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At least 235 records · Page 13

Nitrilotriacetamides: Nitric Acid and Water Extraction and Physicochemical Properties

Nitrilotriacetamides are an emerging class of extractants that have been identified as promising candidates for a variety of separation schemes. Systems incorporating these ligands are prone to third-phase formation at high loading, but this can be mitigated by increasing the alkyl chain length or adding a phase modifier (e.g., 1-octanol). In this work, the impacts of these modifications on HNO 3 extraction, H 2 O extraction, and physiochemical properties (interfacial tension, viscosity, and density) are examined. The studies show that ligand alkyl chain length has very little impact on HNO 3 and H 2 O extraction, whereas the addition of 10% octanol significantly increases extraction of both HNO 3 and H 2 O. Viscosity and interfacial ten-sion are impacted by HNO 3 concentration, alkyl chain length, and the presence of phase modifier but remain in a range that should be compatible with commonly used solvent contacting equipment. Additional studies of physiochemical properties at variable ligand concentration suggest that a change in aggregation occurs above approximately 10-50 mM ligand. Thermodynamic modeling of distribution ratios and spectroscopic studies aimed at understanding speciation in the presence of HNO 3 are also reported. Further, these experiments suggest that the first equivalent of extracted HNO 3 interacts with both the central amine and carbonyl groups of the ligand. The spectroscopic changes at higher HNO 3 concentrations are relatively minor, suggesting additional HNO 3 is associated in an outer-sphere manner

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Hierarchical Ion Interactions in the Direct Air Capture of CO 2 at Air/Aqueous Interfaces

The direct air capture (DAC) of CO 2 using aqueous solvents is plagued by slow kinetics and interfacial barriers that limit effectiveness in combating climate change. Functionalizing air/aqueous surfaces with charged amphiphiles shows promise in accelerating DAC; however, insight into these interfaces and how they evolve in time remains poorly understood. Specifically, competitive ion interactions between DAC reagents and reaction products feedback onto the interfacial structure, thereby modulating interfacial chemical composition and overall function. In this work, we probe the role of glycine amino acid anions (Gly - ), an effective CO 2 capture reagent, that promotes the organization of cationic oligomers at air/aqueous interfaces. These surfaces are probed with vibrational sum frequency generation spectroscopy and molecular dynamics simulations. Our findings demonstrate that the competition for surface sites between Gly - and captured carbonaceous anions (HCO 3 - , CO 3 2 -, carbamates) drives changes in surface hydration, which in turn tunes oligomer ordering. This phenomenon is related to a hierarchical ordering of anions at the surface that are electrostatically attracted to the surface and their ability to compete for interfacial water. These results point to new ways to tune interfaces for DAC via stratification of ions based on relative surface propensities and specific ion effects.

54 ENVIRONMENTAL SCIENCES↗

Driving force and pathway in polyelectrolyte complex coacervation

There is notable discrepancy between experiments and coarse-grained model studies regarding the thermodynamic driving force in polyelectrolyte complex coacervation: experiments find the free energy change to be dominated by entropy, while simulations using coarse-grained models with implicit solvent usually report a large, even dominant energetic contribution in systems with weak to intermediate electrostatic strength. Here, using coarse-grained, implicit-solvent molecular dynamics simulation combined with thermodynamic analysis, we study the potential of mean force (PMF) in the two key stages on the coacervation pathway for symmetric polyelectrolyte mixtures: polycation–polyanion complexation and polyion pair–pair condensation. We show that the temperature dependence in the dielectric constant of water gives rise to a substantial entropic contribution in the electrostatic interaction. By accounting for this electrostatic entropy, which is due to solvent reorganization, we find that under common conditions (monovalent ions, room temperature) for aqueous systems, both stages are strongly entropy-driven with negligible or even unfavorable energetic contributions, consistent with experimental results. Furthermore, for weak to intermediate electrostatic strengths, this electrostatic entropy, rather than the counterion-release entropy, is the primary entropy contribution. From the calculated PMF, we find that the supernatant phase consists predominantly of polyion pairs with vanishingly small concentration of bare polyelectrolytes, and we provide an estimate of the spinodal of the supernatant phase. Finally, we show that prior to contact, two neutral polyion pairs weakly attract each other by mutually induced polarization, providing the initial driving force for the fusion of the pairs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Effects of Salt Aggregation in Perfluoroether Electrolytes

