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At least 37 records · Page 2

18-membered macrocycle appended on resin for selective rare earth element extraction and separation

The rare earth elements are critically important for a wide range of modern technologies. However, obtaining them selectively and efficiently from natural sources and recycled materials is challenging and often requires harsh or wasteful conditions. Here we show that a macrocyclic chelator appended to a solid resin can overcome this challenge by acting as a robust platform for both the extraction and separation of these elements. This resin preferably captures the large rare earth elements in mixtures of these ions, giving rise to higher extraction efficiencies for them over the smaller ions. We further demonstrate that this resin can be used to separate rare earth elements. As a proof-of-principle validation, this resin was demonstrated to selectively extract rare earth elements in the presence of many different types of competing metal ions in a bioleachate solution obtained from autoslag waste, leading to their enrichment.

Coordination chemistry

Exploring the Functional Performance of a Commercial High-Temperature Photopolymer Resin for Vat Photopolymerized Injection Molding Tools

Additive manufacturing (AM) presents a promising approach for rapid tooling, offering significant reductions in production costs and lead times compared to that of conventional moldmaking processes. This work examines the fabrication of molds for injection molding through vat photopolymerization (VPP) AM, using a commercially available photopolymer resin intended for high temperature applications (High Temp V2 resin). The photorheological behavior of the resin is examined to evaluate its curing kinetics and mechanical development during polymerization, ensuring suitability for mold fabrication. The thermal and mechanical properties of the printed photopolymer resin are characterized, alongside assessments of dimensional accuracy and surface finish, which are critical factors influencing the performance and quality of injection molded parts. Additionally, specimens produced using VPP-fabricated molds are evaluated and benchmarked against those molded with traditional metal molds.

Jones, Haley W. [Savannah River National Laborator

Extraction and separation of rare earth elements using LN resins in hydrochloric acid

The separation of the rare earth elements is essential for numerous scientific applications but remains a significant challenge due to the nearly identical chemical properties of the adjacent lanthanide elements. Eichrom’s LN series of extraction chromatographic resins feature organophosphorus extractants and are widely used to achieve adjacent lanthanide separations. While extensive characterization of these resins has been completed for nitric acid matrices, the use of hydrochloric acid is preferred for a variety of applications. Further, the extraction of the rare earth elements, La–Lu and Y, has been characterized on LN and LN2 resins in hydrochloric acid via batch uptake and column chromatographic studies.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA

Mapping Structure and Rheology of pH-Responsive Resins for Low-VOC Coatings

In recent years, the paint and coatings industry has shifted away from traditional resin formulations that require high concentrations of volatile organic compounds (VOCs) to achieve the desired rheological performance and sustainability targets. One approach to eliminate or reduce VOCs in paint and coating formulations while maintaining the final performance is to disperse stimuli-responsive polymer latex particles in water. The chemistry and architecture of these particles have been engineered such that the suspension rheology changes in response to the pH changes. The particles can also be swollen with organic solvents to illicit similar rheological changes. To understand how the particle microstructure influences the observed macroscopic properties, we use small-angle neutron scattering and dynamic light scattering to determine that these particles consist of a cross-linked core with long polymer tails that extend into the dispersing medium. Carboxylic acid groups present on the tails deprotonate with increasing pH, and the extension of the polymer chain due to charge repulsion increases the hydrodynamic drag on the particle. Here we find that adjusting the pH alone has a much more significant effect on the shear dependence of the viscosity of the studied resin than adding organic solvent alone. We also find that this resin architecture is more responsive per mole of pH-responsive group than other architectures of pH-responsive latex particles in the literature.

