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DOE OSTI2014

The Primary and Recycling Sources of OH During the NACHTT-2011 Campaign: HONO as an Important OH Primary Source in the Wintertime

We present OH observation results during the NACHTT-11 field campaign at the Boulder Atmospheric Observatory in Weld County, Colorado. The observed OH levels during the daytime (at noon) were ~ 2.7 × 106 molecules cm-3 at the ground level (2 m above ground level, AGL). HONO and ozone photolysis were the two dominant photochemical OH production pathways during the field campaign. However, alkene ozonolysis, found an important source for OH by two previous winter season OH observations, was a minor contribution to OH primary production (~5 %). To evaluate recycling sources of OH from HO2 and RO2, an observation constrained University of Washington Chemical Mechanism (UWCM) box model is employed to simulated ambient OH levels with different model scenarios. For the base run without constraining observed HONO, the model simulated OH significantly underestimates the observed OH level (20.8 times in the morning and 7.2 times in the daytime). This indicates that the known HONO sources incorporated in the UWCM model cannot explain the observed HONO level. Once HONO is constrained by the observation, the discrepancy between observation and model simulation improves (5.1 times in the morning and 2.1 times in the daytime) but still out of the measurement uncertainty range (35 %). We explore two possible reasons for the observed unexplainably high wintertime OH levels. First, potential roles of Cl atoms produce organic peroxy radicals from the reactions between Cl atmos and alkane compounds. However, the Cl levels during the observation period are estimated very low (~ 103 atoms cm-3) to explain the enhanced OH levels. Second, Impacts of higher HONO levels on the ground was evaluated. Strong HONO gradient towards ground was observed especially during the early morning (6 am to 8 am) was observed and the lowest level available for the HONO observation during the campaign is 5 m AGL. Once we assume the twice of the observed HONO levels averaged between 5 m to 15 m at 2 m AGL, model predicted OH levels agree well within the observation uncertainty range. Wintertime photochemistry has not been investigated as much as the summer season. The results of this study along with a limited number of winter OH observations clearly urge further investigation on tropospheric oxidation capacity in the winter season considering implications of tropospheric oxidation capacity to the short-lived climate forcers especially methane.

Kim, S.↗

DOE OSTI2014

Reactions Between Water Soluble Organic Acids and Nitrates in Atmospheric Aerosols: Recycling of Nitric Acid and Formation of Organic Salts

Atmospheric particles often include a complex mixture of nitrate and secondary organic materials accumulated within the same individual particles. Nitrate as an important inorganic component can be chemically formed in the atmosphere. For instance, formation of sodium nitrate (NaNO3) and calcium nitrate Ca(NO3)2 when nitrogen oxide and nitric acid (HNO3) species react with sea salt and calcite, respectively. Organic acids contribute a significant fraction of photochemically formed secondary organics that can condense on the preexisting nitrate-containing particles. Here, we present a systematic microanalysis study on chemical composition of laboratory generated particles composed of water soluble organic acids and nitrates (i.e. NaNO3 and Ca(NO3)2) investigated using computer controlled scanning electron microscopy with energy dispersive analysis of X-rays (CCSEM/EDX) and Fourier transform infrared micro-spectroscopy (micro-FTIR). The results show that water-soluble organic acids can react with nitrates releasing gaseous HNO3 during dehydration process. These reactions are attributed to acid displacement of nitrate with weak organic acids driven by the evaporation of HNO3 into gas phase due to its relatively high volatility. The reactions result in significant nitrate depletion and formation of organic salts in mixed organic acids/nitrate particles that in turn may affect their physical and chemical properties relevant to atmospheric environment and climate. Airborne nitrate concentrations are estimated by thermodynamic calculations corresponding to various nitrate depletions in selected organic acids of atmospheric relevance. The results indicate a potential mechanism of HNO3 recycling, which may further affect concentrations of gas- and aerosol-phase species in the atmosphere and the heterogeneous reaction chemistry between them.

Aerosols↗

DOE OSTI2024

Redesigned Nylon 6 Variants with Enhanced Recyclability, Ductility, and Transparency

Abstract Geminal ( gem −) disubstitution in heterocyclic monomers is an effective strategy to enhance polymer chemical recyclability by lowering their ceiling temperatures. However, the effects of specific substitution patterns on the monomer's reactivity and the resulting polymer's properties are largely unexplored. Here we show that, by systematically installing gem ‐dimethyl groups onto ϵ‐caprolactam (monomer of nylon 6) from the α to ϵ positions, both the redesigned lactam monomer's reactivity and the resulting gem ‐nylon 6’s properties are highly sensitive to the substitution position, with the monomers ranging from non‐polymerizable to polymerizable and the gem ‐nylon properties ranging from inferior to far superior to the parent nylon 6. Remarkably, the nylon 6 with the gem ‐dimethyls substituted at the γ position is amorphous and optically transparent, with a higher T g (by 30 °C), yield stress (by 1.5 MPa), ductility (by 3×), and lower depolymerization temperature (by 60 °C) than conventional nylon 6.

