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At least 199 records · Page 11
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Role of Silica Support in Phosphoric Acid Catalyzed Production of p -Xylene from 2,5-Dimethylfuran and Ethylene

p-Xylene is a commodity chemical of industrial importance for terephthalic acid production, for which renewable sourcing from naturally abundant lignocellulosic biomass is highly desired. Previous work demonstrated that phosphoric acid stabilized on siliceous zeolite supports (e.g., P-BEA, P-SPP) exhibits high selectivity toward p-xylene (>97%) from 2,5-dimethylfuran (DMF) and ethylene. However, the effect of the support and the contribution of heterogeneous versus homogeneous phosphoric acid on the observed catalytic behavior in the solvated reaction system have not been addressed. Here, we determine the phosphoric acid catalytic activity for DMF conversion and its selectivity to p-xylene when it is supported on a silica support as well as in the absence of a support. Specifically, phosphoric acid catalysis was studied in three different scenarios: (1) phosphoric acid was added in the liquid reaction mixture in the absence of any solid support, (2) phosphoric acid was added in the liquid reaction mixture along with inert silica support including siliceous zeolite (i.e., allowing for phosphoric acid–support assembly to proceed in the reaction mixture), and (3) phosphoric acid was first impregnated on the siliceous zeolite support and then the preassembled supported phosphoric acid catalyst was added in the liquid reaction mixture. We found that the reaction rate and selectivity to p-xylene are different in the above scenarios reflecting the effect of the solid support on the catalytic performance of phosphoric acid. In scenario 1, a low concentration of phosphoric acid (1.7 mM) in the absence of any solid support exhibited high selectivity to p-xylene (80% selectivity to p-xylene at 60% conversion of DMF), which decreased with increasing acid concentration. The selectivity to p-xylene and activity of phosphoric acid significantly increased by adding a silica support into the reaction system (scenario 2). Furthermore, this improvement was attributed to phosphoric acid partial association with the surface of the silica support under the reaction conditions (in situ catalyst assembly). Phosphoric acid predeposited on siliceous zeolite supports (e.g., P-BEA, P-SPP) synthesized via impregnation prior to the reaction (scenario 3) catalyzed the reaction heterogeneously without noticeable leaching and exhibited the highest activity and selectivity to p-xylene, suggesting an important role of the silica support and the need to ensure that phosphoric acid acts as a heterogeneous catalyst in order to accomplish selective conversion of DMF to p-xylene.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Pilot-Scale Continuous Plug-Flow Hydrothermal Liquefaction of Food Waste for Biocrude Production

Pilot-scale hydrothermal liquefaction (HTL) of biowaste is a critical step toward commercialization of the HTL technology. Despite many HTL studies conducted with wet biomass, including food waste, few were performed with a pilot-scale continuous plug-flow reactor (PFR), with the biocrude yield and quality analysis based on dewatering (ASTM D2892 Annex X1). This paper describes the development and performance evaluation of a mobile pilot-scale HTL continuous PFR, with a processing capacity of 60 L/h of wet feedstock and 6 L/h of biocrude production. The reactor system was designed for reaction conditions of up to 325 °C and 17.25 MPa. The reactor has a volume of 28.88 L with an additional counterflow heat exchanger volume of 18.07 L. Two types of food wastes, from a food processing plant and grocery store, were processed at 280 °C for 30 min, producing biocrude oil yields of 52.19 and 47.06 wt %, energy recoveries of 68.17 and 70.77%, and carbon recoveries of 66.91 and 64.78%, respectively. Furthermore, due to its high feedstock capacity and reaction volume, large amounts of biocrude oil and post-HTL wastewater (PHW) were obtained from this pilot-scale reactor to allow downstream research on upgrading biocrude oil for transportation fuel as well as PHW treatment and nutrient recovery.