Electrolytes comprised of polymers mixed with salts have great potential for enabling the use of Li metal anodes in batteries for increased safety. Ionic conductivity is one of the key performance metrics of these polymer electrolytes and achieving high room-temperature conductivity remains a challenge to date. For a bottom-up design of the polymer electrolytes, we must first understand how the structure of polyelectrolytes on a molecular level determines their properties. Here, we use classical molecular dynamics to study the solvation structure and ion diffusion in electrolytes composed of a short-chain perfluoroether with LiFSI or LiTFSI salts. Density functional theory is also used to provide some insights into the structures and energies of the salt interactions with the perfluoroether. We observe the formation of aggregates of salts in the fluorinated systems even at low salt concentrations. The fluorine-fluorine attraction in the solvent is the governing factor for creating the salt aggregates. The aggregates’ size and lifetime change with concentration and anion. These simulations provide an insight into the structure and dynamics of perfluoroether based electrolytes that can be used to improve Li-ion batteries.

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Dual-loop Solvent-based CCS for Net Negative CO 2 Emissions with Lower Cost

This final technical report details the successful design, construction, and operational validation of an innovative dual-loop CO 2 capture technology designed to achieve deep decarbonization (>99%) from Natural Gas Combined Cycle (NGCC) power plants that results in the electricity with carbon intensity of approximate 42 kg CO 2 -eq/MWh, less than the electricity produced by solar PV. The integrated process couples a primary aqueous solvent (in this project, a water lean solvent – WLS) absorption loop for bulk CO 2 removal with a secondary potassium hydroxide (KOH) polishing loop featuring electrochemical regeneration. This architecture leverages the higher exergy efficiency of the primary loop while utilizing the fastest kinetic of the secondary loop to capture dilute residual CO 2 , achieving an overall capture rate of 99.9% and co-producing pure hydrogen after moisture being condensed and dehydrated. Technical feasibility was established through a comprehensive 2,000-hour experimental campaign on a bench-scale fully-integrated unit (using 4” absorber and 4” stripper) with the feeding flue gas flowrate in the range of 8-20 cfm, confirming the attainment of Technology Readiness Level (TRL) 4. The project executed extensive parametric testing followed by 1,000 hours of continuous steady-state testing, demonstrating exceptional process stability with the electrochemical regenerator exhibiting less than a 10% reduction in electrical conductivity over the duration of the campaign. Operational characterization gathering on the bench unit revealed distinct energy profiles for the hybrid system: the primary loop required approximately 280 kJ mol -1 for bulk removal, while the polishing loop required approximately 1,600 kJ mol -1 specifically when reducing dilute CO 2 concentrations from ~740 ppm down to <50 ppm. (Please note those energy values/numbers can only be viewed as relative relationship and should not be extrapolated as absolute values required for CO 2 capture). Furthermore, dynamic testing validated the system’s flexibility for utility applications, demonstrating a rapid process response time of <30 minutes to changes in flue gas flowrate. Emission monitoring confirmed that the dual-loop architecture effectively mitigates solvent losses, utilizing a water wash to remove entrained aerosols to <1 ppm. The Techno-Economic Analysis (TEA) indicates a cost of capture of $\$$59.3/tonne and a Levelized Cost of Electricity (LCOE) of 71.7 $\$$/MWh at the overall capture efficiency of 99.8% of total carbon in the flue gas stream, with sensitivity analysis identifying an economic optimum when the primary loop captures 97% of the total CO 2 . A Life Cycle Assessment (LCA) confirms the technology’s potential for net-negative emissions, determining a Global Warming Potential (GWP) of 52 kg CO 2 -eq/MWh—significantly lower than the baseline—which further decreases to 42 kg CO 2 -eq/MWh when crediting the displacement of conventional hydrogen production.

