Polymerization-Induced Phase Separation in Rubber-Toughened Amine-Cured Epoxy Resins: Tuning Morphology from the Nano- to Macro-scale
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99 GENERAL AND MISCELLANEOUS↗
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Evaluation of high pressure water blast with rotating spray bar for removing paint and rubber deposits from airport runways, and review of runway slipperiness problems created by rubber contamination
A high pressure water blast with rotating spray bar treatment for removing paint and rubber deposits from airport runways is studied. The results of the evaluation suggest that the treatment is very effective in removing above surface paint and rubber deposits to the point that pavement skid resistance is restored to trafficked but uncontaminated runway surface skid resistance levels. Aircraft operating problems created by runway slipperiness are reviewed along with an assessment of the contributions that pavement surface treatments, surface weathering, traffic polishing, and rubber deposits make in creating or alleviating runway slipperiness. The results suggest that conventional surface treatments for both portland cement and asphaltic concrete runways are extremely vulnerable to rubber deposit accretions which can produce runway slipperiness conditions for aircraft operations as or more slippery than many snow and ice-covered runway conditions. Pavement grooving surface treatments are shown to be the least vulnerable to rubber deposits accretion and traffic polishing of the surface treatments examined.
Horne, W. B.↗
Alkali-activated slag (AAS) and OPC-based composites containing crumb rubber aggregate: Physico-mechanical properties, durability and oxidation of rubber upon NaOH treatment
Value-added utilization of waste tires in cementitious materials has been studied for decades, whereas the synergy between rubber and alkali-activated cements deserves more investigations. To this end, we compared physico-mechanical and durability properties of alkali-activated slag (AAS) and OPC-based composites containing NaOH-pretreated/as-received crumb rubber (CR). It was found that the incorporation of CR had both positive and negative effects on specimens due to its special attributes. CR reduced electrical conductivity which was associated with the ion transport ability, since it worked as an electrical insulator and increased hydrophobicity of pore walls. The sulfate expansion decreased with CR content because the flow of sulfate ions was demobilized, and the flexibility of CR relieved the internal stress. CR also improved the freeze-thaw durability of composites if the total CR content was less than 30% in specimens. However, the low Young's modulus of CR impaired the compressive strength and failed to effectively control the total shrinkage upon drying. The composites with CR must avoid high temperature exposure which resulted in the pyrolysis of rubber. In addition, the NaOH pretreatment enhanced adhesion between CR and hydrated cement and improved overall performances of composites. The FTIR spectra confirmed the NaOH-induced accelerated oxidation of CR surface and the generation of polar functional groups including carbonyl and carboxyl groups, increasing the total surface energy of rubber. More importantly, the alkali-activation process for AAS could treat the CR aggregate in the meantime, which means the use of CR in alkali-activated cements does not require the pretreatment of CR before blending.
36 MATERIALS SCIENCE↗
Dynamic and Flight Tests on Rubber-Cord and Oleo-Rubber-Disk Landing Gears for an F6C-4 Airplane
The investigation described in this report was conducted for the purpose of comparing an oleo-rubber-disk and a rubber-cord landing gear, built for use on an F6C-4 airplane. The investigation consisted of drop tests under various loading conditions and flight tests on an F6C-4 airplane. In the drop tests the total work done on each gear and the work done on each of the shock-absorbing units were determined. For both drop tests and flight tests the maximum loads and accelerations were determined. The comparative results showed that the oleo gear was slightly superior in reducing the ordinary landing shocks, that it had a greater capacity for work, and that it was very superior in the reduction of the rebound. The results further showed that for drops comparable to very severe landings, the rubber-cord gear was potentially more effective as a shock-reducing mechanism. However, due to the construction of this chassis, which limited the maximum elongation of the cords, this gear was incapable of withstanding as severe tests as the oleo gear. The action of the oleo gear was greatly inferior to the action of an ideal gear. The maximum accelerations encountered during the flight tests for severe landings were 3.64g for the rubber-cord gear and 2.27g for the oleo gear. These were less than those experienced in free drops of 7 inches on either gear.
Peck, William C↗
Improved silicone-rubber-to-silicon-rubber bonding
Strongest bond of room-temperature-vulcanizing silicon rubber to itself results when freshly-mixed silicon rubber is applied to unprimed lightly-abraded precured silicon rubber surface.
