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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Thermal Activation of Zirconium(IV) Acetylacetonate Catalysts to Enhance Polyurethane Synthesis and Reprocessing

Carbamate formation and exchange catalysts enable efficient polyurethane (PU) manufacturing, as well as emerging recycling and reprocessing methods for PU thermosets. Zirconium β-diketonate complexes, such as Zr acetylacetonate [Zr(acac) 4 ], are effective alternatives to toxic organotin catalysts that have been used for PU reprocessing. Here, we report that Zr(acac) 4 undergoes a thermally activated process in the PU network during reprocessing that transforms it into a more active carbamate exchange catalyst. This process is associated with the irreversible loss of acetylacetonate ligands and is not observed for the more sterically hindered Zr 2,2,6,6-tetramethyl-3,5-heptanedione [Zr(tmhd) 4 ] complex. Crossover experiments between PU thermoplastics indicated enhanced carbamate exchange after the thermal activation of Zr(acac) 4 in the presence of one of the PUs, whereas a sample of Zr(acac) 4 activated in the absence of the PU had no catalytic activity. Thermal gravimetric analysis suggested that this process is associated with the loss of one protonated acac ligand. Stress relaxation analysis of PU thermosets indicated a distinct change in the characteristic relaxation time associated with the thermal activation of Zr(acac) 4 at temperatures above 140 °C; no such change was observed for samples reprocessed using Zr(tmhd) 4 . Density functional theory and molecular experiments suggest that irreversible ligand exchange of acac with alkoxide or carbamate reduces the activation energy for urethane formation and reversion. Furthermore, the Zr(acac) 4 catalyst activated in the presence of a PU’s polyol precursor provided more porous and less dense PU foams compared to those made using the unactivated Zr(acac) 4 catalyst. Furthermore, these findings are important for developing improved PU synthesis and recycling processes. Thermally activating a catalyst during reprocessing may provide more nuanced control of the in-use and reprocessing characteristics of PU thermosets.

Alcohols↗
DOE OSTI2021

Light-Mediated Synthesis and Reprocessing of Dynamic Bottlebrush Elastomers under Ambient Conditions

We introduce a novel grafting-through polymerization strategy to synthesize dynamic bottlebrush polymers and elastomers in one step using light to construct a disulfide-containing backbone. The key starting material—α-lipoic acid (LA)—is commercially available, inexpensive, and biocompatible. When installed on the chain end(s) of poly(dimethylsiloxane) (PDMS), the cyclic disulfide unit derived from LA polymerizes under ultraviolet (UV) light in ambient conditions. Significantly, no additives such as initiator, solvent, or catalyst are required for efficient gelation. Formulations that include bis-LA-functionalized cross-linker yield bottlebrush elastomers with high gel fractions (83–98%) and tunable, supersoft shear moduli in the ~20–200 kPa range. An added advantage of these materials is the dynamic disulfide bonds along each bottlebrush backbone, which allow for light-mediated self-healing and on-demand chemical degradation. These results highlight the potential of simple and scalable synthetic routes to generate unique bottlebrush polymers and elastomers based on PDMS.

36 MATERIALS SCIENCE↗
NASA NTRS2018

TRMM Version 8 Reprocessing Improvements and Incorporation into the GPM Data Suite

The National Aeronautics and Space Administration (NASA) has always included data reprocessing as a major component of every science mission. A final reprocessing is typically a part of mission closeout (known as phase F).The Tropical Rainfall Measuring Mission (TRMM) is currently in phase F, and NASA is preparing for the last reprocessing of all the TRMM precipitation data as part of the closeout. This reprocessing includes improvements in calibration of both the TRMM Microwave Imager (TMI) and the TRMM Precipitation Radar (PR). An initial step in the version 8 reprocessing is the improvement of geolocation. The PR calibration is being updated by the Japan Aerospace Exploration Agency (JAXA) using data collected as part of the calibration of the Dual-Frequency Precipitation Radar (DPR) on the Global Precipitation Measurement (GPM) Core Observatory. JAXA undertook a major effort to ensure TRMM PR and GPM Ku-band calibration is consistent. A major component of the TRMM version 8 reprocessing is to create consistent retrievals with the GPM version 05 (V05) retrievals. To this end, the TRMM version 8 reprocessing uses retrieval algorithms based on the GPM V05 algorithms. This approach ensures consistent retrievals from December 1997 (the beginning of TRMM) through the current ongoing GPM retrievals. An outcome of this reprocessing is the incorporation of TRMM data products into the GPM data suite. Incorporation also means that GPM file naming conventions and reprocessed TRMM data carry the V05 data product version. This paper describes the TRMM version 8 reprocessing, focusing on the improvements in TMI level 1 products.

