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At least 181 records · Page 10
All sourcesNASA NTRSDOE OSTI
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 OSTI2024

Renewable and Biodegradable Polyurethane Foams with Aliphatic Diisocyanates

The transition to renewable plastics will require the development of substitutes with existing industrial standards and manufacturing processes. Polyurethanes (PU), versatile plastics, are traditionally dominated by aromatic diisocyanates, which are challenging to derive from renewable sources. However, for higher biocontent, it is crucial to utilize aliphatic diisocyanates, which can be sourced from renewable plant or algae waste streams. Historically, PU foams relied on aromatic diisocyanates for essential hard segments, resulting in desired physical properties. Here, we report the generation of high-performance renewable and biodegradable PU foams utilizing aliphatic diisocyanates and aromatic polyols, translating hard segments into the polyester polyol component using biosourced furan dicarboxylic acid (FDCA) monomers. We demonstrate that an FDCA-based PU is suitable for foams with performance characteristics that meet commercial tolerances and can biodegrade under backyard compost conditions. Here, this demonstrates steps toward redesigning traditional petrochemical-based polymers to accommodate new biological monomers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Synthesis, Properties, and Metathesis Activity of Polyurethane Thermoplastics and Thermosets from a Renewable Polysesquiterpene Diol

Polyurethanes (PUs) are the sixth most commonly utilized plastic class, yet ∼80% of commodity material is landfilled or incinerated at the end of life. Disposal of thermosets is particularly problematic as cross-linking prevents the repurposing of disposed material. Thus, there is considerable interest in the development of PUs derived from inexpensive feedstocks that can be inherently chemically deconstructed. Ring opening metathesis polymerization (ROMP) of the naturally occurring sesquiterpene β-caryophyllene in the presence of dihydroxy chain terminators afforded the polyol hydroxy-terminated polycaryophyllene (HTPCR). Incorporation of HTPCR into PUs through reaction with polyisocyanates produced polymers with thermal and rheological properties comparable to commodity materials. The feasibility of chemical degradation of both thermoplastic and thermoset materials was also demonstrated through ruthenium-mediated metathesis, utilizing the metathesis-active olefins within the repeat caryophyllene monomer unit. Overall, this work highlights the value of biorenewable, chemically reprocessable polysesquiterpenes in the PU space.

materials↗
DOE OSTI2024

Shelf-Stable Bingham Plastic Polyurethane Thermosets for Additive Manufacturing

Here, this study presents an innovative 3D-printing method for fabricating hybrid-hardness polyurethane (PU) thermosets via direct-ink writing (DIW). This method features an unprecedentedly long pot-life of at least 16 months for uncured material, achieved by employing internally-blocked polymeric uredines as the isocyanate source. This innovation not only extends pot life but also broadens the pre-print processing temperature range. Surface-modified fumed silica, used as a rheology modifier, ensures the maintenance of Bingham fluid characteristics. Rigorous evaluations, including DSC, tensile tests, SEM, OM, and μ-CT, verify the material’s uniform and nearly isotropic structure, devoid of defects. DMA analysis reveals that these 3D-printed PUs withstand processing temperatures up to 240°C. The practical application of this technology is demonstrated through the successful 3D printing of a shoe sole, showcasing the ability to incorporate regions of varying hardness, highlighting the versatile property customization of this method.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Rapid biodegradation of microplastics generated from bio-based thermoplastic polyurethane

The accumulation of microplastics in various ecosystems has now been well documented and recent evidence suggests detrimental effects on various biological processes due to this pollution. Accumulation of microplastics in the natural environment is ultimately due to the chemical nature of widely used petroleum-based plastic polymers, which typically are inaccessible to biological processing. One way to mitigate this crisis is adoption of plastics that biodegrade if released into natural environments. In this work, we generated microplastic particles from a bio-based, biodegradable thermoplastic polyurethane (TPU-FC1) and demonstrated their rapid biodegradation via direct visualization and respirometry. Furthermore, we isolated multiple bacterial strains capable of using TPU-FC1 as a sole carbon source and characterized their depolymerization products. Finally, to visualize biodegradation of TPU materials as real-world products, we generated TPU-coated cotton fabric and an injection molded phone case and documented biodegradation by direct visualization and scanning electron microscopy (SEM), both of which indicated clear structural degradation of these materials and significant biofilm formation.