Teramura, K.↗
Polyfunctional epoxies. I - Rubber-toughened brominated and nonbrominated formulations for graphite composites. II - Nonrubber versus rubber-toughened brominated formulations for graphite composites
A new trifunctional epoxy resin, Tris-(hydroxyphenyl) methane triglycidyl ether, is compared to a state-of-the-art tetraglycidyl 4,4'-diaminodiphenyl methane (TGDDM), in graphite composites. Rubber-toughened brominated formulations of the epoxy resin are compared to nonbrominated ones in terms of their mechanical performance, environmental stability, thermochemical behavior, and flame retardancy. It is shown that the new resin performs almost the same way as the TGDDM does, but has improved glass transition temperature and environmental properties. Brominated polymeric additives (BPA) of different molecular weights are tested as a Br source to flame retardant graphite epoxy composites. The optimal molecular weight of the BPA and its polymeric backbone length are derived and compared with a 10 percent rubber-toughened formulation of the epoxy resin. Results indicate that when the Br content in the graphite composite is increased without the use of rubber, the mechanical properties improved. The use of BPAs as tougheners for graphite composites is also considered.
Nir, Z.↗
Model fire tests on polyphosphazene rubber and polyvinyl chloride (PVC)/nitrile rubber foams
A video tape record of model room fire tests was shown, comparing polyphosphazene (P-N) rubber and polyvinyl chloride (PVC)/nitrile rubber closed-cell foams as interior finish thermal insulation under conditions directly translatable to an actual fire situation. Flashover did not occur with the P-N foam and only moderate amounts of low density smoke were formed, whereas with the PVC/nitrile foam, flashover occurred quickly and large volumes of high density smoke were emitted. The P-N foam was produced in a pilot plant under carefully controlled conditions. The PVC/nitrile foam was a commercial product. A major phase of the overall program involved fire tests on P-N open-cell foam cushioning.
Widenor, W. M.↗
In situ friction and wear behavior of rubber materials incorporating various fillers and/or a plasticizer in high-pressure hydrogen
Polymers are used routinely for equipment and infrastructure in hydrogen vehicle refueling stations, but significant gaps remain in understanding their hydrogen compatibility. The tribological properties of these materials in a high-pressure hydrogen environment is important in preventing component failure and the need for frequent replacement. We present in situ tribological studies on model rubbers, which include common fillers and plasticizer, using an in situ tribometer developed previously. Results suggest a clear, yet complicated, combined effect of the high-pressure hydrogen and the additives on the tribological performance of the chosen materials, as compared to matching experiments performed in ambient air. We find that the additives improved wear resistance in EPDM but deteriorated that in NBR due to disparate additive-polymer interactions.
Kuang, Wenbin↗
Microscopic Origins of the Nonlinear Behavior of Particle-Filled Rubber Probed with Dynamic Strain XPCS
The underlying microscopic response of filler networks in reinforced rubber to dynamic strain is not well understood due to the experimental difficulty of directly measuring filler network behavior in samples undergoing dynamic strain. This difficulty can be overcome with in situ X-ray photon correlation spectroscopy (XPCS) measurements. The contrast between the silica filler and the rubber matrix for X-ray scattering allows us to isolate the filler network behavior from the overall response of the rubber. This in situ XPCS technique probes the microscopic breakdown and reforming of the filler network structure, which are responsible for the nonlinear dependence of modulus on strain, known in the rubber science community as the Payne effect. These microscopic changes in the filler network structure have consequences for the macroscopic material performance, especially for the fuel efficiency of tire tread compounds. In this work, we elucidate the behavior with in situ dynamic strain XPCS experiments on industrially relevant, vulcanized rubbers filled (13 vol %) with novel air-milled silica of ultrahigh-surface area (UHSA) (250 m 2 /g). The addition of a silane coupling agent to rubber containing this silica causes an unexpected and counterintuitive increase in the Payne effect and decrease in energy dissipation. For this rubber, we observe a nearly two-fold enhancement of the storage modulus and virtually equivalent loss tangent compared to a rubber containing a coupling agent and conventional silica. Interpretation of our in situ XPCS results simultaneously with interpretation of traditional dynamic mechanical analysis (DMA) strain sweep experiments reveals that the debonding or yielding of bridged bound rubber layers is key to understanding the behavior of rubber formulations containing the silane coupling agent and high-surface area silica. These results demonstrate that the combination of XPCS and DMA is a powerful method for unraveling the microscale filler response to strain which dictates the dynamic mechanical properties of reinforced soft matter composites. With this combination of techniques, we have elucidated the great promise of UHSA silica when used in concert with a silane coupling agent in filled rubber. Such composites simultaneously exhibit large moduli and low hysteresis under dynamic strain.