Stocker, E. F.↗
DOE OSTI2026

Recyclability of reversible polymer networks over a Dozen reprocessing cycles

Reversible polymer networks capable of reversible reactions along their backbone provide a promising strategy for addressing waste management challenges associated with conventional thermoset products. However, reversible polymer networks cannot be recycled infinitely. Unavoidable side reactions eventually cause significant degradation of mechanical properties or loss of recyclability. This study aims to answer a simple yet critical question on reversible polymer network systems: how many reprocessing cycles can be achieved before profound mechanical degradation or a loss of recyclability? The recyclability of Diels–Alder (DA) network samples was evaluated by repeating consistent reprocessing cycles until they were no longer reprocessable. To enhance their recyclability, the chemical structure of the maleimide precursor was tailored to mitigating side reactions by maleimide homopolymerization. Remarkably, by employing a maleimide precursor with alkyl substitutions on its phenyl group, the DA network system attained 12 reprocessing cycles using injection molding at 160 °C without significant degradation of mechanical properties. However, the 13th reprocessing cycle did not succeed. Rheological analysis revealed the accumulation of non-reversible bonds within the network structure during repeated reprocessing, despite fairly consistent mechanical properties under operating conditions. This study demonstrates that the rational design of the maleimide precursor is an effective means to enhance the reprocessability of DA networks.

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

Nuclear Fuels and Reprocessing Technologies: A U.S. Perspective

Reprocessing and/or waste management issues are of concern to the “back end” of the nuclear fuel cycle. Of course, there are a great many “nuclear fuel cycle” scenarios to consider; if not in practice, then at least in theory. The simplest conceptually is the “once through” fuel cycle in which the spent fuel is discarded. The more complex fuel cycle scenarios involve reprocessing spent nuclear fuels and a family of nuclear reactor technologies to accommodate burning and breeding for various military and commercial needs. Therefore, the selection of a specific “fuel cycle” is what ultimately imposes the engineering requirements of the reprocessing and waste management technologies. No one part is independent of the other parts in a fuel cycle flowsheet; all parts are fully integrated. This paper presents a summary of radiochemical processes, nuclear reactor technologies, nuclear fuel types, and the reprocessing technologies that serve the different nuclear fuel types. Comprehending how this series of topics are related to each other is a prerequisite to understanding the requirements of any reprocessing strategy. The summary materials presented here are selective, as opposed to comprehensive. More detailed information on any one subject can be found in the reference materials.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

Green Catalysts for Reprocessing Thermoset Polyurethanes

Polyurethane (PU) thermosets are usually landfilled at the end of their service lifetimes and cannot be recycled through conventional means. Although dibutyltin dilaurate (DBTDL) is an effective catalyst for reprocessing PU thermosets, organotins are immunotoxic and teratogenic, which is concerning for catalysts embedded within covalent adaptable networks (CANs). Here, we identify Zr(acac) 4 and Zr(tmhd) 4 as catalysts to reprocess PU CANs more sustainably. Thermoset PU foams containing Zr-based catalysts exhibit characteristic stress relaxation times between 6 and 200 s, similar or faster than DBTDL. These catalysts are capable of reprocessing a PU foam for four or five cycles. Dynamic mechanical thermal analysis indicates that zirconium-based catalysts preserve glass transition temperature and crosslink density between cycles and are promising catalysts for bulk reprocessing of thermoset PUs. Here, a solvent-free reprocessing method was developed by co-milling the PU foam and the Zr catalyst. Ultimately, these reprocessing methods using Zr-based catalysts will impart greater sustainability and circularity to PU plastics.

Catalysts↗
DOE OSTI2023

Reprocessing Models for the Optical Light Curves of Hypervariable Quasars from the Sloan Digital Sky Survey Reverberation Mapping Project

We explore reprocessing models for a sample of 17 hypervariable quasars, taken from the Sloan Digital Sky Survey Reverberation Mapping project, which all show coordinated optical luminosity hypervariability with amplitudes of factors ≳2 between 2014 and 2020. We develop and apply reprocessing models for quasar light curves in simple geometries that are likely to be representative of quasar inner environments. In addition to the commonly investigated thin-disk model, we include the thick-disk and hemisphere geometries. The thick-disk geometry could, for instance, represent a magnetically elevated disk, whereas the hemisphere model can be interpreted as a first-order approximation for any optically thick out-of-plane material caused by outflows/winds, warped/tilted disks, and so on. Of the 17 quasars in our sample, 11 are best-fitted by a hemisphere geometry, five are classified as thick disks, and both models fail for just one object. We highlight the successes and shortcomings of our thermal reprocessing models in case studies of four quasars that are representative of the sample. While reprocessing is unlikely to explain all of the variability that we observe in quasars, we present our classification scheme as a starting point for revealing the likely geometries of reprocessing for quasars in our sample and hypervariable quasars in general.