09 BIOMASS FUELS↗
DOE OSTI2022

Tunable polyvinyl chloride (PVC) and thermoplastic polyurethane (TPU)-based soft polymer gel sensors

Abstract Polyvinyl chloride (PVC) gels have recently been found to exhibit mechanoelectrical transduction under mechanical deformation. These mechanoelectrical properties of PVC gels are largely uncharacterized and the underlying transduction mechanisms are currently unknown. These soft electroactive polymers have tunable properties such as modulus and response voltage based on physical dimensions and the amount of plasticizer content within the material making them ideal candidates for complaint sensors. This study aims to investigate PVC gels comprised of various plasticizers to further investigate underlying mechanisms of mechanoelectrical transduction and broaden possible sensing applications. Plasticizers used in this study include dibutyl adipate, dibutyl phthalate, dioctyl phthalate, otherwise known as bis(2-ethylhexyl) phthalate, diisodecyl adipate, and the environmentally friendly biodegradable plasticizer acetyl tributyl citrate (ATBC). ATBC is often used in cosmetics and food packaging applications and is even used as a food additive which may lead to future biocompatibility for these gel sensors. These plasticizers are used to produce PVC gel sensors that are experimentally tested for mechanoelectrical transduction properties and sensing performance. In this study, a Langmuir adsorptive model is fit to the collected mechanoelectrical transduction data. These results are also nondimensionalized and compared to the characteristic dimensionless Langmuir adsorptive model. This simple model agrees very well with the experimental data. Additionally, a study on the mechanoelectrical transduction of an alternative polymer lattice structure, thermoplastic polyurethane (TPU), is discussed. This is a novel electroactive polymer investigated for mechanoelectrical transduction properties. This portion of the study aims to further knowledge of underlying mechanisms of mechanoelectrical transduction as well as show feasibility of additional lattices for soft polymer gel sensors. These TPU gel sensors show strikingly similar mechanoelectrical transduction properties to analogous PVC gels, insinuating that the polymer structure has a limited role in the underlying sensing mechanism and PVC itself is not unique to polymer gel sensing. The TPU-based soft polymer gel sensors however do display some level of mechanoelectrical hysteresis which may be attributed to viscoelastic properties and display a small amount of fatigue possibly due to exudation of liquid plasticizer. This study provides further characterization of mechanoelectrical response for varying plasticizers, provides a theoretical framework for underlying mechanisms, and displays the potential for further polymeric gel sensors.

Instruments & Instrumentation↗
DOE OSTI2021

The preparation and properties of polyurethane foams reinforced with bamboo fiber sources in China

Abstract Polyurethane (PU) foams reinforced with bamboo fiber sources in China, i.e. , bamboo fiber, bamboo α -cellulose fiber, and bamboo nanocellulose fiber, were prepared and their physico-mechanical properties were analyzed in this work. The bamboo fiber sources and PU foams were characterized by Fourier transform infrared spectroscopy (FTIR), Scanning electron microscope (SEM), Thermal gravimetric analysis (TGA) and universal compression testing. The results indicated that the hydroxyl groups on the fiber surfaces were enhanced by removing non-celluloses in the preparation of α -cellulose and nanocellulose. With the addition of small particle size α -cellulose and nanocellulose, the cell sizes of PU foams were reduced due to more nucleating agents being introduced. The FTIR spectra confirmed that the bamboo fiber sources were involved in the foaming reaction. The PU foams with bamboo fiber sources had a higher thermal stability than neat foam, and they were satisfactory enough to be used as insulation. PU foams reinforced with 5% bamboo fiber, 3% α -cellulose fiber and 3% nanocellulose fiber had better physico-mechanical performance than other foams. The reinforcement performance of 3% bamboo α -cellulose fiber on PU foam was comparable with that of high-cost nanocellulose. Accordingly, bamboo α -cellulose fiber was demonstrated to be a promising candidate to reinforce PU foam, which could be used in the reinforcement of foam insulation.

Qiu, Chongpeng↗
DOE OSTI2023

Effect of Dual Environment Aging on Flexible Polyurethane Based Adhesive

Abstract Environmental degradation of adhesives naturally increases with the intensity of the ambient weathering agents involved. During service life, these materials are never subjected to a constant environmental loading. Real-time applications expose the material to multiple weather conditions, ranging from dry to humid or fully wet conditions. While some understanding exists about aging environments in isolation, we intend to investigate the effect of multiple environments on the constitutive behavior of the materials in question. The extent of damage can be accessed by analyzing the changes in constitutive behavior and toughness of aged material. Therefore, this aging experiment was designed around two-way aging regimes involving combinations of thermo-oxidation, hydrolytic and hygrothermal aging environments. We selected a polyurethane based flexible adhesive which is commonly used in the automotive industry as a glass sealant. The aged specimens were subjected to uniaxial tensile tests, and variation in material toughness and constitutive behavior was analyzed to ascertain the mechanics involved in the case of each environmental exposure. We outlined how different environments affect the material in isolation and how they interact with other weathering conditions. This study will help better understand and model the damage mechanics involved in exposure to multiple environmental conditions.