36 MATERIALS SCIENCE↗
Chemical Recycling of Polybutadiene Rubber with Tailored Depolymerization Enabled by Microencapsulated Metathesis Catalysts
The effective management of plastic waste streams to prevent plastic land and water pollution is a growing problem that is also one of the most important challenges in polymer science today. Polymer materials that are stable over their lifetime and can also be cheaply recycled or repurposed as desired could more easily be diverted from waste streams. However, this is difficult for most commodity plastics. It is especially difficult to conceive this with intractable, cross-linked polymers such as rubbers. In this work, we explore the utility of microencapsulated Grubbs’ catalysts for the in-situ depolymerization and reprocessing of polybutadiene (PB) rubber. Second-generation Hoveyda-Grubbs catalyst (HG2) contained within glassy thermoplastic microspheres can be dispersed in PB rubber below the microsphere’s glass transition temperature (T g ) without adverse depolymerization, evidenced by rubber with and without these microspheres obtaining similar shear storage moduli of ≈16 and ≈28 kPa, respectively. The thermoplastic’s T g can be used to tune the depolymerization temperature, via release of HG2 into the rubber matrix. For example, using poly(lactic acid) (PLA) vs polysulfone results in an 85 and 162 °C depolymerization temperature, respectively. Liquefaction of rubber to a mixture of small molecules and oligomers is demonstrated using a 0.01 mol % catalyst loading using PLA as the encapsulant. Furthermore, at that same catalyst loading, depolymerization occurs to a greater extent in comparison to two ex-situ approaches, including a conventional solvent-assisted method, where it occurs at roughly twice the extent at each given catalyst loading. In addition, depolymerization of the microsphere-loaded rubbers was demonstrated for samples stored under nitrogen for 23 days. Lastly, we show that the depolymerized products can be reprocessed back into solid rubber with a shear storage modulus of ≈32 kPa. Thus, we envision that this approach could be used to recycle and reuse cross-linked rubbers at the end of their product lifetime.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Converting polyisoprene rubbers into bio-jet fuels via a cascade hydropyrolysis and vapor-phase hydrogenation process
Producing alternative drop-in bio-jet fuels from biomass provides a promising approach to achieve carbon neutrality. Here, to upcycle biomass-based polyisoprene rubbers into jet-fuel range C 10 cycloalkane, we proposed a cascade hydropyrolysis and vapor-phase hydrogenation process in a flow-through two-stage pressurized fixed-bed reactor. The hydropyrolysis temperature in the first stage is of vital importance for the formation of primary limonene intermediate in the non-catalytic degradation of polyisoprene rubbers, and a reaction temperature of 460 °C maximized limonene yield to 588.6 mg/g for natural rubber and 546.2 mg/g for Eucommia rubber. Over a Pt/C catalyst loaded in the second stage, the limonene intermediate produced from the first-stage reactor can be completely hydrogenated, giving a 642.7 mg/g yield of jet-fuel range C 10 cycloalkane with 83.6% selectivity. The depolymerization mechanism of polyisoprene rubbers was thoroughly studied, and a competitive reaction between limonene hydrogenation and limonene dehydrogenation was observed. This is the first report on producing C 10 cycloalkane from natural rubbers via a cascade hydropyrolysis and hydrogenation process, providing a promising strategy to upcycle polyisoprene rubbers into bio-jet fuels.
30 DIRECT ENERGY CONVERSION↗
Bio-Based Polyisoprene Can Mitigate Climate Change and Deforestation in Expanding Rubber Production
Biomass is a promising renewable feedstock to produce polyisoprene for the rubber industry. Through metabolic engineering, sugars derived from pretreated and hydrolyzed cellulose and hemicellulose can be directly fermented to isoprene to produce rubber. Here we investigate the life cycle environmental impact of isoprene fermentation to produce bio-polyisoprene from agricultural residues (of Zea mays L.). Results show that the greenhouse gas (GHG) intensity of bio-polyisoprene (−4.59 kg CO2e kg−1) is significantly lower than that of natural rubber (Hevea brasiliensis) and synthetic rubber (−0.79 and 2.41 kg CO2e kg−1, respectively), while supporting a circular biogenic carbon economy. We found the land use intensity of bio-polyisoprene to be 0.25 ha metric ton−1, which is 84% lower than that from rubber tree plantations. We compare the direct fermentation to isoprene results with indirect fermentation to isoprene through the intermediate, methyl butyl ether, where dehydration to isoprene is required. The direct fermentation of isoprene reduces reaction steps and unit operations, an expected outcome when employing process intensification, but our results show additional energy conservation and reduced contribution to climate change. Among the ReCiPe life cycle environmental impact metrics evaluated, air emission related impacts are high for bio-polyisoprene compared to those for natural and synthetic rubber. Those impacts can be reduced with air emission controls during production. All other metrics showed an improvement for bio-polyisoprene compared to natural and synthetic rubber.
