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Eingeladener Vortrag
- nein (149)
The demands for modern flame retardants are higher than ever: a flame retardant must function effectively in a certain polymer matrix and avoid critical alterations to the material’s properties. Ideally, a flame retardant additive should be easily miscible and show no sign of leaching or blooming from the matrix. Additionally, the flame retardant should be non-toxic, non-accumulating and biocompatible. Hyperbranched polymers are a promising group of multifunctional flame retardants which fulfill these demands: their complex shape enables high miscibility and avoids leaching or blooming, while their high molecular weight potentially increases biocompatibility and lowers accumulation and toxicity. Moreover, they exhibit a low impact on polymer properties and a good flame retardant performance.
This work examines the efficacy and mode of action of phosphorus-based hyperbranched polymeric flame retardants in bisphenol A-based epoxy matrices. To investigate the effect of the complex shape, the hyperbranched polymers are compared to their corresponding monomeric variants. Furthermore, the materials are synthesized to contain systematically varying oxygen-to-nitrogen ratios, allowing for new insight into what role the chemical surrounding of phosphorous plays in flame retardant efficacy.
Using a multi-methodical approach, including thermogravimetric analysis coupled with Fourier transform infrared spectroscopy (FTIR), hot stage FTIR, micro combustion calorimetry, differential scanning calorimetry, oxygen index (LOI), UL-94 tests and cone calorimetry experiments, the decomposition mechanisms and the flame retardant modes of action of these flame retardants in epoxy resins are investigated, shedding new light on the chemistry of flame retardancy.
Benefits of hyperbranched structure:
Molecular weight, miscibility, number of FR groups, end-group functionalization, glass transition temperature, decreased PBT.
Examples of hyperbranched FRs:
Charring agent, silicone, triazine, etc.
Systematic study of effect of chemical surrounding and impact of Complex shape of phosphorus-based hyperbranched polymers on flame retardant efficacy in epoxy resins.
Most synthetic polymers have a high fire load, and as a result, they require flame retardants (FRs) to ensure their safe use. Phosphorus plays an important role in flame retardancy and has the potential to replace halogenated variants, which are assumed to be harmful to the environment and health. Among phosphorus-based FRs, there exists a trend towards polymeric, high molar mass molecules with complex molecular architectures. In this project, we synthesized a novel series of so-called phosphorus-based hyperbranched polymeric FRs and investigated their use as multifunctional additives to high-performance polymers, i.e. epoxy resins. By cleverly designing the chemical structure to contain varying amounts of P-O and P-N bonds, new insight into the chemical mechanism of flame retardancy was gained, and by comparing the hyperbranched polymers to their monomeric counterparts, a greater understanding of the role of complex architecture was won. This talk aims at presenting some of these results and proposes chemical mechanisms that illustrate what role these novel hyperbranched flame retardants play in molecular firefighting.
The need to develop effective flame retardants that retain polymer properties and are safe for consumers and the environment is a continuous challenge for material scientists. While halogenated flame retardants were once commonplace, the shift to non-halogenated materials has steadily progressed due to concerns over impact on health and the environment. One prominent group of flame retardants has become a viable alternative for halogenated materials, namely phosphorus-based flame retardants. The chemical versatility of phosphorus-based flame retardants and the ability to work as reactive or additive compounds makes them ideally suited for modern materials. There exists a trend toward complex, polymeric, and multifunction flame retardants, as these materials show greater flame retardancy performance than low molecular weight counterparts and affect material properties to a much lesser extent.
One group of organophosphorus flame retardants that shows great potential for high-performance polymers like epoxy resins are hyperbranched phosphorus-based polymers. These additives exhibit great miscibility with the polymer matrix and a significantly decreased diffusion through the material, which greatly reduce leaching or blooming out of the matrix. Moreover, the material’s thermal stability remains intact at elevated temperatures due to its low impact on the glass transition temperature. Finally, following market trends and legislation such as the guidelines for the Restriction of Hazardous Substances Directive implemented by REACH (Registration, Evaluation, Authorization and Restriction of Chemicals) in the EU, these macromolecules are non-accumulating, non-toxic and have a lower risk of leeching or blooming from the matrix, further reducing environmental impact.
The work presented herein focusses on two distinct parts studying hyperbranched polymeric flame retardants and their corresponding monomeric compounds.