03 NATURAL GAS↗

Carbon Capture in Novel Porous Liquids

Direct air capture (DAC) of CO 2 is one of the negative emission technologies under development to limit the impacts of climate change. The dilute concentration of CO 2 in the atmosphere (~400 ppm) requires new materials for carbon capture with increased CO 2 selectivity that is not met with current materials. Porous liquids (PLs) are an emerging material that consist of a combination of solvents and porous hosts creating a liquid with permanent porosity. PLs have demonstrated excellent CO 2 selectivity, but the features that control how and why PLs selectively capture CO 2 is unknown. To elucidate these mechanisms, density functional theory (DFT) simulations were used to investigate two different PLs. The first is a ZIF-8 porous host in a water/glycol/2-methylimidazole solvent. The second is the CC13 porous organic cage with multiple bulky solvents. DFT simulations identified that in both systems, CO 2 preferentially bound in the pore window rather than in the internal pore space, identifying that the solvent-porous host interface controls the CO 2 selectivity. Additionally, SNL synthesized ZIF-8 based PL compositions. Evaluation of the long-term stability of the PL identified no change in the ZIF-8 crystallinity after multiple agitation cycles, identifying its potential for use in carbon capture systems. Through this project, SNL has developed a fundamental understanding of solvent-host interactions, as well as how and where CO 2 binds in PLs. Through these results, future efforts will focus not on how CO 2 behaves inside the pore, but on the porous host-solvent interface as the driving force for PL stability and CO 2 selectivity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Assessment and Non-Destructive Evaluation of the Influence of Residual Solvent on a Two-Part Epoxy-Based Adhesive Using Ultrasonics

Polymers are increasingly being used in higher demanding applications due to their ability to tailor the properties of structures while allowing for a weight and cost reduction. Solvents play an important role in the manufacture of polymeric structures since they allow for a reduction in the polymer’s viscosity or assist with the dispersion of fillers into the polymer matrix. However, the incorrect removal of the solvent affects both the physical and chemical properties of polymeric materials. The presence of residual solvent can also negatively affect the curing kinetics and the final quality of polymers. Destructive testing is mainly performed to characterize the properties of these materials. However, this type of testing involves using lab-type equipment that cannot be taken in-field to perform in situ testing and requires a specific sample preparation. Here, a method is presented to non-destructively evaluate the curing process and final viscoelastic properties of polymeric materials using ultrasonics. In this study, changes in longitudinal sound speed were detected during the curing of an aerospace epoxy adhesive as a result of variations in polymer chemistry. To simulate the presence of residual solvent, samples containing different weight percentages of isopropyl alcohol were manufactured and tested using ultrasonics. Thermogravimetric analysis was used to show changes in the decomposition of the adhesive due to the presence of IPA within the polymer structure. Adding 2, 4, and 6 wt.% of IPA decreased the adhesive’s lap shear strength by 40, 58, and 71%, respectively. Ultrasonics were used to show how the solvent influenced the curing process and the final sound speed of the adhesive. Young’s modulus and Poisson’s ratio were determined using both the longitudinal and shear sound speeds of the adhesive. Using ultrasonics has the potential to non-invasively characterize the quality of polymers in both an in-field and manufacturing settings, ensuring their reliability during use in demanding applications.