36 MATERIALS SCIENCE

Enhancing Resource Recovery through Electro-Assisted Regeneration of an Ammonia-Selective Cation Exchange Resin

Ammonia-selective adsorbents can manage reactive nitrogen in the environment and promote a circular nutrient economy. Weak acid cation exchangers loaded with zinc exhibit high ammonia selectivity but face two implementation barriers: the stability of the zinc–carboxylate bond in complex wastewaters and energy- and logistics-intensive adsorbent regeneration with acidic solutions. In this paper, we examined the stability of zinc–carboxylate bonds in varying solutions (pure ammonium solution, synthetic urine, and real urine) and during electro-assisted regeneration. For electrochemical regeneration, both electrolyte concentration and current density influenced the trade-off between ammonia regeneration and zinc elution. Using 10 mM K 2 SO 4 anolyte at a 0.08 mA/cm 2 current density, we achieved 4% zinc elution and 61% ammonia regeneration. In contrast, using 100 mM K 2 SO 4 at 4.96 mA/cm 2 improved the regeneration efficiency to 97% but eluted 60% of zinc. We found that electrolyte concentration was the key factor influencing the regeneration efficiency of the NH 3 -selective adsorbents. Due to prevalent zinc elution, we designed an in situ procedure for reforming the zinc–carboxylate bond and achieved similar adsorption densities between pre- and post-regenerated resins, thus enabling multiple cycle resin use. Ultimately, this study advances understanding of ammonia-selective resins that can facilitate high-purity, selective, and durable recovery of nutrients from waste streams.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

A Mechanism-Based Reaction–Diffusion Model for Accelerated Discovery of Thermoset Resins Frontally Polymerized by Olefin Metathesis

Frontal ring-opening metathesis polymerization (FROMP) involves a self-perpetuating exothermic reaction, which enables the rapid and energy-efficient manufacturing of thermoset polymers and composites. Current state-of-the-art reaction–diffusion FROMP models rely on a phenomenological description of the olefin metathesis kinetics, limiting their ability to model the governing thermo-chemical FROMP processes. Furthermore, the existing models are unable to predict the variations in FROMP kinetics with changes in the resin composition and as a result are of limited utility toward accelerated discovery of new resin formulations. In this work, we formulate a chemically meaningful model grounded in the established mechanism of ring-opening metathesis polymerization (ROMP). Our study aims to validate the hypothesis that the ROMP mechanism, applicable to monomer-initiator solutions below 100 °C, remains valid under the nonideal conditions encountered in FROMP, including ambient to >200 °C temperatures, sharp temperature gradients, and neat monomer environments. Through extensive simulations, we demonstrate that our mechanism-based model accurately predicts the FROMP behavior across various resin compositions, including polymerization front velocities and thermal characteristics (e.g., T max ). Additionally, we introduce a semi-inverse workflow that predicts FROMP behavior from a single experimental data point. Notably, the physiochemical parameters utilized in our model can be obtained through DFT calculations and minimal experiments, highlighting the model’s potential for rapid screening of new FROMP chemistries in pursuit of thermoset polymers with superior thermo-chemo-mechanical properties.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

Nitrated Anion Exchange Resin Disposal Plan Calcination Studies

Reillex HPQ resin was nitrated in a manner matching procedures in use by the Aqueous Nitrate Recovery Facility. The resin was kept wet and then calcined to determine if nitrate was present in the residue. The potential for dispersion during heating and generation of soot or ash was evaluated. A series of experiments were performed by calcining the resin to 650 °C, and both residual solids and liquids were collected and measured for nitrates by Raman spectroscopy and test strip measurements.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W

Exploring the functional performance of a commercial hightemperature photopolymer resin for vat photopolymerized injection molding tools

• Selective photopolymerization of a liquid photocurable resin using ultraviolet (UV) or visible light in discrete layers • Photocurable resins are typically a mixture of monomer(s), oligomer(s), photoinitator(s), and additive(s), when applicable • Recent advances in high-performance resins have made VPP increasingly viable for functional tooling applications

Jones, Haley W. [Savannah River National Laborator

Zwitterionic Photocurable Resin for High‐Resolution 3D Printing of Ultralow‐Fouling Microstructures

