Influence of high temperatures on the strength of solidified resins and materials based on resins
Temperature effects on strength of phenol formaldehyde, phenol phosphorus, melamine formaldehyde, and organosilicon resins
ORGANIC SILICON COMPOUND↗
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Influence of Temperature on Creep, Stress-rupture and Static Properties of Melamine-resin and Silicone-resin Glass-fabric Laminates
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Findley, William N↗
Loading Capacity and Dilute Nitric Acid Rinse of Diglycolamide Resin for the Recovery of Transplutonium and Rare Earth Elements from Mark-18A Targets
N,N,N′,N′-tetraoctyldiglycolamide (TODGA) as a resin (“DGA resin”) produced by Eichrom Technologies will be used by Savannah River National Laboratory for the indiscriminate extraction of trivalent actinides and rare earth elements with the intent of recovering Cm and Am from dissolved irradiated 242 Pu Mark-18A targets in 7 to 9 M nitric acid. The extracted constituents will be recovered as an oxide by direct thermal decomposition of the loaded resin followed by calcination of the resultant residue. The characteristics of DGA resin with non-radiological feed simulant representative of the anticipated feed in the Mark-18A process, with Sm and Nd as surrogates for Cm and Am, respectively, including breakthrough point and saturation capacity were evaluated in this work. Additionally, this work examined the losses from the loaded resin by rinsing the resin bed with dilute acid to reduce the nitrate concentration in the resin bed prior to thermal decomposition operations to improve the safety posture of the process. A resin loading profile was developed, and the resin was determined to have a trivalent metal saturation capacity of 74 μmol/mL resin under the experimental conditions evaluated. Following a wash of the loaded resin bed with fresh 8 M HNO 3 , the trivalent metals retained was reduced to 68 μmol/mL resin, which represents the practical capacity of the resin for the Mark-18A process. Lighter lanthanides breakthrough the resin well before the saturation capacity is reached. Rinsing the saturated resin bed with 0.26 M HNO 3 was found to result in a rapid reduction in retention of rare earth elements by the resin. After 2.8 bed volumes of dilute acid rinse, the mean resin bed free acid concentration was reduced to 0.28 M and 3.1 bed volumes of dilute acid rinse resulted in a reduction of the cumulative rare earth element retention to 52 μmol/mL of resin.
Transplutonium separations↗
Sulfate Conversion of Reillex HPQ Anion Exchange Resin for Disposal (Interim Report)
This report describes preliminary data to validate the Savannah River Plutonium Processing Facility’s (SRPPF) flowsheet for conversion of used Reillex HPQ anion exchange resin from the nitrate form to the sulfate form. The nitrate form is an oxidizer and therefore does not meet acceptance criteria for disposal at the Waste Isolation Pilot Plant (WIPP). The purpose of this study is to develop data to support acceptance for this disposition pathway. Due to the challenges characterizing the nitrate concentration on solid resin, the data developed to date are based upon indirect analysis of the ion exchange column effluent by ion chromatography. These challenges are discussed and two methods for quantification of nitrate directly on the resin are recommended for further development: TGA-MS and permanganate digestion followed by IC. The resin used for this work was provided in the chloride form; this is the form in which resin is supplied by the manufacturer. However, it had to be converted to the nitrate form, which is the form that will be used in SRPPF’s ion exchange process, prior to use in the sulfate conversion experiments. The chloride-form resin was characterized. A lab-scale procedure for the conversion of Reillex HPQ resin from the chloride to nitrate form was validated. The nitrate-form resin was assessed for particle size and chloride concentration to ensure it met SRPPF’s facility specifications. The baseline sulfate conversion flowsheet was tested. However, nitrate was still detectable in the effluent after approximately 10 bed volumes of 1 M sodium sulfate had been passed through the resin bed. Additional experiments were performed to assess the effect of increasing the feed volume, reducing the flowrate, the use of 2 M sulfuric acid instead of sodium sulfate, and the use of irradiated resin. The sulfuric acid test was the only one which provided a nondetectable nitrate concentration (<0.002 M) in the effluent. Detectable nitrate in the column effluent suggests that nitrate is still present on the resin itself.