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Environmentally improved CdTe photovoltaic recycling through novel technologies and facility location strategies

Abstract Photovoltaic waste is projected to reach up to 78 million tons across globally dispersed locations through 2050. Current recycling infrastructure is inadequate to process these waste volumes responsibly. This necessitates commercializing novel, environmentally advantageous photovoltaic recycling technologies that improve upon incumbent industrial operations. CdTe photovoltaic recycling is a promising candidate for improvements as 25,000 tons of spent modules are recycled worldwide annually. This paper evaluates the operational performance and compares six novel technologies, the incumbent technology used in industry and one technology which extends the incumbent process across ten environmental impact categories. The tradeoff between incurring a transportation burden (ship or road) to recycle in a large‐scale centralized facility with a higher operational efficiency and avoiding transportation by recycling in a small‐scale decentralized facility with a lower operational efficiency is evaluated. Thermal delamination to eliminate the ethylene vinyl acetate and separate the photovoltaic glass panels is preferable to the incumbent mechanical process across nine environmental impact categories and decreases the climate‐change impact of CdTe photovoltaic recycling by 23%. Bath and probe sonication are ineffective for delamination, and the use of organic solvents is more environmentally burdensome than the incumbent mechanical process. Centralized recycling with shipping is environmentally preferable than with road‐based transportation. For every 100‐km increase in road transportation from the decentralized to the centralized facility, the inventory requirement in the centralized facility should be 6% lower than the decentralized facility for centralized recycling to have a lower climate‐change impact than decentralized recycling. The corresponding value for shipping is 0.4%.

Ravikumar, Dwarakanath↗

The impact of climate on solvent-based direct air capture systems

Direct air capture (DAC) is increasingly seen as a critical technology to reach mid-century net-zero targets and limit climate change to well below 2 °C. While the commercialization of DAC technologies is being pursued by numerous companies, there remains remarkably little information on their performance under “real-world” conditions. In this paper, for the first time, we investigate the influence of temperature and relative humidity of air on the CO 2 capture rate at the air contactor, overall energy requirement, CO 2 capture efficiency, and levelized cost of liquid-solvent based DAC systems. We observe that the overall energy demand decreases from 11.1 to 8.3 GJ/tCO 2 as the CO 2 capture rate increases from 40 to 85 % and that high capture rates can only be achieved in hot and humid climate conditions. We observe that a CO 2 capture rate of 75 % is only possible above 17 °C and 90 % relative humidity, and this drops dramatically at lower temperatures. It is also observed that water evaporation in the air contactor is highest at dry and low relative humidity, as expected. The sensitivity analysis showed that CO 2 capture efficiency is relatively insensitive to climate conditions for the liquid-solvent based DAC plant. Lastly, the levelized cost of natural gas standalone scenario varies from $240/tCO 2 to $409/tCO 2 , and this is more sensitive to temperature than relative humidity. The levelized cost of the natural gas stand-alone case is between 7 % and 10 % lower than that of an electric grid-connected case across all climate conditions.

54 ENVIRONMENTAL SCIENCES↗

Modified Phenylethynyl Containing Imides for Secondary Bonding: Non-Autoclave, Low Temperature Processable Adhesives

As part of a program to develop structural adhesives for high performance aerospace applications, research continued on the development of modified phenylethynyl containing imides, LaRC(trademark)MPEIs. In previous reports, the polymer properties were controlled by varying the molecular weight, the amount of branching, and the phenylethynyl content and by blending with low molecular weight materials. This research involves changing the flexibility in the copolyimide backbone of the branched, phenylethynyl terminated adhesives. These adhesives exhibit excellent processability at pressures as low as 15 psi and temperatures as low as 288 C. The Ti/Ti lap shear specimens are processable in an autoclave or a temperature programmable oven under a vacuum bag at 288-300 C without external pressure. The cured polymers exhibit high mechanical properties and excellent solvent resistance. The chemistry and properties of these adhesives are presented.