High‐resolution 3D printing technologies are enabling a new generation of microstructured materials for applications where biocompatibility is critical. However, most conventional 3D‐printable resins yield materials that exhibit trade‐offs between antifouling properties and mechanical robustness, limiting their applicability in living systems. In nature, zwitterionic surface groups form tightly bound hydration layers that act as effective barriers against protein and cell attachment. Inspired by this strategy, a zwitterionic acrylamide‐based photoresist—carboxybetaine di‐methacrylamide (CBDA)—is developed for projection‐based vat photopolymerization, enabling the fabrication of complex microarchitectures with exceptional antifouling properties. The bifunctional monomer allows the formation of dense, cross‐linked networks that resist swelling while maintaining a high density of zwitterionic groups. Printed structures exhibit strong resistance to protein and cell adhesion, as confirmed by porcine blood assays, alongside robust mechanical performance. As a demonstration, a tubular structure featuring a negative Poisson's ratio lattice is printed to showcase structural fidelity and versatility. This resin formulation offers a broadly applicable strategy for fabricating microscale devices and surfaces where antifouling performance and structural integrity are both essential—spanning biomedical interfaces, soft robotics, and beyond.

3D printing

Separation of radium and actinium in acetic acid/acetate solutions using TK101 resin

Here, the uptake and elution behavior of Ra and Ac was studied on TK101 resin using acetic acid and acetate buffer (acetic acid/lithium acetate) solutions. There is high extraction of Ra (>10 3 ) over a wide range of acetic acid concentrations (0.02 to 4 M) with slightly lower extraction (>10 2 ) in the acetate buffer solutions (pH 3.9 to 5.6). The Ac extraction is considerably lower with a maximum D w of ∼100, and negligible extraction at high acetic acid concentrations (> 1 M) and in the acetate buffer solutions. The difference in D w can be leveraged for highly efficient separations of Ac from Ra, with no detectable Ra in the Ac fractions and high Ac yields (∼100%). These separations may be useful for radiopharmaceutical applications as the Ac purity is extremely high and the elution conditions can be optimized to be biologically safe and appropriate for chelation to molecules relevant to targeted alpha therapy.

and nuclear chemistry

Epoxy resin reinforced with carbonized chicken feathers: An innovative composite material with sustainable potentials

Here, this article explores a novel method for enhancing the mechanical properties of epoxy resin composites by incorporating carbonized chicken feathers as a filler material. The fabrication process involves carbonizing chicken feathers at 600°C and incorporating 5-10 wt% of the fillers into an epoxy matrix. The composites showed enhanced mechanical properties and samples containing 10 wt% filler exhibit the best properties. The performance corresponds to 49% increase in tensile strength, 16% rise in Young’s modulus, 40% improvement in flexural modulus, and 57% in flexural strength. X-ray diffraction and scanning electron microscopy with energy dispersive spectroscopy were employed to characterize the filler. This characterization provides valuable insights into the structure and chemical composition of the pulverized carbonized chicken feathers that contributed to the attained improvement in composites’ properties. Microstructural examination of the developed composite under scanning electron microscope also provides insights into matrix-filler interface and dispersion of the fillers within the composite matrix. The study not only highlights the unique combination of carbonized feathers’ inherent strength and compatibility with the epoxy matrix but also underscores the eco-friendly nature of utilizing agricultural waste. The findings suggest promising applications in industries demanding lightweight, high-strength materials, which can contribute to sustainable engineering solutions.