The first part, involving the low molecular weight components, investigated the role of the chemical surrounding of phosphorus in terms of flame retardant efficacy. Here, a systematic variance of the surrounding of phosphorus was investigated: by changing the ratio of oxygen to nitrogen (4:0 until 1:3), four materials, namely phosphoester (4:0), phosphoramidate (3:1), phosphorodiamidate (2:2), and phosphoramide (1:3), were synthesized, characterized, and finally added to Bisphenol A based epoxy resins (10 wt.-% loading). Pyrolysis investigations showed that low molecular weight components volatize at lower temperatures than the polymer matrix. Additionally, cone calorimeter measurements and TGA-FTIR investigations show trends in respect to FR efficacy in pyrolysis and full flaming conditions.
The second part involves the hyperbranched variants of the monomeric counterparts and investigates the role of complex shape on flame retardant efficacy. By comparing the low to the high molecular weight compounds, the influence of the complex shape becomes apparent and can be quantified. Cone calorimeter measurements show an increase in flame retardancy for some materials, while for others, the mode of action is altered.
By implementing a multi-methodical approach, various flame retardancy aspects, from pyrolysis behavior in the gas and condensed phase, to ignitability / reaction-to-small-flame performance, to action in forced flammability experiments, are identified and quantified, allowing for a clearer understanding of the behavior in fire of these novel flame retardants. By comprehending the roles of chemical composition and complex shape, it opens the path for new and effective multifunctional, polymeric flame retardants with decreased PBT, higher miscibility, and low impact on Tg.
This work is funded by the Deutsche Forschungsgemeinschaft (DFG: SCHA 730/15-1; WU 750/8-1).
We are interested in accidental fire impingement of HazMat pressure vessels. Want to develop improved models for predicting time to failure or empty (if PRV present). We are still trying to properly predict pressurization and time to first PRV activation due to liquid temperature stratification for a range of fire scenarios (Full and partial engulfing pool fire, jet fires, with roll over, with TP defects, etc.)
The interest in hydrogen-based green energy is increasing worldwide, and the same is true for hydrogen-powered vehicles. Among the possible solutions to store hydrogen in such vehicles, cryogenic tanks equipped with multi-layer insulation (MLI) are the most promising to increase the amount of energy stored per unit volume. However, MLI is affected by severe deterioration when exposed to an external source of heat such as a fire following a car accident, leaving the tank unprotected and leading to failure in a relatively short time. In this work, a one-dimensional model to evaluate MLI thermal degradation when a liquid hydrogen tank is exposed to fire is presented. The relevance of taking MLI degradation into account when simulating the pressure increase due to external fire exposure is here demonstrated through the analysis of several case studies. The results show that MLI systems performance depletes within a few minutes of exposure to hydrocarbon poolfire.
Bare steel constructions are often integrated in modern buildings. Intumescent coatings are widely used to protect the steel from heating up too quickly in a case of fire. As the functionality of intumescent coatings decreases with the impact of weathering processes, it is important to understand the mechanisms of material degradation to maintain long durability. The weathering-induced degradation behavior of a water-borne intumescent coating was examined, and the weakest points of the formulation were identified by a systematic approach. Resulting from this investigation, adjustments to the formula were made, leading to improved weathering resistance.
Revolutionizing our polymer industry for adaption to a sustainable carbon circular economy has become one of today’s most demanding challenges. Exploiting renewable resources to replace fossil-fuel—based plastics with biopolymers such as poly(lactic acid) (PLA) is inevitable while using waste streams as a raw material resource at least is promising. When it comes to using PLA as technical polymer, its high flammability must be addressed by flame retardants compatible with the thermoplastic processing of PLA and its compostability. This study proposes microalgae enriched with phosphorus from wastewater (P-Algae) as an elegant way towards a kind of sustainable organophosphorus flame retardant. The concept is demonstrated by investigating the processing, pyrolysis, flammability, and fire behavior of PLA/P-Algae, while varying the P-Algae content and comparing P-Algae with four alternative bio-fillers (phosphorylated lignin, biochar, thermally treated sewage sludge, and metal phytate) with different P-contents as meaningful benchmarks.