Tian, Jun‐Jie↗

DOE OSTI2015

Structural evolution of recycled tire rubber in asphalt

ABSTRACT The performance of recycled‐tire‐rubber‐modified asphalt mainly depends on the structure of rubber in the asphalt. The effects of the curing temperature, mixing time, and shearing on the evolution of the chemical structure and morphological structure of crumb rubber in asphalt were investigated. The crosslink density, compositions, and morphological evolution of the residual crumb rubber were characterized. The results show that the structure evolution of tire rubber in asphalt was greatly affected by the curing temperature. At a low curing temperature (180°C), the crosslinking network of the tire rubber was broken down, and this led to the partial dissolution of natural rubber (NR). However, at high curing temperature (240°C), the dissolution of NR, synthetic rubber, carbon black, and inorganic filler was observed. The released carbon black covered with a thin layer of bound rubber dispersed at a microstructured or nanostructured size in the asphalt. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133 , 42954.

Yao, Hongru↗

DOE OSTI2020

Sustainable Direct Recycling of Lithium-Ion Batteries via Solvent Recovery of Electrode Materials

Separation of electrode materials from their current collectors is an enabling step toward recovering critical materials from spent lithium-ion batteries. In this study, a highly efficient, cost-effective, and environmentally sustainable separation process was developed for that purpose. Ethylene glycol, a vital commodity chemical as an antifreeze and polymer precursor, is used to delaminate electrode materials at low temperatures in seconds without altering the crystalline structure and morphology of active electrode materials. The recovered current collectors were intact without any corrosion. The authors also found that the solvent could be continuously reused, leading to the development of a closed-loop ecosystem and lithium-ion battery circular economy. The ultrafast delamination was driven by the competitive inhibition of binding through the weakening of hydrogen bonding. The ethylene glycol-based separation is a sustainable electrode recovery process that paves the way for battery recycling.

25 ENERGY STORAGE↗

DOE OSTI2021

Reducing Antisolvent Use in the STRAP Process by Enabling a Temperature–Controlled Polymer Dissolution and Precipitation for the Recycling of Multilayer Plastic Films

The recently reported processing strategy called solvent-targeted recovery and precipitation (STRAP) enables deconstruction of multilayer plastic packaging films into their constituent resins by selective dissolution. It uses a series of solvent washes that are guided by thermodynamic calculations of polymer solubility. In this work, the use of antisolvents in the STRAP process was reduced and solvent mixtures were considered to enable the temperature-controlled dissolution and precipitation of the target polymers in multilayer films. This was considered as a means to further improve the STRAP process and its estimated costs. Two STRAP approaches were compared based on different polymer precipitation techniques: precipitation by the addition of an antisolvent (STRAP-A) and precipitation by decreasing the solvent temperature (STRAP-B). Both approaches were able to separate the constituent polymers in a post-industrial film composed primarily of polyethylene (PE), ethylene vinyl alcohol (EVOH), and polyethylene terephthalate (PET) with near 100 % material efficiency. Technoeconomic analysis indicates that the minimum selling price (MSP) of the recycled resins with STRAP-B is 21.0 % lower than that achieved with STRAP-A. This provides evidence that thermally driven polymer precipitation is an option to reduce the use of antisolvents, making the STRAP process more economically and environmentally attractive. A third process, STRAP-C, was demonstrated with another post-industrial multilayer film of a different composition. Here, the results demonstrate that this process can also recover polymers at similar costs to those of virgin resins, indicating that the STRAP technology is flexible and can remain economically competitive as the plastic feed complexity is increased.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Kinetic Monte Carlo Tool for Kinetic Modeling of Linear Step-Growth Polymerization: Insight into Recycling of Polyurethanes

