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In this study, multicomponent flame retardant systems, consisting of Ammonium polyphosphate (APP), aluminum trihydroxide (ATH), and polyaniline (PANI), were used in ethylene propylene diene monomer (EPDM) rubber. The multicomponent system was designed to improve flame retardancy and the mechanical properties of the rubber compounds, while simultaneously reducing the amount of filler. PANI was applied at low loadings (7 phr) and combined with the phosphorous APP (21 phr) and the mineral flame retardant ATH (50 phr). A comprehensive study of six EPDM rubbers was carried out by systematically varying the fillers to explain the impact of multicomponent flame retardant systems on mechanical properties. The six EPDM materials were investigated via the UL 94, limiting oxygen index (LOI), FMVSS 302, glow wire tests, and the cone calorimeter, showing that multicomponent flame retardant systems led to improved fire performance.
In cone calorimeter tests the EPDM/APP/ATH/PANI composite reduced the maximum average rate of heat emission (MARHE) to 142 kW·m-2, a value 50% lower than that for the unfilled EPDM rubber. Furthermore, the amount of phosphorus in the residues was quantified and the mode of action of the phosphorous flame retardant APP was explained. The data from the cone calorimeter were used to determine the protective layer effect of the multicomponent flame retardant systems in the EPDM compounds.
The impact of polyaniline in phosphorus flame retardant ethylene-propylene-diene-rubber (EPDM)
(2019)
Usually elastomers are loaded with high amounts of flame retardants to fulfill fire safety requirements. In this study the potential char precursor polyaniline (PANI) and the established fire retardant pentaerythritol (PER) were implemented in ethylene-propylene-diene monomer rubber (EPDM). PANI and PER were used in low loadings (7 phr) and combined with two phosphorous flame retardants, Ammonium polyphosphate (APP) and a piperazine-pyrophosphate/phosphoric acid compound (FP), to boost their performance. A comprehensive study is presented, explaining the impact of PANI on curing and mechanical properties, including compensation for the plasticizer-like effect of APP in EPDM, and improved flame retardancy. In the cone calorimeter test, the combination of EPDM/FP/PANI reduced the effective heat of combustion by 20%. All nine EPDM rubber compounds were investigated with the LOI and UL 94 tests, cone calorimeter, FMVSS 302 and glow wire testing to quantify fire performance. The PANI containing EPDM rubbers, EPDM/APP/PANI and EPDM/FP/PANI outperformed the corresponding PER containing, EPDM/APP/PER and EPDM/FP/PER rubbers in various tests. Moreover, the study investigated the impact of PANI and PER on the mode of action of the phosphorus species and showed that the addition of PANI increased the amount of phosphorus in the condensed phase. To receive a broader understanding of the flame retardant mode of action of PANI in combination with APP and FP, calculations were carried out to estimate the impact of PANI on the protective layer effect.
Alkali-silica reaction (ASR) is a serious Problem concerning the deterioration of concrete. This leads to significant maintenance and reconstruction costs for concrete infrastructures all over the world. The geographical regions, which play a major role in concrete deterioration, are for example coastal Areas or in general, areas with a high air humidity/salinity due to closeness of rivers or lakes.
These exemplary results show, the application of Raman spectroscopy establishes a valuable approach for characterizing the chemical and structural composition of ASR-products. The results prove the potential to trace the kind of reaction products, developing in dependence on the aggregate and to follow up its local alteration from origin of the gel.
Developing halogen‐free flame retardants with reasonably high efficiency, which thus function at limited loadings in polypropylene‐based wood/plastic composites (WPC), is still a challenge. Cost‐effective flame‐retarded WPC have been identified as a way to open the door to an interesting, broader spectrum of application in the building and transportation sectors. This work imparts a systematic comprehensive understanding and assessment of different basic routes to halogen‐free flame‐retarded WPC, taking into account economic and environmental considerations. Cheap, halogen‐free single‐component flame retardants and their multicomponent systems are investigated at reasonable filling grades of 20 wt%. The basic routes of promising synergistic multicomponent systems are discussed, and their potential and Limits assessed. Optimizing the consistency of fire residue; closing the surface of inorganic‐organic residual layers; the thermal stabilization and design of the residue, eg, synergistic combination of ammonium polyphosphate and expandable graphite; and the combination of different flame‐retardant mechanisms, eg, intumescence and flame inhibition, are proposed as promising routes to boost the flame‐retardant efficiency.