Wasserstoff wird als ein potenzieller alternativer Energieträger gesehen, mit dem die für 2050 gesetzten Klimaziele erreicht werden könnten. Der Transport von Wasserstoff ist mittels verschiedener Speichertechniken möglich, von denen der kryogene Transport mit den größten volumetrischen Energiedichten einhergeht. Hierdurch eignen sich diese Speicher besonders für die energieintensiven Verkehrsmittel im Land-, See- und Flugverkehr.
Im Vortrag werden Speichertechniken, Gefahren im Umgang mit kryogenen Gasen sowie bisherige Störfälle dargestellt. Darauf aufbauend wird ein Teil der aktuellen Forschungsarbeit an der BAM vorgestellt, die die Sicherheit dieser Speicher unter außergewöhnlichen Belastungen adressiert.
Basierend auf Methan aus regenerativen Quellen, stellt LNG einen alternativen Kraftstoff für den schweren Fernverkehr da. Gegenüber seinen positiven Eigenschaften birgt der Kraftstoff aber auch Risiken, durch seine sehr niedrige Temperatur und seine Brennbarkeit, für die Personen- und Bauwerkssicherheit. Für die Erforschung der Risiken eignen sich CFD-Modelle, deren Erforschung unter anderem Ziel des TF-SiVi Projekts der BAM war.
Einen Einblick in die angewendete Methodik zur Erforschung von Unfallszenarien mit LNG gibt der Vortrag.
Liquefied Natural Gas (LNG) aus regenerativen Quellen, stellt einen potenziellen Kraftstoff für den Schwer- und Fernverkehr des Straßenverkehrs dar. Gegenüber seinen positiven Eigenschaften zu dem in diesem Verkehrssektor häufig verwendeten Kraftstoff Diesel birgt der Kraftstoff aber auch Gefahren für Personen und Bauwerke durch seine sehr niedrige Temperatur bei der Speicherung von ca. -160 °C und seine Explosionsfähigkeit in der Gas-Phase. In der Arbeit wurde sich mit der Gefährdung von Personen und Bauwerken hinsichtlich der von LNG ausgehenden Gefahren in Tunneln auseinandergesetzt.
Tunnel stellen besonders schützenswerte Bauwerke dar, da aus vorhergehenden Störfällen in Tunneln bekannt ist, dass diese mit hohen Personen-, Bauwerks-, und Volkswirtschaftlichen-Schäden einhergehen können.
Untersuchungsschwerpunkt bei der Bewertung von Gefährdungen durch LNG stellte eine Ereigniskaskade bestehend aus Freisetzung, Verdampfung, Stoffausbreitung und Zündung des sich gebildeten explosionsfähigen LNG-Gas/Luft-Gemisches dar. Mit dem Ziel eine solche Ereigniskaskade realitätsnah vorhersagen und zukünftig hierzu Risikoanalysen durchführen zu können wurden innerhalb der Arbeit Parameterstudien sowie Kalibrierungen und Validierungen gegenüber experimentellen Untersuchungen durchgeführt.
Mit den Modellen wurden in der Arbeit exemplarische Fallbeispiele zu Störfällen untersucht. Ergebnisse dieser waren, dass Gefährdungen insbesondere von flüssigem LNG nach dessen Freisetzung und der Verbrennung von LNG-Gas/Luft-Gemischen ausgingen.zeige weniger
Der Markt von LNG als Transportgut und als Kraftstoff ist seit Jahrzehnten kontinuierlich am Wachsen, wobei das Hauptanwendungsgebiet im Schiffsverkehr lag. LNG ist verflüssigtes Erdgas mit Hauptbestandteil Methan, das neben fossilen, aus erneuerbaren Quellen, wie synthetischen Methan oder Biogas, gewonnen werden kann. LNG hat als Kraftstoff sehr gute Eigenschaften dessen Potenzial als alternativer Kraftstoff zu Diesel im Schwerlast- und Fernverkehr gesehen wird. Dabei weist LNG gegenüber Diesel geringere Emissionen von CO2, Feinstaub, Stickoxiden und Lärm auf und hat gegenüber anderen erneuerbaren Energiespeichern wie CNG, Elektrobatterien oder Wasserstoff die höchste volumetrische und zweitgrößte gravimetrische Energiedichte. Neben seinen Vorteilen zu anderen erneuerbaren Energieträgern birgt LNG durch seine sehr niedrige Temperatur von bis zu 160°C und seiner Brennbarkeit aber auch neue Gefahren für Personen und Infrastrukturen.