09 BIOMASS FUELS↗
DOE OSTI2021

Growth of Extra-Large Chromophore Supramolecular Polymers for Enhanced Hydrogen Production

The control of morphology in bioinspired chromophore assemblies is key to the rational design of functional materials for light harvesting. Here, we investigate here morphological changes in perylene monoimide chromophore assemblies during thermal annealing in aqueous environments of high ionic strength to screen electrostatic repulsion. We found that annealing under these conditions leads to the growth of extra-large ribbon-shaped crystalline supramolecular polymers of widths from about 100 nm to several micrometers and lengths from 1 to 10 μm while still maintaining a unimolecular thickness. This growth process was monitored by variable-temperature absorbance spectroscopy, synchrotron X-ray scattering, and confocal microscopy. The extra-large single-crystal-like supramolecular polymers are highly porogenic, thus creating loosely packed hydrogel scaffolds that showed greatly enhanced photocatalytic hydrogen production with turnover numbers as high as 13 500 over ~110 h compared to 7500 when smaller polymers are used. Our results indicate great functional opportunities in thermally and pathway-controlled supramolecular polymerization.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Selective and Efficient Production of Biomass-Derived Vinylfurans

We describe a two-step catalytic process for the selective and rapid conversion of biomass-derived acetylfurans into vinylfurans. This is accomplished by nearly quantitatively reducing acetylfurans into furyl alcohols using a copper chromite catalyst and exploiting the promoter-like properties of ethanol, the solvent. Subsequently, furyl alcohol is dehydrated using solid-acid catalysts. Catalyst deactivation due to oligomeric species is a major issue, but the activity can be partially recovered by calcination. Optimization of reaction conditions showed that the selectivity could be increased by using nitrobenzene, a polar aprotic solvent. Here, the high-boiling point solvent allows the formation of vinylfurans with a selectivity of up to 85%; the product can be isolated in high purity by distillation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Origin of Selective Production of Hydrogen Peroxide by Electrochemical Oxygen Reduction

Oxygen reduction reaction (ORR) is one of the most important electrochemical reactions. Starting from a common reaction intermediate *–O–OH, the ORR splits into two pathways, either producing hydrogen peroxide (H 2 O 2 ) by breaking the *–O bond or leading to water formation by breaking the O–OH bond. However, it is puzzling why many catalysts, despite the strong thermodynamic preference for the O–OH breaking, exhibit high selectivity for hydrogen peroxide. Moreover, the selectivity is dependent on the potential and pH, which remain not understood. Here, for this work, we develop an advanced first-principles model for effective calculation of the electrochemical reaction kinetics at the solid–water interface, which were not accessible by conventional models. Using this model to study representative catalysts for H 2 O 2 production, we find that breaking the O–OH bond can have a higher energy barrier than breaking *–O, due to the rigidity of the O–OH bond. Importantly, we reveal that the selectivity dependence on potential and pH is rooted into the proton affinity to the former/later O in *–O–OH. For single cobalt atom catalyst, decreasing potential promotes proton adsorption to the former O, thereby increasing the H 2 O 2 selectivity. In contrast, for the carbon catalyst, the proton prefers the latter O, resulting in a lower H 2 O 2 selectivity in acid condition. These findings explain the experiments and highlight the kinetic origins of the selectivity. Our work improves the understanding of ORR by uncovering the proton affinity as a new factor and provides a new model to effectively simulate the atomic-level kinetics of heterogeneous electrochemistry.

08 HYDROGEN↗
DOE OSTI2022

Highly selective and productive reduction of carbon dioxide to multicarbon products via in situ CO management using segmented tandem electrodes

Electrochemical CO 2 reduction provides a promising route to the sustainable generation of valuable chemicals and fuels. Tandem catalysts enable sequential CO 2 -to-CO and CO-to-multicarbon (C 2+ ) product conversions on complementary active sites, to produce high C 2+ Faradaic efficiency (FE). Unfortunately, previous tandem catalysts exhibit poor management of CO intermediates, which diminishes C 2+ FE. Here, we design segmented gas-diffusion electrodes (s-GDEs) in which a CO-selective catalyst layer (CL) segment at the inlet prolongs CO residence time in the subsequent C 2+ -selective segment, enhancing conversion. This phenomenon enables increases in both the CO utilization and C 2+ current density for a Cu/Ag s-GDE compared to pure Cu, by increasing the *CO coverage within the Cu CL. Lastly, we develop a Cu/Fe-N-C s-GDE with 90% C 2+ FE at C 2+ partial current density (j C2+ ) exceeding 1 A cm -2 . These results prove the importance of transport and establish design principles to improve C 2+ FE and j C2+ in tandem CO 2 reduction.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2025

Production of high-performance biodegradable polyurethane products made from algae precursors