Dezern, James F.↗

Characterization of Sequentially Extracted Soil Organic Matter by Electrospray Ionization and Atmospheric Pressure Photoionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry

Soil organic matter (SOM) is a complex mixture of small molecules and biopolymers that are active in various biogeochemical processes. However, the chemical diversity of biopolymer-derived SOM remains poorly explored. Identifying this diversity is important because global environmental changes may well alter SOM chemistry, as field experiments are beginning to show. Here, organic solvent-extractable (DcMe-SOM), base-hydrolyzable (KOH Hy -SOM), and CuO-oxidizable (CuO Ox -SOM) SOM fractions from a forest with a long-term nitrogen addition experiment were sequentially extracted and characterized by Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) coupled with negative-ion electrospray ionization (ESI) or atmospheric pressure photoionization (APPI). From DcMe-SOM to CuO Ox -SOM, the total number of assigned formulas, average O/C ratio, aromaticity, and unsaturation degree of SOM continuously increased, while the average m/z and H/C ratio decreased. Moreover, the dominant chemical category shifted from lipid-like components to phytochemical- and protein-like components. Complementary to ESI, APPI effectively facilitated detection of additional compounds with low polarity. With long-term nitrogen addition, the average m/z, unsaturation degree, aromaticity, and oxidation state of SOM increased, and more aromatic nitrogen-containing formulas were detected in CuOOx-SOM. Our study demonstrates that chronic nitrogen deposition in forests alters both the small molecules and biopolymers of SOM fundamentally.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A molecular switch regulating transcriptional repression and activation of PPARγ

Nuclear receptor (NR) transcription factors use a conserved activation function-2 (AF-2) helix 12 mechanism for agonist-induced coactivator interaction and NR transcriptional activation. In contrast, ligand-induced corepressor-dependent NR repression appears to occur through structurally diverse mechanisms. We report two crystal structures of peroxisome proliferator-activated receptor gamma (PPARγ) in an inverse agonist/corepressor-bound transcriptionally repressive conformation. Helix 12 is displaced from the solvent-exposed active conformation and occupies the orthosteric ligand-binding pocket enabled by a conformational change that doubles the pocket volume. Paramagnetic relaxation enhancement (PRE) NMR and chemical crosslinking mass spectrometry confirm the repressive helix 12 conformation. PRE NMR also defines the mechanism of action of the corepressor-selective inverse agonist T0070907, and reveals that apo-helix 12 exchanges between transcriptionally active and repressive conformations—supporting a fundamental hypothesis in the NR field that helix 12 exchanges between transcriptionally active and repressive conformations.

59 BASIC BIOLOGICAL SCIENCES↗

Leak Detection and Sensor Importance Within a Solvent Extraction Process Abstract

In anticipation of the Special Nuclear Material test bed (Beartooth), Idaho National Laboratory has developed a smaller, multi-sensor system for analyzing the solvent extraction process. These systems will allow for research into nuclear fuel processing operations. The multi-sensor system consists of a row of centrifugal contactors and allows for measurement sources that are not traditionally used in the solvent extraction process to be explored including temperature, vibration, acoustics, pH, color, flow, and motor current. Currently, the solvent extraction process is very labor intensive and requires vigilant operators to identify the occurrence of leaks, which can be common during startup or after any change to the system. This study aims to locate leaks using non-traditional measurement sources then to identify which signals were of greatest importance in making this classification using Local Interpretable Model-agnostic Explanations. These results can be used to help solvent extraction process operators detect leaks and to inform future test beds designers to which sensors contain relevant, actionable information in this scenario.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Kinetic processes of phase separation and aggregation behaviors in slot-die processed high efficiency Y6-based organic solar cells