Zur Bewertung von Gefahren und zur späteren Durchführung von Risikobewertungen bedarf es Methoden und Modellen deren Untersuchung Ziel des Forschungsprojekts war. Schwerpunkt der Untersuchung stellt die Freisetzung von LNG in Tunnel, mit sich anschließender Stoffausbreitung und verzögerter Zündung des Kraftstoff-Luftgemisches dar. Unfallszenarien mit Brandereignissen in Tunnel haben gezeigt, dass diese meist mit hohen Personen, Bauwerks und volkswirtschaftlichen Schäden verbunden sind. Des Weiteren zeigten Untersuchungen das von Gasexplosionen in Umschließungen wie sie ein Tunnel darstellt, mehr Gefahren ausgehen als von Gasexplosionen im Freifeld.
Im Vortrag werden die untersuchten Modelle und die aus dem Projekt gewonnenen Erkenntnisse für die Stoffausbreitung und Verbrennung der Gasphase von LNG in Umschließungen vorgestellt.
Liquefied Hydrogen (LH2) or Liquefied Natural Gas (LNG) establish themselves as important energy carriers in the transport sector. Its storage requires tanks with Thermal Super Insulations (TSI) to keep the transported fluid cold. The presentation includes 2 main topics of the department.
First TSI has proven itself in various applications over a long time, but not in the land transport sector, where accidents involving collisions, fires, and their combination are to be expected. To analyze fire scenarios a High-Temperature Thermal Vacuum Chamber (HTTVC) was developed that allows the thermal loading of thermal insulation material in a vacuum and measuring the heat flow through the TSI in parallel. Within this chamber, 5 samples were tested regarding 3 different types of MLI, rock wool, and perlites. In the presentation, the results are presented.
Second, the studying of accident scenarios enables the improvement of thermal superinsulation and to find novel insulation concepts. This is necessary for LH2 large-scale storages, for which state-of-the-art solutions are not suitable. Within the presentation, a novel insulation concept will be presented.
The importance of tanks for storing cryogenic fluids in the energy industry is increasing because of ongoing political conflicts and the implementation of more environmentally friendly energy sources. Key representatives for the application of cryogenic tanks are natural gas in the form of Liquefied Natural Gas (LNG) and hydrogen, e. g. in the form of Liquefied Hydrogen (LH2), for which significantly higher transport capacities can be achieved with the same transport volume using cryogenic storages than with storages based solely on overpressure.
What applies to all cryogenic transported fluids in common is their condition that must be maintained. Hence heat flows into the preserved fluid must be minimized. Thermal super Insulations (TSI) based on e. g. multilayer insulations (MLI), perlites, and vacuum are utilized for this purpose and have already proven themselves in similar applications. However, for the use of tanks for cryogenic fluids in the transport sector, there is insufficient knowledge regarding the course and consequences of incidents, which is due to the still short period of use and the few documented incidents, hence few investigations carried out in this field. Typical scenarios in the transport sector represent car accidents with collisions, fires, and their combination, which are associated with extraordinary loads on the tank.
The focus of this study is to investigate the behavior of TSI as a result of their thermal exposure to a heat source representing a fire. It is worth mentioning that this could lead to an increase of the heat flux into a tank by several orders of magnitude, and to permanent damage of the TSI, ultimately rapid release of flammable gas as well as a Boiling Liquide Expanding Vapour Explosion (BLEVE). For this purpose, a high temperature thermal vacuum chamber (HTTVC) has been developed that allows thermal loading of MLI or perlites in a vacuum and simultaneous measurement of heat flow through this TSI. The HTTVC is designed to represent realistic insulation conditions and to withstand thermal loads from typical design fires.
The HTTVC was applied to investigate TSI based on MLI and vacuum. It is shown that the thermal stress caused permanent damage to the TSI, with shrinkage, phase change, pyrolysis, and condensation being significant damage mechanisms. The results are relevant for the evaluation of accident scenarios and can thus contribute to the improvement of TSI and the development of emergency measures for the protection of persons and infrastructures.