Shaafaey, Mamoon↗
DOE OSTI2023

On the 3D printability of one-part moisture-curable polyurethanes via direct ink writing (DIW)

Direct ink writing (DIW) is an ambient temperature additive manufacturing (AM) method that accommodates many possible ink materials. Here, in this work, we demonstrate using a moisture-curable commercially available polyurethane (PU) sealant as an alternative ink for DIW. We discussed the fundamentals of PU chemistry and determined the best 3D printing parameters. Studies on rheological, thermogravimetric, spectroscopic characterization, and initial finite element analyses (FEA) showed properties expected from a performance sealant with high elongation and low modulus of a 3D-printed object. This affirms the flexibility of the DIW technique as an accessible AM method amenable for future materials development from commercial model formulations.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Dynamic characterization of frequency response of shock mitigation of a polymethylene diisocyanate (PMDI) based rigid polyurethane foam

Kolsky compression bar experiments were conducted to characterize the shock mitigation response of a polymethylene diisocyanate (PMDI) based rigid polyurethane foam, abbreviated as PMDI foam in this study. The Kolsky bar experimental data was analyzed in the frequency domain with respect to impact energy dissipation and acceleration attenuation to perform a shock mitigation assessment on the foam material. The PMDI foam material exhibits excellent performance in both energy dissipation and acceleration attenuation, particularly for the impact frequency content over 1.5 kHz. This frequency (1.5 kHz) was observed to be independent of specimen thickness and impact speed, which may represent the characteristic shock mitigation frequency of the PMDI foam material under investigation. The shock mitigation characteristics of the PMDI foam material were insignificantly influenced by the specimen thickness. As a result, impact speed did have some effect.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Accelerated Aging of BKC 44306-10 Rigid Polyurethane Foam: FT-IR Spectroscopy, Dimensional Analysis, and Micro Computed Tomography

An accelerated aging study of BKC 44306-10 rigid polyurethane foam was carried out. Foam samples were aged in a nitrogen atmosphere at three different temperatures: 50 °C, 65 °C, and 80 °C. Foam samples were periodically removed from the aging canisters at 1, 3, 6, 9, 12, and 15 month intervals when FT-IR spectroscopy, dimensional analysis, and mechanical testing experiments were performed. Micro Computed Tomography imaging was also employed to study the morphology of the foams. Over the course of the aging study the foams the decreased in size by a magnitude of 0.001 inches per inch of foam. Micro CT showed the heterogeneous nature of the foam structure likely resulting from flow effects during the molding process. The effect of aging on the compression and tensile strength of the foam was minor and no cause for concern. FT-IR spectroscopy was used to follow the foam chemistry. However, it was difficult to draw definitive conclusions about the changes in chemical nature of the materials due to large variability throughout the samples.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Validation of Heat Transfer Thermal Decomposition and Container Pressurization of Polyurethane Foam.

Polymer foam encapsulants provide mechanical, electrical, and thermal isolation in engineered systems. In fire environments, gas pressure from thermal decomposition of polymers can cause mechanical failure of sealed systems. In this work, a detailed uncertainty quantification study of PMDI-based polyurethane foam is presented to assess the validity of the computational model. Both experimental measurement uncertainty and model prediction uncertainty are examined and compared. Both the mean value method and Latin hypercube sampling approach are used to propagate the uncertainty through the model. In addition to comparing computational and experimental results, the importance of each input parameter on the simulation result is also investigated. These results show that further development in the physics model of the foam and appropriate associated material testing are necessary to improve model accuracy.