Superglassy polymers with a large fractional free volume have emerged as novel materials with a broad range of applications, especially in the field of membrane separations. Highly permeable addition-type substituted polynorbornenes with high thermal resistance and chemical stability are among the most promising materials. The major obstacle for extending the practical membrane application is their strong tendency to physical aging, leading to a partial decline in their superior transport performance over time. In the present study, broadband dielectric spectroscopy with complementary X-ray scattering techniques were employed to reveal changes in microporous structure, molecular mobility, and conductivity by systematic
comparison of two polynorbornenes with different numbers of trimethylsilyl side groups. Their response upon heating (aging) was compared in terms of structure, dynamics, and charge transport behavior. Furthermore, a detailed analysis of the observed
Maxwell−Wagner−Sillars polarization at internal interfaces provides unique information about the microporous structure in the
solid films. The knowledge obtained from the experiments will guide and unlock potential in synthesizing addition-type polynorbornenes with versatile properties.
Polymers of Intrinsic Microporosity (PIMs) of high performance have developed as materials with a wide application range in gas separation and other energy-related fields. Further optimization and long-term behavior of devices with PIMs require an understanding of the structure-property relationships including physical aging. In this context the glass transi-tion plays a central role, but with conventional thermal analysis a glass transition is usually not detectable for PIMs be-fore their thermal decomposition. Fast scanning calorimetry provides evidence of the glass transition for a series of PIMs, as the time scales responsible for thermal degradation and for the glass transition are decoupled by employing ultrafast heating rates of tens of thousands K s-1. The investigated PIMs were chosen considering the chain rigidity. The estimated glass transition temperatures follow the order of the rigidity of the backbone of the PIMs.
Polymeric membranes represent a low-cost, energy efficient solution for gas separation. Recently polymers of intrinsic microporosity (PIMs) have emerged as prestigious membrane materials featuring a large concentration of pores smaller than 1 nm, a BET surface area larger than 700 m2/g and high gas permeability and selectivity. Unusual chain structure combining rigid segments with sites of contortion gives rise to the intrinsic microporosity. However, this novel class of glassy polymers are prone to pronounced physical aging. The initial microporous structures approach a denser state via local small scale fluctuataions, leading to a dramatic reduction in the gas permeabilities. For the first time, dielectric relaxation spectroscopy with state-of-the-art high-resolution analyzers was employed to investigate three representative PIMs with a systematic change in chain rigidity: PIM-EA-TB 〉 PIM-1 〉 PIM-MDPH-TB. The molecular mobility, the charge transport and their response upon heating (aging) in the polymers were measured in a broad temperature range through isothermal frequency scans during different heating / cooling cycles. Multiple dielectric processes following Arrhenius behavior were observed for the investigated polymers. Local fluctuations, Maxwell-Wagner-Sillars (MWS) polarization and structural relaxation phenomena were discussed and attempted to be correlated with the structural features of PIMs. Moreover, all PIMs showed conductivity in the glassy state. The significant increase in the conductivity with increasing temperature far below the glass transition temperature of PIMs is explained in terms of the loosely packed microporous structure and the formation of local intermolecular agglomerates due to interaction of π-electrons in aromatic moieties of the polymer backbone.
High performance polymers of intrinsic microporosity (PIMs) have emerged as novel materials with broad applications from gas separation to electronic devices. Sufficiently rigid, even contorted polymer chains show only limited molecular mobility, therefore undergo inefficient packing and give rise to intrinsic microporosity with pore size generally smaller than 1 nm and BET surface areas larger than 700 m2/g. Further performance optimization and long-term stability of devices incorporating PIMs rely on our understanding of structure-processing-property relationships and physical aging, in which glass transition plays a key role. Up to now no glass transition temperature (Tg) of PIMs could be detected with conventional thermal analysis techniques before degradation. Decoupling the time scales responsible for the glass transition and the thermal decomposition is a reliable strategy to overcome this. This was achieved by employing fast scanning calorimetry (FSC) based on a chip sensor, which is capable to heat and cool a small sample (ng-range) with ultrafast rates of several ten thousand K/s. FSC provides definitive evidence of glass transition of a series of PIMs with a special consideration on the chain rigidity. The determined glass transition temperature of these PIMs follows the order of the rigidity of their backbone structures. FSC provides the first clear-cut experimental evidence of the glass transition of PIM-EA-TB with a Tg of 663 K, PIM-1 of 644 K and PIM-DMDPH-TB of 630 K at a heating rate of 1Χ104 K/s. Local fluctuations are featured in glass transition of highly rigid PIMs. As conformational changes are prevented by the backbone rigidity, the glass transition must rather be assigned to local small scale fluctuations.