A kinetic Monte Carlo model of polyurethane polymerization which explicitly tracks the polymer sequences is developed and shared. Here this model is benchmarked against theoretical and experimental polyurethane data and used to investigate the effect on oligomer distributions of unequal reactivity of the first and second isocyanate to react. The reverse reactions using thermodynamic consistency are then added to the framework, and analogous to the addition polymerization concept of ceiling temperature, equilibrium chain length distributions at various temperatures are calculated. For a mixture of three monomers AA, BB, and CC, where BB and CC do not react with one another, are present in stoichiometric proportions, and have different enthalpies of reaction with AA, an odd-even effect emerges. Odd length chains are more likely than even length chains for temperatures at which BB and CC have significantly different equilibrium conversions. The concept of ceiling temperature that is typically cited for addition polymers is extended here to provide a measure of conditions under which depolymerization for recycling is favored.

condensation polymerization↗

DOE OSTI2024

Phosphorus recycling by mineral-catalyzed ribonucleotide cleavage on iron and manganese oxides

Abstract Phosphorus is an essential element influencing both food security via plant fertilization, and water pollution through excessive phosphorus use, yet the phosphorus cycle in ecosystems is poorly known. In particular, beyond adsorption, the role of iron and manganese oxides in catalyzing the abiotic dephosphorylation of biomolecules is debated. Here, we studied the reactions of ribonucleotides, containing different phosphate bonding, with goethite, hematite, and birnessite. We employed both high-resolution mass spectrometry of solution species and molecular modeling simulations of ribonucleotide-mineral complexes. Results disclose an up to fivefold preferential hydrolytic cleavage of a phosphoanhydride bond over a phosphoester bond, indicating that mineral-catalyzed reactions reflect the hierarchy reported for the activity of phosphatase enzymes. The fourfold higher catalytic reactivity of goethite and birnessite versus hematite is explained by mineral-specific binding rather than surface area differences. Corresponding simulated adsorbate conformations at the water–mineral interfaces are proposed. Overall, our findings provide new insights on the catalytic recycling of organic phosphorus species by mineral oxides.

58 GEOSCIENCES↗

DOE OSTI2018

Modification of Thermo-Mechanical Properties of Recycled PET by Vinyl Acetate (VAc) Monomer Grafting Using Gamma Irradiation

Vinyl acetate (VAc) monomer of different percentage was grafted onto the recycled polyethylene terephthalate (r-PET) films using gamma irradiation. The properties of these modified films were characterized by Fourier transform infrared spectroscopy (FTIR), mechanical properties testing (Tensile strength, Elongation at break), dynamic mechanical analysis (DMA) and thermo-gravimetric analysis (TGA). The Tensile Strength (TS) of the modified PET film increased by 132.25 % to the highest value of 50.12 MPa at 15% VAc monomer concentration at 3 kGy gamma dose, while the elongation at break (EB) decreased by 31.83 %. FTIR was used to investigate the molecular interaction of the modified films. TGA revealed that curve of the modified PET film shifted toward higher temperature region by 95 °C, which is very close to that of PET film made from virgin flakes. The results indicate that modified PET films of better mechanical and thermal properties were successfully prepared using VAc monomer grafting by gamma irradiation technique.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Recycled Poly(Ethylene Terephthalate)/Clay Nanocomposites: Rheology, Thermal and Mechanical Properties

Polymer nanocomposites containing recycled poly(ethylene terephthalate) (r-PET) as a polymer matrix and Cloisite{sup ®} 10A as a reinforcement were prepared through melt compounding. First, a masterbatch containing 20 wt% of Cloisite{sup ®} 10A clay was prepared and later diluted with neat r-PET to obtain nanocomposites containing 1, 2, 4 and 6 wt% of clay. The rheological, thermal, mechanical and morphological properties of the PET–clay nanocomposites were characterized. The complex viscosity of the nanocomposites gradually increases with increase in clay content. The storage modulus and loss modulus of nanocomposite containing 1 wt% of clay was similar to neat r-PET but increases with increase in clay content. Incorporation of clay into a r-PET slightly increases the crystallisation temperature and degree of crystallinity due to the heterogenous nucleating effect of clay. Thermal stability and glass transition temperature of nanocomposite containing Cloisite{sup ®} 10A clay at lower loadings was similar to r-PET and gradually decreases with increase in clay content. The tensile properties of PET–clay nanocomposites increased gradually with clay content. The impact strength of nanocomposites was not altered until 4 wt% and decreased at 6 wt%. Morphological investigations indicated homogeneous dispersion of clay in r-PET.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Preparation of Low-Density Microcellular Foams from Recycled PET Modified by Solid State Polymerization and Chain Extension