36 MATERIALS SCIENCE

Extraction of americium, curium, and californium with LN resin from HCl and HNO 3

The uptake of 241 Am, 244 Cm and 249 Cf with LN resin was studied in HCl and HNO3 solutions with concentrations ranging from 0.02 to 2.5 M. There is high uptake at concentrations < 0.1 M in both acids for all three isotopes with decreasing uptake at higher concentrations and negligible extraction at ≥ 0.6 M. Californium has a higher extraction than americium and curium, which are extremely similar. Kinetics studies showed rapid uptake of all three isotopes. Here, column studies were performed to demonstrate the separation of 241 Am and 249 Cf, and a bulk separation including nine stable lanthanides along with 241 Am, 249 Cf, and 88 Y.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA

TALSPEAK-based separation of the trivalent actinides from rare earth elements using LN resin

The separation of 241 Am, 244 Cm and 249 Cf from rare earth elements using LN resin and lactate buffer solutions with diethylenetriaminepentaacetic acid is described with numerous columns studies. The elutions are based on TALSPEAK liquid–liquid extraction chemistry, and provide high yield (> 90%), rapid, simple separations of the trivalent actinides from the lanthanides, which is often challenging due to similarities in chemical behavior among the trivalent f-block elements. Further, all three actinides can be separated from rare earth elements, including from massless fission product samples and samples with small amounts (~ 1–5 mg) of stable lanthanides. Separations with no detectable overlap between the actinide and lanthanide elutions is possible with massless samples, and in samples with mass high separation factors can be achieved (Am/Eu: 171; Am/La: 10 6 ).

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA

Resin chemistry and particle size influence on stereolithography with silicon carbide

Stereolithography (SLA) is an established process able to produce high resolution polymer parts with complex geometries. Silicon carbide (SiC) has uses in a variety of applications, but traditionally was difficult to manufacture into complex geometries. There have been advances in producing SiC through SLA using a SiC-derived ceramic such as silicon oxycarbide (SiOC). In this study, a slurry using a commercially available resin as the base material with additional modifiers was investigated to create a SiC slurry ready for pressureless sintering. The effects of photoinitiator, dispersant and a bimodal distribution of SiC particle sizes was studied using a design of experiments (DOE). A slurry with a bimodal distribution of 70 % coarse and 30 % fine SiC powder at 40 % solids loading by volume was prepared and successfully printed. Rheology measurements show the slurry to have viscoelastic shear thinning behavior below the recommended 1000 Pas necessary for printing. Printing parameters for the new material on a commercially available SLA printer were studied parametrically. The laser marking speeds found to print the slurry was 260 mm/s and 130 mm/s. A slurry and printing parameters were determined to produce a green part with a proposed debinding cycle.

Herd, Tien [ORNL]

Pixelated plastic scintillator array manufacturing using fast-, photo-curable resin

Pixelated plastic scintillator arrays can serve as high efficiency and high resolution neutron imaging detectors. Manufacturing these arrays is intensive in both time and labor. This article presents a fabrication method based on additive manufacturing for two-dimensional plastic organic scintillator arrays using a custom-built automated assembly machine and a custom photocurable resin that has significant non-aromatic acrylate oligomer content. The process involves two main stages: fully autonomous production of one-dimensional layered arrays, followed by semi-autonomous cutting and stacking to form two-dimensional pixel arrays. One-dimensional arrays were manufactured at a rate of around 4 layers per hour with minimal defects and tight dimensional tolerances, while two-dimensional arrays up to 7 x 7 pixels and 70 mm in length were completed in approximately 3.5 hours. Final arrays exhibited dimensional deviations of less than 0.5 mm. Two-dimensional arrays read out by a multi-anode photomultiplier tube demonstrated per-pixel position resolution and pulse-shape discrimination, enabling gamma–neutron interaction separation in mixed radiation environments.