Vorgestellt wird ein 2018 gestartetes Projekt zur Überprüfung der Extrapolation von im Labormaßstab ermittelten Selbstentzündungstemperaturen auf technisch relevante Volumina. Für die Ermittlung reaktionskinetischer Daten von Feststoffschüttungen stehen eine Reihe von Untersuchungsmethoden zur Verfügung. Dies sind thermische Analysen wie z.B. die differential scanning calorimetry DSC sowie Mikrokalorimetrie zur hochgenauen Messung von Wärmeströmen, bei denen sehr geringe Probenmengen zum Einsatz kommen. In der Regel wird das Selbstentzündungsverhalten jedoch mit Hilfe von isoperibolen oder adiabaten Warmlagerungsversuchen beurteilt, hier liegen die Probenvolumina üblicherweise im Bereich von ca. 100 cm³ bis zu einigen Litern. Die Extrapolation über mehrere Größenordnungen auf technische Volumina birgt Unsicherheiten, da mit Zunahme des Lagervolumens veränderte Start- und Randbedingungen vorliegen können. Zudem besteht die Möglichkeit, dass bei in technischen Lagern vorherrschenden niedrigen Temperaturen Reaktionen ablaufen, die in Standard- Laborversuchen nicht erfasst werden aber einen wesentlichen Einfluss auf das Selbstentzündungsverhalten aufweisen können. Hauptziel des Projektes ist es daher, die im Labormaßstab vorhandenen Prüfeinrichtungen durch einen Versuchsstand zur Untersuchung von Probengrößen von bis zu 1000 dm³ zu erweitern, die Eignung (oder Nichteignung) der etablierten Methoden nachzuweisen und im Labormaßstab nicht erfassbare Einflussgrößen zu ermitteln. Zudem sollen anhand der kleinskaligen Tests Entscheidungskriterien abgeleitet werden, ob eine Extrapolation nach den derzeit üblichen Methoden zulässig ist.
Accident safe packages for the transport of spent nuclear fuel and high-level waste shall fulfil international IAEA safety requirements. Compliance is shown by consecutive mechanical and thermal testing. Additional numerical analysis are usually part of the safety evaluation. For damage protection some package designs are equipped with wood filled impact limiters encapsulated by steel sheets.
The safety of these packages is established in compliance with IAEA regulations. Cumulative mechanical and fire tests are conducted to achieve safety standards and to prevent loss of containment. Mechanical reliability is proven by drop tests. Drop testing might cause significant damage of the impact limiter steel sheets and might enable sufficient oxygen supply to the impact limiter during the fire test to ignite the wood filling. The boundary conditions of the fire test are precisely described in the IAEA regulatory. During the test the impact limiter will be subjected to a 30 minutes enduring fire phase. Subsequent to the fire phase any burning of the specimen has to extinguish naturally and no artificial cooling is allowed.
At BAM a large-scale fire test with a real size impact limiter and a wood volume of about 3m³ was conducted to investigate the burning behaviour of wood filled impact limiters in steel sheet encapsulation. Until today burning of such impact limiters is not sufficiently considered in transport package design and more investigation is necessary to explore the consequences of the impacting fire. The objective of the large scale test was to find out whether a self-sustaining smouldering or even a flaming fire inside the impact limiter was initiated and what impact on the cask is resulting.
The amount of energy transferred from the impact limiter into the cask is of particular importance for the safety of heavy weight packages. With the intention of heat flux quantification, a new approach was made and a test bench was designed.
Renewable alternatives for common thermoset resins are demanded to go for sustainability. The objective is to create a flame retarded epoxy resin from a commercial bio epoxy resin with halogen free inorganic and organic flame retardants, respectively. Alumina trihydrate, aluminum diethyl phosphinate, a DOPO-based phosphonamidate and ammonium polyphosphate seem to have promising performances. Properties are enhanced with different bio fillers: pyrolyzed cocoa shells and plant waste (provided by Otto A. Müller Recycling GmbH, thanks!), short fibers and nonwovens of the natural fiber kenaf, hydroxypropyl-ß-cyclodextrin and sulfobutylether-ß-cyclodextrin.
Fire performance is investigated by cone calorimeter examinations, LOI and UL-94 ratings. Thermal analysis is given by TG-FTIR and DSC measurements.
Combinations of flame retardants and bio-fillers lead to reduced PHRR and THR, reach V0 in UL-94 and have a significant increase in LOI of up to 37 vol.-%. 10 % ammonium polyphosphate with 10 % pyrolyzed cocoa shell performs best, builds a magnificent protective layer, and shows good intumescence.
The work aims to assess the textile reinforced concrete at elevated temperatures and applications of additional fire protection as well.