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
Extraction of Pure Plastic Resins From PCR Plastic Waste by Solvent-Targeted Recovery and Precipitation (STRAP)
For this work, we have been developing a solvent‐based plastic recycling technology called STRAP. The technology is based on dissolving a targeted plastic resin in a specific solvent that does not dissolve other resins. We have demonstrated STRAP in thousands of bench scale experiments for a large variety of wastes. Recently we have demonstrated the technology for PCR, using mixed plastic wastes (MPWs), from a wet Material Recovery Facility (MRF). The process includes (1) infrared (IR) characterization to determine the plastic composition for accurate selection of the solvent to be used for the extraction of the pure resins. (2) Shredding to the right size and aspect ratio required for flowable and fast dissolvable process. (3) Mixing the MPW in the first solvent to dissolve the first resin. (4) Filtration of the solution plastic blend, to separate the nondissolved plastic from the solution. (5) Further filtration of the solution to remove micron‐sized particle of pigments and fibers. (6) Cooling for precipitation. (7) Filtration of pure resins. (8) Drying of a pure resin. (9) Extrusion of the resin to pellets. (10) Generating films or other products from the pure resin. Steps 1–10 can be considered as one‐cycle that extracted the first resin. (11) A second resin can be extracted with a respective solvent from the plastic that did not dissolve in the first cycle and following steps 1–10 described above. The process also includes characterization of interim and final products. The effort includes building a pilot system at 25 kg/h throughput. We will present specific results for various PCR.
IR characterization↗
Effect of Composition Variation on Isothermal Rapid Curing Resins for Aerospace Applications
To meet the projected demand for single-aisle composite aircraft in 2040, the production rate of these aircraft will need to increase by four to six times what is currently achievable. A composite manufacturing process with the potential to enable the targeted rates is isothermal resin infusion where infusion and cure occur at the same temperature. However, presently there is not an accepted aerospace-grade resin that can support this isothermal infusion process and maintain acceptable resin properties. Therefore, resin development initiatives have designed anionic catalyzed epoxy systems capable of isothermal infusion and rapid cure at a temperature below 100 ˚C in one hour. High-performance aerospace properties are achieved after undergoing a freestanding post-cure. The resins facilitate faster, energy efficient production cycles by reducing the time and temperature required for cure and eliminating temperature ramps typically required of materials used in the aerospace industry. This work discusses several of the developed resin systems and the impact of varying composition on rheological, thermal, and mechanical properties. Carbon fiber composites were fabricated for one composition by resin transfer molding to demonstrate the potential of these isothermal, rapid cure systems for meeting industry needs.
resin transfer molding↗
PFAS Removal by Ion Exchange Resins: Background and Knowledge Gaps with Respect to the Hanford Site
Per- and polyfluoroalkyl substances (PFAS) have been a rising concern for the past two decades, with the United States Department of Defense and Environmental Protection Agency investing millions of dollars in research into remediation and clean-up technologies. Due to the environmental persistence, toxicity, biological uptake, and ongoing changes in both federal and state regulatory space, understanding the fate and transport of PFAS compounds has been of growing concern to the US Department of Energy (DOE). The DOE’s Hanford Site is investigating historical use of PFAS and will be doing site characterization for PFAS. Thus, PFAS have not yet been identified as a contaminant concern in regulatory documents. Based on historical records that mention the discharge of aqueous film-forming foam containing PFAS and having on-site fire stations (a risk factor for PFAS contamination), it seems likely that environmental releases of PFAS may have occurred. Pump and treat (P&T) remediation is the selected remedy for multiple groundwater contaminant plumes at Hanford. These P&T systems use ion exchange (IX) as a component of aboveground treatment, with the specific resins depending on the target contaminants. There is potential that these IX resins may be able to remove PFAS from groundwater, but investigation is needed to understand affinity/selectivity and removal capacity given the groundwater composition and the operating conditions. This report provides background on PFAS uses and chemistry, then provides a review of IX resin applications for PFAS, identifying knowledge gaps. Recommendations are provided regarding research needed to address knowledge gaps and acquire information needed to propose IX as a future PFAS remediation technology at the Hanford Site, as well as other U.S. Department of Energy sites. Generally, PFAS compounds are fluorinated substances that contain at least one fully fluorinated methyl or methylene carbon – with a few noted exceptions, any chemical with at least a perfluorinated methyl group (–CF3) or a perfluorinated methylene group (–CF2–) is a PFAS. These chemical compounds are characterized as non-biodegradable, non-reactive, non-photolytic, and hydrolysis resistant. This makes them highly recalcitrant within the environment, however polyfluoroalkyl materials are less recalcitrant as the carbon chains contain C–H bonds which are more easily broken than carbon – fluorine (C–F) bonds. The backbone carbon structures are commonly punctuated with a head group, the most well-known of them are perfluorooctanesulfonic acid and perfluorooctanoic acid, which possess a sulfonate and a carboxylate group, respectively. IX resins are marketed for the removal of PFAS from water systems and industrial water, however, the mechanism of removal is not as well understood as for anion or cation removal. A better understanding of the mechanism of removal would enable the development of IX resins that have improved specificity for PFAS removal. Four knowledge gaps were identified: 1) the effect of dissolved ions on the IX resin PFAS removal effectiveness, 2) the effect of additional primary contaminants of concern (PCOCs) or secondary contaminants of concern (SCOCs) on the effectiveness of PFAS via IX resin, 3) the mechanisms of PFAS removal from water, and 4) practical solutions to IX resin regeneration and waste disposal.