Scott, Sarah Nicole↗
DOE OSTI2014

Mechanical Characterization of Rigid Polyurethane Foams

Foam materials are used to protect sensitive components from impact loading. In order to predict and simulate the foam performance under various loading conditions, a validated foam model is needed and the mechanical properties of foams need to be characterized. Uniaxial compression and tension tests were conducted for different densities of foams under various temperatures and loading rates. Crush stress, tensile strength, and elastic modulus were obtained. A newly developed confined compression experiment provided data for investigating the foam flow direction. A biaxial tension experiment was also developed to explore the damage surface of a rigid polyurethane foam.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Experiments to Populate and Validate a Processing Model for Polyurethane Foam: Additional Data for Structural Foams

We are developing computational models to help understand manufacturing processes, final properties and aging of structural foam, polyurethane PMDI. Th e resulting model predictions of density and cure gradients from the manufacturing process will be used as input to foam heat transfer and mechanical models. BKC 44306 PMDI-10 and BKC 44307 PMDI-18 are the most prevalent foams used in structural parts. Experiments needed to parameterize models of the reaction kinetics and the equations of motion during the foam blowing stages were described for BKC 44306 PMDI-10 in the first of this report series (Mondy et al. 2014). BKC 44307 PMDI-18 is a new foam that will be used to make relatively dense structural supports via over packing. It uses a different catalyst than those in the BKC 44306 family of foams; hence, we expect that the reaction kineti cs models must be modified. Here we detail the experiments needed to characteriz e the reaction kinetics of BKC 44307 PMDI-18 and suggest parameters for the model based on these experiments. In additi on, the second part of this report describes data taken to provide input to the preliminary nonlinear visco elastic structural response model developed for BKC 44306 PMDI-10 foam. We show that the standard cu re schedule used by KCP does not fully cure the material, and, upon temperature elevation above 150°C, oxidation or decomposition reactions occur that alter the composition of the foam. These findings suggest that achieving a fully cured foam part with this formulation may be not be possible through therma l curing. As such, visco elastic characterization procedures developed for curing thermosets can provide only approximate material properties, since the state of the material continuously evolves during tests.

36 MATERIALS SCIENCE↗
DOE OSTI2015

A Kinetic Approach to Modeling the Manufacture of High Density Polyurethane Structural Foam: Foaming and Polymerization

This report details the study of PMDI structural foam and the development of a computational model to represent it. This polyurethane has a fast catalyst, such that foaming and polymerization occur simultaneously. The foam is over-packed to twice or more of its free rise density to reach the density of interest. Our approach is to combine model development closely with experiments to discover underlying physical phenomena, to parameterize models, and to validate the models once they have been developed. The model must be able to represent the expansion, filling of molds, curing, and final foam properties. PMDI is a chemically blown foam, where carbon dioxide is produced via the reaction of water and isocyanate. The isocyanate also reacts with polyol in a competing reaction, which produces the polymer. A new kinetic model is developed and implemented, which follows a simplified mathematical formalism that decouples these two reactions. The model predicts the polymerization reaction via condensation chemistry, where vitrification and glass transition temperature evolution must be included to correctly predict the temperature dependence of the kinetics. The foam gas generation kinetics are determined by tracking the molar concentration of both water and carbon dioxide. Understanding the thermal history and loads on the foam due to exothermicity and oven curing is very important to the results, since the kinetics and material properties are all sensitive to temperature. The conservation equations, including the equations of motion, an energy balance, and three rate equations are solved via a stabilized finite element method. We assume generalized-Newtonian rheology that is dependent on the extent of cure, gas fraction, and temperature. The conservation equations are combined with a level set method to determine the location of the free surface over time. Results from the model are compared to experimental flow visualization data and post-test X-ray computed tomography (CT) data for the density. Several geometries are investigated including a mock encapsulation part, two configurations of a mock structural part, and a bar geometry to specifically test the density model. We have found that the model predicts both average density and filling profiles well. However, it under predicts density gradients, especially in the gravity direction. Further model improvements are also discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Modeling Manufacturing Impacts on Aging and Reliability of Polyurethane Foams

Polyurethane is a complex multiphase material that evolves from a viscous liquid to a system of percolating bubbles, which are created via a CO2 generating reaction. The continuous phase polymerizes to a solid during the foaming process generating heat. Foams introduced into a mold increase their volume up to tenfold, and the dynamics of the expansion process may lead to voids and will produce gradients in density and degree of polymerization. These inhomogeneities can lead to structural stability issues upon aging. For instance, structural components in weapon systems have been shown to change shape as they age depending on their molding history, which can threaten critical tolerances. The purpose of this project is to develop a Cradle-to-Grave multiphysics model, which allows us to predict the material properties of foam from its birth through aging in the stockpile, where its dimensional stability is important.

36 MATERIALS SCIENCE↗