79 ASTRONOMY AND ASTROPHYSICS↗
NASA NTRS1999

Reprocessing in Luminous Disks

We develop and investigate a procedure that accounts for disk reprocessing of photons that originate in the disk itself. Surface temperatures and simple, black body spectral energy distributions (SEDs) of protostellar disks are calculated. In disks that flare with radius, reprocessing of stellar photons results in temperature profiles considerably shallower than r(sup -3/4). Including the disk as a radiation source (as in the case of actively secreting disks) along with the stellar source further flattens the temperature profile. Disks that flare strongly near the star and then smoothly curve over and become shadowed at some distance ("decreasing curvature" disks) exhibit nearly power-law temperature profiles which result in power-law infrared SEDs with slopes in agreement with typical observations of young stellar objects. Disk models in which the photospheric thickness is controlled by the local opacity and in which the temperature decreases with radius naturally show this shape. Uniformly flaring models do not match observations as well; progressively stronger reprocessing at larger radii leads to SEDs that flatten toward the infrared or even have a second peak at the wavelength corresponding (through the Wien law) to the temperature of the outer edge of the disk. In FU Orionis outbursting systems, the dominant source of energy is the disk itself. The details of the reprocessing depend sensitively on the assumed disk shape and emitted temperature profile. The thermal instability outburst models of Bell Lin reproduce trends in the observed SEDs of Fuors with T varies as r(sup -3/4) in the inner disk (r approx. less than 0.25au corresponding to lambda approx. less than 10 microns) and T varies as r(sup -1/2) in the outer disk. Surface irradiation during outburst and quiescence is compared in the region of planet formation (1 - 10 au). The contrast between the two phases is diminished by the importance of the reprocessing of photons from the relatively high mass flux outer disk (dot-M = 10(exp -5) solar mass/yr) which is present during both outburst and quiescence.

Bell, K. Robbins↗
NASA NTRS2003

Algorithm Updates for the Fourth SeaWiFS Data Reprocessing

The efforts to improve the data quality for the Sea-viewing Wide Field-of-view Sensor (SeaWiFS) data products have continued, following the third reprocessing of the global data set in May 2000. Analyses have been ongoing to address all aspects of the processing algorithms, particularly the calibration methodologies, atmospheric correction, and data flagging and masking. All proposed changes were subjected to rigorous testing, evaluation and validation. The results of these activities culminated in the fourth reprocessing, which was completed in July 2002. The algorithm changes, which were implemented for this reprocessing, are described in the chapters of this volume. Chapter 1 presents an overview of the activities leading up to the fourth reprocessing, and summarizes the effects of the changes. Chapter 2 describes the modifications to the on-orbit calibration, specifically the focal plane temperature correction and the temporal dependence. Chapter 3 describes the changes to the vicarious calibration, including the stray light correction to the Marine Optical Buoy (MOBY) data and improved data screening procedures. Chapter 4 describes improvements to the near-infrared (NIR) band correction algorithm. Chapter 5 describes changes to the atmospheric correction and the oceanic property retrieval algorithms, including out-of-band corrections, NIR noise reduction, and handling of unusual conditions. Chapter 6 describes various changes to the flags and masks, to increase the number of valid retrievals, improve the detection of the flag conditions, and add new flags. Chapter 7 describes modifications to the level-la and level-3 algorithms, to improve the navigation accuracy, correct certain types of spacecraft time anomalies, and correct a binning logic error. Chapter 8 describes the algorithm used to generate the SeaWiFS photosynthetically available radiation (PAR) product. Chapter 9 describes a coupled ocean-atmosphere model, which is used in one of the changes described in Chapter 4. Finally, Chapter 10 describes a comparison of results from the third and fourth reprocessings along the US. Northeast coast.