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
Imide modified epoxy matrix resins
High char yield epoxy using novel bisimide amines (BIA's) as curing agents with a state of the art epoxy resin was developed. Stoichiometric quantities of the epoxy resin and the BIA's were studied to determine the cure cycle required for preparation of resin specimens. The bisimide cured epoxies were designated IME's (imide modified epoxy). The physical, thermal and mechanical properties of these novel resins were determined. The levels of moisture absorption exhibited by the bisimide amine cured expoxies (IME's) were considerably lower than the state of the art epoxies. The strain-to-failure of the control resin system was improved 25% by replacement of DDS with 6F-DDS. Each BIA containing resin exhibited twice the char yield of the control resin MY 720/DDS. Graphite fiber reinforced control (C) and IME resins were fabricated and characterized. Two of the composite systems showed superior properties compared to the other Celion 6000/IME composite systems and state of the art graphite epoxy systems. The two systems exhibited excellent wet shear and flexural strengths and moduli at 300 and 350 F.
Scola, D. A.↗
Performance Properties of Graphite Reinforced Composites with Advanced Resin Matrices
This article looks at the effect of different resin matrices on thermal and mechanical properties of graphite composites, and relates the thermal and flammability properties to the anaerobic char yield of the resins. The processing parameters of graphite composites utilizing graphite fabric and epoxy or other advanced resins as matrices are presented. Thermoset resin matrices studied were: aminecured polyfunctional glycidyl aminetype epoxy (baseline), phenolicnovolac resin based on condensation of dihydroxymethyl-xylene and phenol cured with hexamine, two types of polydismaleimide resins, phenolic resin, and benzyl resin. The thermoplastic matrices studied were polyethersulfone and polyphenylenesulfone. Properties evaluated in the study included anaerobic char yield, limiting oxygen index, smoke evolution, moisture absorption, and mechanical properties at elevated temperatures including tensile, compressive, and short-beam shear strengths. Generally, it was determined that graphite composites with the highest char yield exhibited optimum fire-resistant properties.
Kourtides, Demetrius A.↗
Separation of dilute plutonium(IV) from nitric acid solutions via Reillex HPQ anion exchange resin
Anion exchange is a common method for the separation of plutonium (Pu) in aqueous systems, providing high recovery and decontamination from impurities. Reillex HPQ anion exchange resin has been used around the Department of Energy complex in this application for decades but has typically been used for Pu feed concentrations greater than 1 g/L. It is desirable to recover Pu at more dilute concentrations from a dissolved used fuel or target element, for example. In this work, the performance of Reillex HPQ anion exchange resin was characterized with feed solutions of ca. 0.24 g/L Pu. A significant reduction in the performance of the resin was realized with this dilute concentration relative to a feed solution of 2.35 g/L Pu with similar feed flow rates and the same resin column, likely due to the increased driving force for mass transfer with a higher feed concentration. The maximum capacity of Reillex HPQ resin for Pu can be improved by reducing the flow rate and increasing the feed Pu concentration. Furthermore, the breakthrough point of Pu can be improved in the same manner and by increasing the resin bed height. Diffusion of Pu into the resin was illustrated to be the rate limiting step.