We successfully developed and scaled the production of high-performance, fully biodegradable thermoplastic polyurethanes (TPUs) derived from algae-based precursors. By employing innovative flow chemistry and chemo-enzymatic methodologies, the research team produced materials with up to 100% bio-based content that match or exceed the mechanical properties of traditional petroleum-based plastics. These algae-derived TPUs were proven to be fully home-compostable, achieving over 90% decomposition within 110 to 120 days while demonstrating practical advantages such as reduced solvent requirements in fabric coating applications.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Cloud processing of dimethyl sulfide (DMS) oxidation products limits sulfur dioxide (SO 2 ) and carbonyl sulfide (OCS) production in the eastern North Atlantic marine boundary layer

Dimethyl sulfide (DMS) is the major sulfur species emitted from the ocean. The gas-phase oxidation of DMS by hydroxyl radicals proceeds through the stable, soluble intermediate hydroperoxymethyl thioformate (HPMTF), eventually forming carbonyl sulfide (OCS) and sulfur dioxide (SO 2 ). Recent work has shown that HPMTF is efficiently lost to marine boundary layer (MBL) clouds, thus arresting OCS and SO 2 production and their contributions to new-particle formation and growth events. To date, no long-term field studies exist to assess the extent to which frequent cloud processing impacts the fate of HPMTF. Here, we present 6 weeks of measurements of the cloud fraction and the marine sulfur species methanethiol, DMS, and HPMTF made at the Atmospheric Radiation Measurement (ARM) research facility on Graciosa Island, Azores, Portugal. Using an observationally constrained chemical box model, we determine that cloud loss is the dominant sink of HPMTF in this region of the MBL during the study, accounting for 79 %–91 % of HPMTF loss on average. When accounting for HPMTF uptake to clouds, we calculate campaign average reductions in DMS-derived MBL SO 2 and OCS of 52 %–60 % and 80 %–92 % for the study period. Using yearly measurements of the site- and satellite-measured 3D cloud fraction and DMS climatology, we infer that HPMTF cloud loss is the dominant sink of HPMTF in the eastern North Atlantic during all seasons and occurs on timescales faster than what is prescribed in global chemical transport models. Accurately resolving this rapid loss of HPMTF to clouds has important implications for constraining drivers of MBL new-particle formation.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRS1970

Saturn S-2 production operations techniques: Production welding. Volume 1: Bulkhead welding

The complex Saturn S-2 welding processes and procedures required considerable development and refinement to establish a production capability that could consistently produce aluminum alloy welds within specified requirements. The special processes and techniques are defined that were established for the welding of gore-to-gore and manhole- or closeout-to-gore.

Abel, O. G.↗
NASA NTRS1982

Coal desulfurization by chlorinolysis production and combustion test evaluation of product coals

Laboratory-scale screening tests were carried out on coal from Harrison County, Ohio to establish chlorination and hydrodesulfurization conditions for the batch reactor production of chlorinolysis and chlorinolysis-hydrodesulfurized coals. In addition, three bituminous coals, were treated on the lab scale by the chlorinolysis process to provide 39 to 62% desulfurization. Two bituminous coals and one subbituminous coal were then produced in 11 to 15 pound lots as chlorinolysis and hydrodesulfurized coals. The chlorinolysis coals had a desulfurization of 29-69%, reductions in voltatiles and hydrogen. Hydrodesulfurization provided a much greater desulfurization (56-86%), reductions in volatiles and hydrogen. The three coals were combustion tested in the Penn State ""plane flame furnace'' to determine ignition and burning characteristics. All three coals burned well to completion as: raw coals, chlorinolysis processed coals, and hydrodesulfurized coals. The hydrodesulfurized coals experienced greater ignition delays and reduced burning rates than the other coals because of the reduced volatile content. It is thought that the increased open pore volume in the desulfurized-devolatilized coals compensates in part for the decreased volatiles effect on ignition and burning.

Kalvinskas, J. J.↗
NASA NTRS1987

A new look at oxygen production on Mars - In situ propellant production (ISPP)

Consideration is given to the technique of producing oxygen on Mars from CO2 in the Martian atmosphere via in situ propellent production (ISPP). Mission implications of ISPP for both manned and unmanned Mars missions are described as well as ways to improve system reliability. Technology options that improve reliability and reduce power requirements include the use of adsorption pumps and advanced zirconia membranes. It is concluded that both manned and unmanned missions will benefit greatly from ISPP, especially in the context of a permanent manned base on Mars.

Frisbee, Robert H.↗