Hooker, Stanford, B.↗
NASA NTRS2017

First Reprocessing of Southern Hemisphere ADditional OZonesondes (SHADOZ) Profile Records (1998-2015): 1. Methodology and Evaluation

Electrochemical concentration cell ozonesonde measurements are an important source of highly resolved vertical profiles of ozone with long-term data records for deriving ozone trends, model development, satellite validation, and air quality studies. Ozonesonde stations employ a range of operational and data processing procedures, metadata reporting, and instrument changes that have resulted in inhomogeneities within individual station data records. A major milestone is the first reprocessing of seven Southern Hemisphere ADditional OZonesondes (SHADOZ) station ozonesonde records to account for errors and biases in operating/processing procedures. Ascension Island, Hanoi, Irene, Kuala Lumpur, La Reunion, Natal, and Watukosek station records all show an overall increase in ozone after reprocessing. Watukosek shows the largest increase of 9.0 plus or minus 2.1 Dobson Units (DU) in total column ozone; Irene and Hanoi show a 5.5 plus or minus 2.5 DU increase, while remaining sites show statistically insignificant enhancements. Negligible to modest ozone enhancements are observed after reprocessing in the troposphere (up to 8%) and stratosphere (up to 6%), except at La Reunion for which the application of background currents reduces tropospheric ozone (2.1 plus or minus1.3 DU). Inhomogeneities due to ozonesonde/solution-type changes at Ascension, Natal, and La Reunion are resolved with the application of transfer functions. Comparisons with EP-TOMS, Aura's Ozone Monitoring Instrument and Microwave Limb Sounder (MLS) satellite ozone overpasses show an overall improvement in agreement after reprocessing. Most reprocessed data sets show a significant reduction in biases with MLS at the ozone maximum region (50-10 hPa). Changes in radiosonde/ozonesonde system and nonstandard solution types can account for remaining discrepancies observed at several sites when compared to satellites.

Electrochemical concentration cell ozonesonde meas↗
NASA NTRS2020

TESS Data Release Notes:Reprocessing of Sectors 14–19, DR30 & DR33

TESS data release 30 (DR30) provides reprocessed data products of Sector 14 to 19. The updated data products were generated using version 4.0 of the science processing pipeline and conform to the final set of data anomaly flags defined over the last two years of TESS data analysis and pipeline development. Data release 33 (DR33) corresponds to a multisector search for transiting planets in the same reprocessed data. A detailed description of the changes in the data products in DR30 and DR33 is discussed in§2, and a brief list of changes is summarized here: The timestamps for 2 minute cadence and FFI data are more accurate. The differences between reprocessed data and previous data releases are less than 2.0 seconds in all cases. Photometric apertures were increased in size for targets with T mag<11. Three new Data Anomaly Flags were added to mitigate the effects of scattered light:–Cadences with strong scattered light signals or saturation effects that corrupt the calibration data are flagged and removed from analysis (bit 15, value 16384, “Bad Calibration Exclude”).–Scattered light data anomaly flags are customized for each target, and flagged automatically based on the local background level (bit 13, value 4096, ”Scattered light flag”).–Cadences with insufficient targets to derive cotrending basis vectors are flagged and the PDCSAP FLUX light curves are set to NULL at these times (bit 16, value 32768, “Insufficient Targets for Error Correction Exclude”). The planet search of the reprocessed light curves produced a different set of TCEs from the original processed data. Although there is a high degree of overlap between the original and reprocessed data (∼83% of targets produced TCEs in common), new TCEs were produced in DR30 and not every TCE from previous data releases was recovered. The same is true of the multisector search results from DR33 compared to DR28

TESS'↗
DOE OSTI2023

Circular Reprocessing of Thermoset Polyurethane Foams

Thermoset polyurethane (PU) foams are widely used in industrial applications, but they cannot be recycled by conventional melt reprocessing because of their cross-linked structures. The introduction of carbamate exchange catalysts converts thermoset PU into covalent adaptable networks (CANs), which are amenable to reprocessing at elevated temperatures. However, this approach has produced solid PU films, which have fewer uses and lower commercial demand. In this work, simultaneous reprocessing and refoaming of thermoset PU foams is demonstrated by leveraging the melt-processability of PU CANs and allowing cell growth by gas generation in a twin-screw extruder. The optimal operating temperature of the refoaming process is determined through chemical, thermal, and structural analysis of PU foam extrudates. The foam-to-foam extrusion process produces controllable, continuous, and uniform foam structures, as characterized by cell diameter and cell number density. Low-density PU foams are obtained through a process simulating injection molding. The compression properties of reprocessed PU foam are compared with as-synthesized PU foam to demonstrate efficacy of the refoaming processes. These results demonstrate that PU foams can be prepared through recycling while maintaining microstructural and chemical integrity. In the future, this strategy may be applied to thermoset PU foams of various chemical compositions and shows promise for scalability.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Dioctyl ether radiolysis under used nuclear fuel reprocessing conditions: Foundational knowledge for the development of sacrificial ligand grafts

