cell catalyst ionomers based on Tetramers proprietary polymer chemistry, as highlighted under subtopic 17a Innovative Approaches Toward Discovery and Development of Improved Ionomers for Polymer Electrolyte Membrane Fuel Cell Catalyst Layer.

30 DIRECT ENERGY CONVERSION↗

Characterization of Pt/SnO2 catalysts for CO oxidation

Results are presented of surface characterization of 2% and 1% (w/w) Pt on SnO2 catalysts which are being used in promoting the oxidation of CO in pulsed CO2 lasers. The N2 adsorption BET surface area for both catalysts is 6.9 sq m/g. The CO chemisorbed area at 313K is 0.17 sq m/g and 0.062 sq m/g for the 2% and 1% catalysts, respectively. Monitoring the reaction between CO and O2 by the same technique, at the same temperature yields a turn-over frequency (TOF) for the 2% catalyst of 2.7 x 100 molecules of CO2/site/s and for the 1% catalyst a value of 1.2 x 100. The ratio of the TOFs for the two catalysts is 2.2 which is approximately the ratio of the Pt loading.

Brown, K. G.↗

Novel manganese-promoted inverse CeO 2 /CuO catalyst: In situ characterization and activity for the water-gas shift reaction

In this study, the behavior of a novel manganese-promoted inverse CeO 2 /CuO catalyst under water-gas shift (WGS) reaction conditions is studied. CeO 2 /CuO and CeO 2 /Mn-CuO catalysts are characterized by X-ray diffraction (XRD), Raman and X-ray photoelectron spectroscopy (XPS). Structure/activity relationships and redox characteristics are established on the basis of such results along with those of in situ XRD and X-ray absorption fine structure (XAFS) experiments performed either under WGS or CO-temperature programmed reduction (TPR) conditions. The manganese coprecipitated together with the copper during the preparation of the samples and the Mn-CuO phase strongly affected the size and chemical properties of the catalytically-active ceria nanoparticles. A manganese-induced enhancement on the WGS activity was observed. As a result, differences in the characteristics of the supported ceria particles are proposed as most relevant to explain the observed Mn-promoting effect.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A comparative study between real-world and laboratory accelerated aging of Cu/SSZ-13 SCR catalysts

Elucidating aging mechanisms in real-world applications is a critical component for developing and maintaining Cu/SSZ-13 SCR catalysts. To reveal gaps between laboratory accelerated aging and real-world aging, herein we report thorough comparative studies between 6 representative catalysts. Here, we apply a wide range of catalyst characterization methods, including surface area/porosity analysis, X-ray diffraction (XRD), H 2 -temperature programmed reduction, NH3-temperaure programmed desorption, solid-state nuclear magnetic resonance (NMR), in situ X-ray photoelectron (XPS) and electron paramagnetic resonance (EPR) spectroscopies, to gain atomic-level knowledge on Cu transformation under different aging protocols. We then correlate such knowledge to SCR, NH 3 /NO oxidation kinetic behavior of the catalysts. We found that sulfur aging plays the most important role in interpreting catalyst degradation during real-world application, including direct sulfur poisoning of isolated Cu II SCR active species to CuSO 4 -like species, the agglomeration of such species to multinuclear CuSO 4 clusters, and eventually, CuO formation during desulfation treatments. Such chemistries convert SCR active Cu to SCR inert Cu moieties without severely deteriorating catalyst support integrity. These characteristics are partially replicated by hydrothermal aging in the presence of SOx but are poorly mimicked by hydrothermal aging alone.

36 MATERIALS SCIENCE↗

Hydrogenolysis of Polypropylene and Mixed Polyolefin Plastic Waste over Ru/C to Produce Liquid Alkanes

Catalytic depolymerization of polyolefins is a promising chemical recycling strategy to create value-added products from waste plastics, which are accumulating in landfills and the natural environment at unsustainable rates. The cleavage of strong C–C bonds in polyolefins can be performed using a noble metal and hydrogen via a hydrogenolysis mechanism. Previously, we identified ruthenium nanoparticles supported on carbon (Ru/C) as a highly active heterogeneous catalyst for the conversion of polyethylene into liquid and gaseous n-alkanes under mild conditions. In the present study, we investigated the catalytic depolymerization of polypropylene (PP) under mild conditions (200–250 °C, 20–50 bar H 2 ). We demonstrate that Ru/C produces C 5 –C 32 iso-alkane yields above 68% in the absence of solvent and identify trade-offs between product yield and temperature, hydrogen pressure, and reaction time. We apply a rigorous analytical method to quantify all liquid and gaseous alkane products. The characterized catalyst was found to be recyclable after the complete depolymerization of high molecular weight PP (M w ~ 340,000 Da) to liquid and gaseous hydrocarbons and after depolymerization of a postconsumer PP centrifuge tube. Finally, the catalyst was shown to be effective in depolymerizing a mixture of high-density polyethylene and PP to produce a mixture of linear and branched liquid alkanes, demonstrating feasibility for the depolymerization of streams of mixed polyolefin waste.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