Morphological optimization has proved to be one crucial factor contributing to the 19% efficiency of Y6-based organic solar cells (OSCs). Although the relationship between component miscibility and film morphology has been established, it has not been clarified how the film formation processes proceed, especially for methods compatible with large-area fabrication, i.e. slot-die coating, which restricts the further optimization of the morphology. Herein, we comprehensively investigate the effect of miscibility and the film-formation kinetic process on film morphology during processing with different solvents. A highest power conversion efficiency (PCE) of 17.38% can be obtained in a D18:Y6 device processed with slot-die coating in an open-air environment. However, due to their relatively poor miscibility, incorporating a trace amount of chlorobenzene (CB) into CF can sufficiently promote Y6 aggregation, leading to increased phase separation and thus the average PCE drops to 15.16%. In contrast, a PM6:Y6 blend shows insensitive changes in the kinetic process as well as the final morphology, and thus in the comparable PCEs when cast with different solvents, which is ascribed to their relatively good miscibility. As a result, this work provides scientific guidelines for device optimization by combining the intermediate gap from miscibility to kinetic process and their impact on final morphology.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Spatiotemporal Route to Understanding Metal Halide Perovskitoid Crystallization

Here, a spatiotemporal experimental route is reported for the antisolvent vapor diffusion crystal growth of metal halide perovskitoids. A computational analysis combining automated image capture and diffusion modeling enables the determination of the critical concentrations required for nucleation and crystal growth from a single experiment. Five different solvent systems and ten distinct organic ammonium iodide salts were investigated with lead iodide, from which nine previously unreported compounds were discovered. Automated image capture of the mother liquor and antisolvent vials was used to determine changes in solution meniscus positions and detect the nucleation event location. Matching the observations to a numerical solution of Fick's second law diffusion model enables the calculation of reactant, solvent, and antisolvent concentrations at both the time and position of the first stable nucleation and crystal growth. A machine learning model was trained on the resulting data, and it reveals solvent- and amine-specific crystallization tendencies. Solvent systems that interact more weakly with dissolved lead species promote crystallization, while those with stronger interactions can prevent crystallization through increased solubilities. Organic amines that interact more strongly with inorganic components and exhibit greater rigidity are more likely to be incorporated into crystalline products.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Recent Advances in the Use of Ionic Liquids and Deep Eutectic Solvents for Lignocellulosic Biorefineries and Biobased Chemical and Material Production

Biorefineries, which process biomass feedstocks into valuable (bio)products, aim to replace fossil fuel-based refineries to produce energy and chemicals, reducing environmental and health hazards, including climate change, and supporting a sustainable economy. In particular, lignocellulose-based biorefineries, utilizing the most abundant renewable feedstock on Earth, have significant potential to supply sustainable energy, chemicals and materials. Ionic liquids (ILs, organic salts with low melting temperatures) and deep eutectic solvents (DESs, mixtures with eutectic points lower than the ideal mixture) are capable of dissolving some of the key lignocellulose polymers, and even the whole biomass. Furthermore, they have intrinsic advantages over molecular solvents, including safer usage profiles and high tunability, which allow tailored physicochemical properties. Such properties provide unique opportunities for the development of new processes that could unlock the full potential of future biorefineries. Here, we review the current state of lignocellulosic biomass processing with ILs and DESs, with a specific focus on the pretreatment chemistry, process flow and products from each component; followed by discussions on sustainability assessments and technological challenges. We aim to inform the research community about the opportunities, challenges and perspectives in developing truly sustainable lignocellulose-based biorefineries.

09 BIOMASS FUELS↗

Accelerating Solvent Selection for Type II Porous Liquids

Type II porous liquids, comprising intrinsically porous molecules dissolved in a liquid solvent, potentially combine the adsorption properties of porous adsorbents with the handling advantages of liquids. Previously, discovery of appropriate solvents to make porous liquids had been limited to direct experimental tests. We demonstrate an efficient screening approach for this task that uses COSMO-RS calculations, predictions of solvent pK a values from a machine-learning model, and several other features and apply this approach to select solvents from a library of more than 11,000 compounds. Additionally, this method is shown to give qualitative agreement with experimental observations for two molecular cages, CC13 and TG-TFB-CHEDA, identifying solvents with higher solubility for these molecules than had previously been known. Ultimately, the algorithm streamlines the downselection of suitable solvents for porous organic cages to enable more rapid discovery of Type II porous liquids.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