Batten, Rahamim↗
Friction characteristics of three 30 by 11.5-14.5, type 8, aircraft tires with various tread groove patterns and rubber compounds
A test program was conducted to evaluate friction performance and wear characteristics on wet runways of three 30 x 11.5-14.5, type, aircraft tires having two different tread patterns and natural rubber contents. All test tires had the standard three circumferential groove tread, but two had molded transverse grooves which extended from shoulder to shoulder. The tread rubber content of the two tires with transverse grooves differed in that one had a 100 percent natural rubber tread and the other had a rubber tread composition that was 30 percent synthetic and 70 percent natural. The third test tire had the conventional 100 percent natural rubber tread. Results indicate that the differences in tire tread design and rubber composition do not significantly affect braking and cornering friction capability on wet or dry surfaces. Braking performance of the tires decreases with increased speed, with increased yaw angle and, at higher speeds, with increased wetness of the surface.
Yager, T. J.↗
ODC-Free Solvent Implementation Issues for Vulcanized Rubber and Bond Systems
Thiokol Propulsion has worked extensively to replace 1,1,1-trichloroethane (TCA) with ozone depleting chemicals (ODC)-free solvents for use in the manufacture of the Reusable Solid Rocket Motor (RSRM) for the Space Shuttle Program. As Thiokol has transitioned from sub-scale to full-scale testing and implementation of these new solvents, issues have been discovered which have required special attention. The original intent of Thiokol's solvent replacement strategy was to replace TCA with a single drop-in solvent for all equivalent applications. We have learned that a single candidate does not exist for replacing TCA. Solvent incompatibility with process materials has caused us to seek for niche solvents and/or processing changes that provide an ODC-free solution for special applications. This paper addresses some of the solvent incompatibilities, which have lead to processes changes and possible niche solvent usage. These incompatibilities were discovered during full-scale testing of ODC-free solvents and relate to vulcanized rubber and bond systems in the RSRM. Specifically, the following items are presented: (1) Cure effects of d-limonene based solvents on Silica Filled Ethylene Propylene Diene Monomer (SF-EPDM) rubber. During full-scale test operations, Thiokol discovered that d-limonene (terpene) based solvents inhibit the cure of EPDM rubber. Subsequent testing showed the same issue with Nitrile Butadiene Rubber (NBR). Also discussed are efforts to minimize uncured rubber exposure to solvents; and (2) Cured bond system sensitivity to ODC-free solvents. During full scale testing it was discovered that a natural rubber to steel vulcanized bond could degrade after prolonged exposure to ODC-free solvents. Follow on testing showed that low vapor pressure and residence time seemed to be most likely cause for failure.
Hodgson, James R.↗
Energy based fracture initiation criterion for strain-crystallizing rubber-like materials with pre-existing cracks
Fracture prediction is indispensable for polymers, like rubbers, which have a broad range of applications mainly due to their high extensibility. The phenomenon known as strain-induced crystallization further contributes to the fracture toughness of certain rubbers. Here in this study, a criterion based on internal bond energy, incorporating the effects of crystallization, is proposed to predict fracture initiation in rubber-like materials with pre-existing cracks. First, a multi-scale mechanical model is developed for characterizing the behavior of rubber when subjected to both uniaxial and biaxial deformation states. At the microscale, both the amorphous and crystalline chain segments are modeled as elastic in order to consider the energy contribution by the molecular bond distortions. This internal energy is considered along with the entropic and crystalline free energy for each chain. In the chain model, the effects of loading condition and the relative orientation of a chain on its crystallinity are taken into account. At the macroscopic scale, an existing crystallinity distribution function is adapted and a mixed finite element formulation with an augmented Lagrangian multiplier is utilized to impose the incompressibility constraint. A non-affine maximal advance path constraint based homogenization model is utilized for bridging the two scales. Its potential to account for anisotropy in the stretched network compels the model to be preferable due to its physical significance, for the purpose of fracture modeling. The rigidity of the crystallites is accounted for by proposing a crystallite distortion energy in addition to the critical bond dissociation energy, for fracture initiation to occur. The model is validated by comparison with existing experimental results for both crystallizing and non-crystallizing rubbers. In addition to its potential to predict the material behavior when subjected to uniaxial and biaxial loading, the capability of the model to quantitatively estimate the effect of crystallization on fracture initiation is also verified.