Recycled polyethylene-terephthalate (RPET) bottle regrinds were physically foamed after two types of industrially feasible molecular weight increasing processes. Intrinsic viscosity (IV) of initial waste (0.71 dL/g) increased both after reactive extrusion carried out using a multifunctional epoxy-based chain extender (0.74 dL/g) and after solid state polycondensation (SSP) (0.78 dL/g), while capillary rheometry revealed higher degree of branching in the chain extended PET material. Despite the relatively low IV values (below 0.80 dL/g), physical foaming, a mild and cost-efficient way, was successful in both cases, uniform microcellular foam structures with void fractions ranging between 75 and 83% were achieved. During the experiments morphology change in the materials was tracked by differential scanning calorimetry (DSC) besides recording IV values. The IV drop during foaming was between 0.03 and 0.10 depending on the pre-processing technology. Structure of foams produced from the two different modified RPET materials was compared with each other based on scanning electron microscopic imaging of cryogenic fracture surfaces. The average cell diameters were measured to be 213 and 360 µm in the case of chain extended and SSP-modified materials, respectively.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Effect of Natural and Accelerated Aging on the Mechanical Performance of a Composite Based on Recycled Multilayer Carton

A composite elaborated from waste material was studied for its proposed use as a wood plastic composite. Multilayer food cartons and recycled high density polyethylene were used for the elaboration of laminates, in a proportion of 55% and 45% volume fraction, respectively. The samples were subjected to an aging in an accelerated weathering (AW) chamber for 0, 500, 1000 and 2000 h with UVB radiation, temperature and humidity cycles. Samples exposed to natural weathering (NW) for 0, 1300, 2600 and 5200 h, in a warm sub-humid environment were also studied, the aim being to elucidate a correlation of the useful lifespan of the material. In both cases, after the exposure, three-point bend tests were performed to evaluate the effect on the mechanical properties. The analysis of the degradation process was carried out by infrared spectroscopy, indicating that the AW and NW samples showed deterioration of the material in different proportions. By mean of thermal analysis, it was possible to associate the degradation with the appearance and/or growth of the endothermic peaks, showing a variation in the melting temperature as the time of exposure to AW and NW increased, resulting in a change in the crystallinity percentage. The modulus of rupture (MOR) and the flexural modulus of elasticity decreased by 20% in samples subjected to AW for 2000 h; while in the samples exposed to NW, required of 5200 h to obtain a reduction of 16% in the MOR.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Recyclability study on Inconel 718 and Ti-6Al-4V powders for use in electron beam melting

In this study, powder bed based additive manufacturing technologies offer a big advantage in terms of reusability of the powders over multiple cycles that result in cost savings. However, currently there are no standards to determine the factors that govern the powder reuse times. This work presents the results from a recyclability study conducted on Inconel 718 and Ti-6Al-4V powders. It has been found that the Inconel 718 powders are chemically stable over a large number of cycles and their reuse time is limited by physical characteristics of powders such as flowability. Ti-6Al-4V, on the other hand, finds its reuse time governed by the oxygen pick up that occurs during and in between build cycles. The detailed results have been presented.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Criticality concerns of a group actinide co-crystallization separations approach to used nuclear fuel recycling

We report the co-crystallization of hexavalent actinides with uranyl nitrate hexahydrate has been established as a viable approach to achieving group actinide separation in used nuclear fuel recycle while avoiding the difficulties associated with the solvent-extraction process altogether. A preliminary neutronics safety analysis has been performed to alleviate criticality concerns associated with this group hexavalent actinide co-crystallization approach. The basic uranyl nitrate hexahydrate material compositions used are representative of used fuel found at commercial pressurized water reactors all around the U.S. This material is subsequently doped with various percentages of either typical reactor grade plutonium or with the total transuranic vector, replacing the uranium atoms in the crystal lattice structure. Infinite and effective neutron multiplication factors were calculated using the state-of-the-art Monte Carlo neutron transport code MCNP in a variety of plausible material configurations, assuming an acceptable safety limit for criticality to be an effective neutron multiplication factor less than 0.95. The results indicate that the crystal structures form a very subcritical intrinsic geometry even with six water molecules being incorporated into the crystal structure. In conclusion, the results of this research suggest that significant opportunity exists for the safe transfer of the group actinide separation approach from a laboratory to an operational scale.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2017

Economic analysis of drying microalgae Chlorella in a conveyor belt dryer with recycled heat from a power plant