For the purpose of increasing payload and reduce freight cost, lightweight composite tank containers used for Transportation have been progressively developed during the last years. Compared to conventionally produced cylindrical steel tanks, the fiber-reinforced solutions allow greater flexibility in the tank design. Despite a number of further material-related benefits of fiber-reinforced composites as non-conductive and non-magnetic behavior as well as corrosion resistance and high strength, the optimization of their thermal degradation properties during combustion is still a challenge. To improve the fire performance of lightweight composite containers, special intumescent fire protection coatings can be applied onto the outside tank surface. This paper presents fire tests on glass-fiber-reinforced plastic transport tanks with complex geometries sheltered with different surface-applied fire protection systems. To evaluate the fire resistance of the tank structures, a fiber optic monitoring system was developed. This system is based on distributed temperature measurements using high-Resolution optical backscatter reflectometry and pointwise reference measurements using fiber Bragg gratings. Thereby, all the fiber optic sensors were directly integrated in the composite layer structure of the tanks. The focus of the presented work is on the demonstration of capability of fiber optic monitoring system in such high-temperature application. Moreover, the fiber optic measurements provide new insights into the efficiency of intumescent coating applied for fire protection of fiber-reinforced plastic transport tanks.
Für Bauteile (Komponenten) von Versorgungsanlagen für flüssige Brenn- und Kraftstoffe muss die Beständigkeit der metallenen Werkstoffe und Polymere nachgewiesen werden. Im Anwendungsfall von Heizöl mit 20 % biogenen Anteilen in Form von Rapsölfettsäuremethylester (FAME, Biodiesel) ist es für eine konservative Beurteilung des Korrosionssystems Werkstoff/Medium/Umgebung wichtig, die Alterungseffekte des Mediums einzubeziehen.
Entwicklung eines Prüfverfahrens für die Untersuchung der Beständigkeit von metallenen Werkstoffen und Polymeren in Heizöl und Heizöl-FAME-Blends, das für eine Vorauswahl der Werkstoffe und zum Nachweis der Beständigkeit im Hinblick auf die bauaufsichtlichen Zulassungsverfahren geeignet ist. Ein Schwerpunkt wird bei den metallenen Werkstoffen auf der Erprobung von Messmethoden liegen, mit denen sich in kurzer Versuchszeit ein Korrosionsangriff detektieren lässt.
Metallene Werkstoffe:
Weder örtliche Korrosion noch erhöhte Flächenkorrosion (Korrosionsrate:< 0,1 m/Jahr) sind bei den bisher geprüften Werkstoffen: Aluminium,
C-Stahl 1.0037, austenitischer CrNi-Stahl 1.4301, Kupfer und Messing in Heizöl und B20 (Heizöl mit 20% Biodiesel) aufgetreten. Diese Werkstoffe sind in den Prüfmedien Heizöl und B20 als beständig zu bewerten.
Es wurde keine signifikante Veränderung des pH-Wertes der Prüfmedien gemessen.
Polymere:
Massebestimmung:
Die Prüfkörper der Elastomere ACM, HNBR und PUR sowie in geringerem Maße PE neigten zur Quellung in Heizöl und B20 nach 42 d und 84 d Auslagerung; für PA 6, POM und PVC wurde keine Masseänderung gemessen. Die Masseänderung der Prüfkörper in Heizöl und B20 ist mit Ausnahme von PUR vergleichbar. Bei PE traten Verfärbungen durch die Brennstoffe auf.
Zugeigenschaften:
ACM, HNBR, PE und PVC sind in Heizöl und B20 beständig, da die Änderung der Zugfestigkeit und der Reißdehnung < 15 % beträgt. PA und POM sind bedingt beständig, da die Änderung der Zugfestigkeit und der Reißdehnung < 30% beträgt.