36 MATERIALS SCIENCE↗
Structural and Dynamical Roles of Bound Polymer Chains in Rubber Reinforcement
The addition of nanofillers to rubber matrices is a powerful route to improve the mechanical properties. Here, we focus on a molecular understanding of basic mechanisms that are important for the reinforcement in rubbers. The key role in this process is ascribed to bound rubber (BR) that engages with the matrix as well as with adjacent nanofillers. To date, this understanding has been impeded by the lack of experimental tools to directly probe the BR chains buried in a polymer matrix composed of the same polymer. To tackle this challenge, we combine neutron scattering/spectroscopy techniques with isotope-labeling and molecular dynamics simulations. The system is a simplified carbon-black-filled polybutadiene. The combined experimental and computational results provide new insights into the local structural and dynamical heterogeneities of BR chains and their interactions with the matrix polymer, highlighting (i) the structural partition of the bound chains into three components (i.e., trains, loops, and tails) and their fractions; (ii) their dynamical hierarchies, i.e., the trains that remain immobile on the filler surface, the loops that are fairly large and hence allow the interdigitation of matrix chains, and the tails with their unique characteristics to reach far out into the matrix and entangle with matrix chains. These multiple roles of the constituent components of the BR chains promote the formation of a well-developed adhesive polymer–filler interface, enhancing the elastic property of a filled rubber. Finally, the comprehensive understanding derived and validated by the model rubber will be translatable to many other polymer nanocomposites.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Friction characteristics of 20 x 4.4, type 7, aircraft tires constructed with different tread rubber compounds
A test program was conducted at the Langley aircraft landing loads and traction facility to evaluate the friction characteristics of 20 x 4.4, type, aircraft tires constructed with experimental cut-resistant, tread rubber compounds. These compounds consisted of different blends of natural rubber (NR) and an alfin catalyzed styrene-butadiene copolymer rubber (SBR). One tire having a blend of 30 SBR and 70 NR and another having a blend of 60 SBR and 40 NR in the tread were tested together with a standard production tire with no SBR content in the tread rubber. The results of this investigation indicated that the test tires constructed with the special cut-resistant tread rubber compositions did not suffer any significant degradation in tire friction capability when compared with the standard tire. In general, tire friction capability decreased with increasing speed and surface wetness condition. As yaw angle increased, tire braking capability decreased while tire cornering capability increased. Tread-wear data based on number of brake cycles, however, suggested that the tires with alfin SBR blends experienced significantly greater wear than the standard production tire.
Dreher, R. C.↗
Impact properties of rubber-modified epoxy resin-graphite-fiber composites
To improve the impact resistance of graphite-fiber composites, a commercial and an experimental epoxy resin were modified with liquid reactive rubber and a brominated epoxy resin. The commercial epoxy was a tetrafunctional resin, and the experimental epoxy was a trifunctional resin. The reactive rubber was a carboxyl-terminated butadiene-acrylonitrile copolymer. The rubber content was varied from 0 to 25 percent (wt). The brominated epoxy resin was used at Br levels of 4, 19, and 35 percent of the resin. Composites were prepared with woven graphite cloth reinforcement. The composites were evaluated by using flexural strength in the dry state and an elevated temperature after saturation with water. The impact properties were determined by measuring shear strength after falling-ball impact and instrumented impact. The rubber-modified, trifunctional resin exhibited better properties, when tested in hot-wet conditions in a heated oven at 366 K (after boiling the material for 2 h in demineralized water), than the tetrafunctional resin. Improved impact resistance was observed with the addition of the reactive rubber to the epoxy resin. Further improvement was observed with the addition of the brominated epoxy resin.
Gilwee, W. J.↗