Plutonium separations↗
Utilization of traceable standards to validate plutonium isotopic purification and separation of plutonium progeny using AG MP-1M resin for nuclear forensic investigations
Radio-chronometric studies on plutonium (Pu) materials require independent measurement of the Pu (parent) content and isotopic distribution as well as concentration and isotopic distribution of the plutonium isotopic decay products. We performed a series of experiments to demonstrate the consistency of separations using the Lewatit MP 800 macroporous anion exchange resin and the AG MP-1M resin with traceable Pu isotopic certified reference material (CRM) standards 136, 137, 138, and 126-A. Two different mesh-sizes of the AG MP-1M resin were tested and the 50–100 mesh size resin was found to work more efficiently for the separation task. Both Lewatit and AG MP-1M resins were found to perform satisfactorily for quantitatively extracting the americium (Am) and uranium (U) progeny as well as gallium (Ga) present as a tracer in the Pu material. Both resins were effective in removing isobaric interferences from the Pu fraction used in isotopic measurements by thermal ionization mass spectrometry (TIMS). To address the co-elution of uranium and gallium, Alizarin red S (ARS) was used as a colorimetric dye to determine the behavior of UO 2 2+ and Ga 3+ on AG MP-1M resin with various acidic solutions as eluents using UV–vis spectra. Poor resolution of these peaks complicated quantitative analysis by UV–vis spectroscopy, but these results were informative in planning automated separation experiments by HPLC. LA-UR-24-28919.
38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
Evaluation of chromatographic resins for high efficacy separation of radium from chemical analogues
The separation of Radium (Ra) from interfering chemical analogues is of major importance for both the accurate measurement of Ra-226 in environmental samples and the preparation of radium targets destined for medical isotope production. The adsorption behavior of Ra, Barium (Ba), and Strontium (Sr) was investigated on multiple crown-ether-based proprietary extraction chromatographic resins developed by TrisKem Int. Among these, the TK101 resin, characterized by a novel room-temperature ionic liquid (RTIL) dual extractant–solvent system, demonstrated enhanced affinity and selectivity, particularly at low acid concentrations, achieving a D w of 3477 ± 73 for Ra in 0.04 M HNO₃, whereas the maximum Ra D w obtained with the traditional Sr resin in 8 M HNO 3 was only 12.33 ± 0.4. In 0.04 M HNO 3 , a Ra distribution ratio (D w ) of 776 was achieved within 1 min, indicating rapid uptake kinetics. The adsorption capacities were estimated at 19.6 ± 0.1 mg/g for Ba and 12.0 ± 0.2 mg/g for Sr. However, competing alkali metals significantly reduced alkaline earth metal uptake, indicating that the TK101 resin is best suited for radium purification following a preconcentration step to minimize matrix effects in high salinity samples. Dynamic column studies confirmed the strong chromatographic performance of the TK101 resin, with no significant Ba or Sr breakthrough in the Ra fraction and a Ra recovery of 87 ± 2.8%. These results demonstrate the potential of the TK101 resin for selective radium separation in analytical and radiochemical applications.
and nuclear chemistry↗
Surviving nanoscale interfacial stability in extreme thermal expansion contrast Zn(CN) 2 -epoxy resin matrix composites
Here, we report the remarkable stability at the nanoscale matrix-filler interface in a series of overall low coefficient of thermal expansion (CTE) zinc cyanide (ZC)/epoxy resin composites. These interfaces demonstrate the stability of highly contrasting materials. These composites are designed to optimize the properties of both materials: epoxy resins are valued for their high strength, superb chemical resistance, low dielectric properties, and adhesive abilities. ZC, a model flexible framework, exhibits negative thermal expansion (NTE) behavior and compensates for the epoxy resin’s detrimentally large thermal expansion values. Filled resins minimize the native 65 ppm/°C CTE values to 19 ppm/° C over a wide temperature range while maintaining linearity, yielding composites compatible with typical metal and ceramic substrates’—commonly bonded to the resin— 0–20 ppm/° C CTE values. Additionally, with significant intrinsic differences in the materials, we use wide-angle X-ray diffraction and atomic force microscopy to elucidate thermal movement. The ZC/epoxy interface is surprisingly resilient over 1,000 cycles between -55° C and 75° C, extremes typical to aerospace applications. Further, we show that the resin viscosity remains less than 21 Pa*s at up to 30 vol% ZC, an important consideration for workability. We also discuss settling distribution, glass transition temperature, flexural strength, and longevity. All results point favorably towards practical implementation in low thermal expansion application needs: filling the gap in component design.