36 MATERIALS SCIENCE

CO 2 Sorption in Moisture Swing Anion Exchange Resins for Direct Air Capture: Experimental Isotherm Determination and Modeling

Moisture swing (MS) sorption is a promising direct air capture (DAC) technology to achieve negative CO 2 emissions and counter global warming. Here, in this study, MS CO 2 sorption in a model MS sorbent, IRA900, was investigated. IRA900 is a macroporous commercial strong-base anion exchange resin (AER) with quaternary ammonium functional groups. A rigorous CO 2 desorption process was developed to desorb all CO 2 from the sample and obtain CO 2 sorption isotherms as a function of relative humidity, CO 2 partial pressure, and temperature. CO 2 sorption increased with decreasing relative humidity, decreasing temperature, and increasing CO 2 partial pressure. Remarkably, the total CO 2 uptake from the sorption isotherms matched the ion exchange capacity (IEC) of the material, suggesting a stoichiometry of one CO 2 molecule reacting per active site. An isotherm model for CO 2 sorption starting with empty sorption sites (i.e., with the AER in the OH – form) described the experimental data well, supporting the hypothesis that the bicarbonate-loaded AER fully unloaded to the OH – state following rigorous CO 2 desorption. CO 2 sorption kinetics were studied, and carbon diffusion coefficients were estimated as a function of %RH and CO 2 partial pressure. Overall, this study provides a roadmap for the systematic evaluation of MS CO 2 DAC materials.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI

Adsorption Equilibrium, Kinetics, and Column Breakthrough Data of Acetic Acid, Butyric Acid, and Lactic Acid on IRN-78 Ion-exchange Resin at Initial pH ~3 – 7 and Temperature 25 – 55 °C

This work presents systematic aqueous-phase adsorption equilibrium, kinetics, and column breakthrough measurements with three key biointermediates that are common compounds in many bioprocesses. Adsorption equilibrium experiments were carried out with acetic acid, butyric acid, and lactic acid on a commercial ion-exchange resin, Amberlite IRN-78, at wide ranges of acid concentration (8-500 mmol/L), initial pH (similar to 3-7), and temperature (25-55 degrees C), simulating the effluent characteristics from different fermenter operations. The kinetics and column breakthrough experiments were conducted at an initial pH of 6 and a concentration of 200 mmol/L. The equilibrium study shows a higher loading at the initial pH < pK(a) and a lower loading at the initial pH > pK(a). Overall removal varies between 16 and 99% depending on the initial pH, temperature, and organic acid concentration and type. The study further indicates monolayer adsorption at the equilibrium pH > 10 and multilayer adsorption at the equilibrium pH < 6. The thermodynamic modeling of adsorption isotherm data was carried out using Langmuir and Freundlich isotherms. IRN-78 presents fast adsorption kinetics as the maximum loading was attained in <= 10 min and nearly the same breakthrough time for all three organic acids involved in this study.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

Adsorption Equilibrium, Kinetics, and Column Breakthrough Data for Aqueous Solutions of Binary-Acid and Ternary-Acid Mixtures of Acetic Acid, Butyric Acid, and Lactic Acid on IRN-78 Ion-Exchange Resin at Initial pH Levels of ∼3–7 and at 25–55 °C

This work is part of an effort to develop thermophysical property data and models supporting adsorptive process development for organic acid separation from a dilute aqueous solution of fermentation broth. It presents systematic experimental measurements for aqueous-phase adsorption equilibrium, kinetics, and column breakthrough for three binary-acid aqueous mixtures (acetic acid + lactic acid, butyric acid + lactic acid, and acetic acid + butyric acid) and one ternary-acid aqueous mixture (acetic acid + butyric acid + lactic acid) on Amberlite IRN-78 ion-exchange resin. The equilibrium measurements covered broad ranges of the initial acid concentration (100–400 mmol/L), initial pH (∼3–7), and temperature (25–55 °C). The equilibrium data for the binary-acid and ternary-acid aqueous mixtures indicate selective adsorption of lactic acid at initial pH levels of ∼3 and 4, while acetic acid and butyric acid are selectively adsorbed at initial pH levels of 5, 6, and 7. The subsequent kinetics and column breakthrough experiments were performed at 200 mmol/L with equimolar ratios, an initial pH of 6, and 25 °C. In conclusion, the measurements provide essential data sets for rigorous thermodynamic modeling and process simulation of adsorptive separation processes for organic acid separation from fermentation broth.

Adsorption