Here, the objective of this research is to estimate the cost of drying microalgae chlorella in a conveyor belt dryer using waste heat from an industrial source. The recycling system consists of a run around thermal fluid between two tube heat exchangers. The dryer is mathematically modeled and the mass transport coefficient is obtained from empirical thin-layer kinetic data.The dryer and heat recovery system are designed for the production of 1000 kg/h dried microalgae at a moisture content of 10% (wet basis, w.b.). The input moisture content can range from 35 to 75% (wet basis). Depending upon the applied Hand factor, the total cost to dry microalgae from 55% to 10% ranges from 46.13 to 109.64 per ton of dried product. Using natural gas assumed at 6.27/GJ, the drying cost increases to 83.47 per ton (using hand factor equal to 1). The drying cost using a commercial spray dryer is 109.05 per ton of dried product (using hand factor equal to 1). The paper discusses the sensitivity of drying costs to initial moisture content as well. The results show that integrating waste heat recovery with conveyor belt dryer decreases the drying costs of chlorella drying in comparison to two other drying methods.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2018

Microbial electrolysis using aqueous fractions derived from Tail-Gas Recycle Pyrolysis of willow and guayule

Here, this study investigated microbial electrolysis of two aqueous phase waste products derived from guayule and willow generated from Tail Gas Recycle Pyrolysis (TGRP). The highest average current density achieved was 5.0 ± 0.7 A/m 2 and 1.8 ± 0.2 A/m 2 for willow and guayule respectively. Average hydrogen productivity was 5.0 ± 1.0 L/L-day from willow and 1.5 ± 0.2 L/L-day for guayule. Willow also generated higher coulombic efficiency, anode conversion efficiency, and hydrogen recovery than guayule at most organic loading conditions. Compounds investigated exceeded 80% degradation, which included organic acids, sugar derivatives, and phenolics. Mass spectrometric analysis demonstrated the accumulation of a long chain amine not present in either substrate before treatment, and the persistence of several peptide residues resulting from the TGRP process. Lastly, new biorefineries may one day capitalize on this otherwise discarded byproduct of TGRP, further improving the potential applications and value of microbial electrolysis towards energy production.

09 BIOMASS FUELS↗

DOE OSTI2026

Insights into mixing of non-isothermal multi-polymer melts for complex plastics recycling

Catalytic recycling or upcycling of plastics is often limited not by catalyst performance, but by transport, arising from highly viscous, non-Newtonian polymer melts. In this work, we develop a reactor-scale framework that integrates rheological measurements, constitutive modeling, computational fluid dynamics (CFD), and experiments to quantify mixing, heat transfer, and dispersion in surrogate hydrocarbon melts representing mixed plastics systems. Temperature- and shear rate-dependent viscosity of low-density polyethylene (LDPE) and high-density polyethylene (HDPE) is measured to create two surrogate polymers (PLD and PHD) that capture the dominant shear-thinning flow behavior while neglecting strong elastic effects, enabling tractable simulation of non-isothermal, polymer-melt mixing using a Carreau-Arrhenius generalized Newtonian framework. Three-dimensional CFD simulations are employed to evaluate impeller performance in PLD using mixing time, cavern volume, thermal uniformity, and interfacial area for regimes in which viscoelastic effects are not dominant. We show that magnetic stir bars commonly used in lab-scale studies produce large thermal gradients (~60 °C) and poor mixing, even under idealized power delivery and polymer flow conditions. In contrast, close-clearance anchor impellers achieve near-isothermal operation, reduce mixing times by up to 5×, and provide >90% active circulation volume. We further demonstrate that, at low pseudo-Deborah number (De*), motor power requirements can be predicted directly from shear rate-dependent rheology using the Carreau-Arrhenius framework, enabling rational selection of operating conditions. Extension to surrogate immiscible multi-polymer systems based on PLD and PHD shows that interfacial area is highly sensitive to operating conditions and impeller design, with coaxial anchor-turbine configurations enhancing dispersion by up to 4 × .

Close-clearance impellers↗

DOE OSTI2011

The effect of recycled concrete aggregate properties on the bond strength between RCA concrete and steel reinforcement

The purpose of this study was to investigate the influence that replacing natural coarse aggregate with recycled concrete aggregate (RCA) has on concrete bond strength with reinforcing steel. Two sources of RCA were used along with one natural aggregate source. Numerous aggregate properties were measured for all aggregate sources. Two types of concrete mixture proportions were developed replacing 100% of the natural aggregate with RCA. The first type maintained the same water-cement ratios while the second type was designed to achieve the same compressive strengths. Beam-end specimens were tested to determine the relative bond strength of RCA and natural aggregate concrete. On average, natural aggregate concrete specimens had bond strengths that were 9 to 19% higher than the equivalent RCA specimens. Bond strength and the aggregate crushing value seemed to correlate well for all concrete types.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