42 ENGINEERING↗
Reactive Modified Epoxy Resin and Its Miscible Blends Based on Recycled Oligomers from Solvolysis
Chemical depolymerization of fully cured epoxy resin with 20% reactive modifier was successfully performed via a solvent-assisted solvolysis process into low molecular weight recyclable oligomers (RO) at 240 °C in a pressure vessel at 650 psi for 4 h. The thermoset epoxy resin was depolymerized into transparent brown viscous fluid with a higher viscosity than the uncured epoxy resin with approximately 93% yield. Different concentrations of the RO were homogeneously mixed with the pure epoxy resin, and their curing kinetics, viscosity, FTIR, mechanical properties, DMA, and cross-link density were investigated. The curing kinetics of the pure reactive modified epoxy resin (baseline) and its mixtures with RO of different concentrations were investigated under both isothermal and nonisothermal conditions using small amplitude oscillatory shear flow. The elastic and viscous moduli (G′ and G″), complex viscosity (η*), and tan δ values were evaluated at different curing times and temperatures. The G′, G″, and η* increased dramatically, while tan δ decreased strongly by several orders of magnitude at the gel point. The zero-shear viscosity (η 0 ) was determined from the angular frequency dependent on η* based on the Cross model for different blend compositions in the liquid state before curing. The composition dependence of η 0 showed a positive deviation from the linear mixing rule and was well described by the Lecyar model. Here, the apparent activation energy of curing (E a ) was also evaluated according to the Arrhenius equation and was found to be 46 ± 2 kJ/mol regardless of the different contents of RO. For all blends up to 40 wt % RO, only one tan δ peak systematically shifting to lower temperatures with increasing content of RO was observed in the DMA measurements, indicating that the epoxy resin and the RO are miscible with up to 40 wt % RO.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Graphite fiber reinforced thermoplastic resins
Mechanical properties of neat resin samples and graphite fiber reinforced samples of thermoplastic resins were characterized with particular emphasis directed to the effects of environmental exposure (humidity, temperature and ultraviolet radiation). Tensile, flexural, interlaminar shear, creep and impact strengths were measured for polysulfone, polyarylsulfone and a state-of-the-art epoxy resin samples. In general, the thermoplastic resins exhibited environmental degradation resistance equal to or superior to the reference epoxy resin. Demonstration of the utility and quality of a graphite/thermoplastic resin system was accomplished by successfully thermoforming a simulated compressor blade and a fan exit guide vane.
Novak, R. C.↗
Bismaleimide resins for flame resistant honeycomb sandwich panels
Bismaleimide resins are prime candidates for nonflammable aircraft interior panels. Three resin types with different structures and processing characteristics were formulated. Resin M 751 was used to fabricate 100 kg of glass fabric prepregs which were used for the preparation of face sheets for honeycomb sandwich panels. Prepreg characteristics and curing cycles for laminate fabrication are provided. In order to advance beyond the current solvent resin technology for fibre and fabric impregnation, a hot melt solvent-less resin system was prepared and characterized. Preliminary tests were performed to develop a wet bonding process for the fabrication of advanced sandwich honeycomb panels by use of polybismaleimide glass fabric face sheets and polybismaleimide Nomex honeycomb core. B-stage material was used for both the core and the face sheet, providing flatwise tensile properties equivalent to those obtained by the state-of-the-art 3-step process which includes an epoxy adhesive resin.
Stenzenberger, H. D.↗
Thermal expansion and swelling of cured epoxy resin used in graphite/epoxy composite materials
The paper presents results of experiments in which the thermal expansion and swelling behavior of an epoxy resin system and two graphite/epoxy composite systems exposed to water were measured. It was found that the cured epoxy resin swells by an amount slightly less than the volume of the absorbed water and that the swelling efficiency of the water varies with the moisture content of the polymer. Additionally, the thermal expansion of cured epoxy resin that is saturated with water is observed to be more than twice that of dry resin. Results also indicate that cured resin that is saturated with 7.1% water at 95 C will rapidly increase in moisture content to 8.5% when placed in 1 C water. The mechanism for this phenomenon, termed reverse thermal effect, is described in terms of a slightly modified free-volume theory in conjunction with the theory of polar molecule interaction. Nearly identical behavior was observed in two graphite/epoxy composite systems, thus establishing that this behavior may be common to all cured epoxy resins.
Adamson, M. J.↗