Radiation-induced ligand destruction and concomitant degradation product formation is unavoidable under envisioned used nuclear fuel reprocessing conditions, and ultimately limits the recyclability of a given solvent system formulation. With this in mind, a novel approach to ligand innovation for advanced separations processes is in the design of tailored “protomolecules,” which when exposed to ionizing radiation undergo desired chemical transformations, thereby allowing for a reprocessing solvent system to advantageously evolve with absorbed radiation dose. Here we provide foundational knowledge for the time-resolved (electron pulse) and steady-state (cobalt-60 gamma) radiolytic behavior of dioctyl ether, a protomolecule grafting surrogate. Gamma irradiation of single-phase solutions of dioctyl ether (5–100 vol.%) in n-dodecane resulted in the loss of dioctyl ether (G = -0.72 µmol J –1 ) and the formation of octane (G = 0.11 µmol J –1 ) and octanol (G = 0.15 µmol J –1 ) degradation products, the latter of which is a known reprocessing phase modifier and radioprotectant. Further, these radiation-induced changes were attributed to direct radiation effects, for more concentrated dioctyl ether solutions, and indirect radiation effects, predominantly driven by the reaction of dioctyl ether with the dodecane radical cation, for which we report a second-order rate coefficient of k = (1.53 ± 0.05) × 10 10 L mol –1 s –1 . Under typical biphasic extraction (4.0 mol L –1 HNO 3 ) and strip (0.1 mol L –1 HNO 3 ) reprocessing conditions, gamma irradiation of 5 vol.% dioctyl ether solvent systems afforded negligible change in the rate of parent molecule destruction but promoted significant differences in the radiolytic behavior of its degradation products. These differences are attributed to their respective interactions with [dioctyl ether/HNO 3 /H 2 O] and [octanol/HNO 3 /H 2 O] adducts extracted into the organic phase. Overall, these results support the grafting of ether linkages to advanced separations ligands (e.g., modified diglycolamides).

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2023

Cost-Benefit Assessment of Krypton and Xenon Recovery from Aqueous Reprocessing

The purpose of this paper is to provide an understanding of the cost-benefit of capturing Kr and Xe from the existing process of aqueous reprocessing of UNF. The study accomplishes this with a market assessment of Xe prices and volumes today, coupled with a cost estimate of Kr and Xe capture out of cryogenic distillation within aqueous reprocessing. The market assessment shows that the average price of Xe is about $\$ $60/L while the average price of Kr is about $\$ $1/L. The assessment also shows that the market structure for Xe is one of oligopoly, in other words, very few suppliers to the Xe market. The assessment shows growing demand for Xe, particularly in medical applications like anesthesia. The cost assessment finds the unit cost of Xe to range from $\$ $71.50/L to $\$ $131.13/L. This range is only slightly above the current range of market prices today, and with growing demand for Xe, prices could reach the range it would take to support extraction of Xe from aqueous reprocessing. On the other hand, the estimated cost range for Kr is $\$ $830.15/L up to $\$ $1,522.52/L, which far exceeds the range of market prices for Kr. However, as the text notes, Kr capture is already part of aqueous reprocessing so these costs are sunk costs (already incurred) whereas the cost estimates for Xe are marginal cost (if Xe is desired, then the cost estimate would result from the Xe capture).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

Reprocessable polyhydroxyurethane networks reinforced with reactive polyhedral oligomeric silsesquioxanes (POSS) and exhibiting excellent elevated temperature creep resistance

The rapid development of covalent adaptable networks or vitrimers shows promise for addressing the long-standing recycling issues associated with conventional, permanently cross-linked thermosets. At the same time, it is important to demonstrate that properties of reprocessable polymer networks can be optimized to meet the ongoing demand for high-performance materials. We have fabricated reprocessable polyhydroxyurethane (PHU) network composites reinforced with reactive polyhedral oligomeric silsesquioxanes (POSS). With functionalized POSS serving as a fraction of the cross-linkers, the PHU–POSS network nanocomposites exhibit significantly enhanced storage modulus at the rubbery plateau region relative to the neat PHU network. With up to 10 wt% POSS loading, these network composites can undergo melt-state reprocessing at 140 °C with 100% property recovery associated with cross-link density. We also show that hydroxyurethane dynamic chemistry leads to excellent creep resistance at elevated temperature up to 90 °C and is unaffected by reactive incorporation of POSS. In conclusion, this study demonstrates the effectiveness of POSS as nanofillers for designing high-performance, organic-inorganic dynamic PHU networks with excellent reprocessability.

42 ENGINEERING↗