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Paper des Monats
- ja (7)
Although numerous investigations study the improvement of flame retardancy of epoxy resins using additives, maintaining the flame retardant (FRs) modes of action present in the resins upon transfer to composites is challenging. In this study, ammonium polyphosphate (APP) and inorganic silicate (InSi) are loaded at 10%, 30%, and 50% by weight, in a diglycidyl ether of bisphenol A (DGEBA) resin cured with dicyandiamide and transferred to bidirectional (BD) glass fiber (GF) composites. Although a 50% loading of the FRs impacts the curing kinetics of the resin system, the effect on the glass transition temperature of the resin system remains negligible compared to reactive FRs in the state of the art integrated into the resin's chemical structure. Increasing the FR content improved the heat release characteristics in both the resins and composites. However, the charring mode of action is completely suppressed in the formulation with 10% APP + InSi. A 30% concentration of the FRs restored the charring action in the composite and the GFs provide increased protective layer action upon transfer to the composites. This study highlights the importance of accounting for the changing dynamics related to processing and flame retardancy upon transferring FRs from resins to composites.
INTRODUCTION: Most polymeric materials in most fire scenarios burn based on an anaerobe pyrolysis feeding the flame with fuel. Understanding the thermal decomposition in the condensed phase is key to tailor flame retardancy. Adjusting the decomposition temperature of flame retardant and polymer as well as providing the desired chemical structure for specific reactions determine the molecular mechanisms and thus the flame-retardant modes of action. Hereby, it is not only charring in the condensed phase and radical scavenging in the gas phase, but also physicochemical and physical effects such as melt flow and protective layer formation. This paper delivers thought-provoking impulses on how the understanding of the pyrolysis can be used for evidenced-based development and optimization of flame-retardant polymeric materials. Some rather overseen details are picked up as well as rethinking of concepts memorized long ago is encouraged to discover something new. The talk tries to fill some gaps between flame-retardant mechanisms, flame-retardant modes of action, and fire performance.
EXPERIMENTAL: Materials - This paper deduces its conclusions from results of several research projects performed in the working group of the author. For a detailed description of the materials, their compounding, and the preparation of test specimens please go for the comprehensive description in the original papers.[1-10]
Methods - A multi-methodical approach based on thermogravimetry (TGA), TGA coupled with evolved gas analysis (TGA-FTIR), hot stage FTIR, pyrolysis GC/MS, and residue analysis was used for investigating the pyrolysis. The flammability in the fire scenario ignition was addressed using oxygen index (OI) and testing in the UL 94 burning chamber. The fire behaviour in developing fires was investigated using a cone calorimeter. Additional efforts complete the studies, such as other fire tests, advanced analysis of the fire residue, melt rheology, or particle finite element simulations (PFEM). Tailored and self-designed experiments and advanced data evaluation described fire phenomena or modes of action. For a detailed description of the experimental the reader is relegated to the original papers.[1-10]
RESULTS AND DISCUSSION: One important aspect in achieving, adjusting, and optimising flame retardancy is exploiting specific chemical reactions in the condensed phase between the pyrolyzing polymer and the flame retardant at the right place, time, and temperature.[1-3] At the same time, these reactions of partly decomposed or hydrolysed flame retardants in the condensed phase competes with releasing as volatile into the gas phase. Based on three comparisons this field is illuminated in detail: reactive phosphine oxide, phosphinate, phosphonate, and phosphate are compared in the same epoxy resins evaluating the influence of the oxidation state,[1] different phosphorous flame retardants in different epoxy resins underlining the specific reactions between the partly decomposed or hydrolysed flame retardant and the partly decomposed polymer,[3] and the comparison of three aryl phosphates with different volatility highlights the competition of chemical reaction in the condensed phase and gasification.[2]
Any fire residue reduces fire risks, when the release of hydrocarbon fuel into the gas phase is replaced by storing fuel in the condensed phase as carbonaceous char. Thus, charring describing crosslinking, dehydration, aromatization, and graphitization is the flame retardancy mechanisms, whereas charring describing the reduction in fire load the flame-retardant mode of action. The phenomenon charring belongs to a complete pyrolysis or complete pyrolysis step; the char yield indicates the amount of fuel stored in the residue. Further, any fire residue works as protective layer. The barrier properties depend on the physical properties of the residue but not necessarily on its amount.[4] Usually, a residue design such as a tailored morphology of the fire residue is demanded. The mass loss rate and heat release rate are reduced. The main mechanisms are heat shielding and thermal insulation.[5] Sometimes the protective layer is good enough to cause incomplete pyrolysis due to extinguishing before the pyrolysis front went through the whole sample.[6.7] Analogous to charring also incomplete pyrolysis can result in efficient reduction in fire load. Proper data evaluation and key experiments are used to sort out and understand these different phenomena. Flame retardant polyurethane foams passing the heat release and smoke toxicity requirements of EN 45545 are discussed as evidence-based development using charring and incomplete pyrolysis due to an efficient protective layer.[7,8]
The thermal decomposition into liquid intermediate products increases crucially the melt flow during burning,[9] whereas charring and the ablation of the polymer matrix increasing the content of fillers yield melt viscosities enlarged by orders of magnitude.[10] Violent burning of some polymers at the end of a cone calorimeter test can be understood as pyrolysis enabling a pool fire. The understanding of the thermal decomposition of the polymeric material harbours the explanation of non-flaming dripping extinguishing the flame via sufficient cooling, retreat effects preventing ignition, and efficient nondripping flame retardancy.
This paper leads the audience from chemistry over complex macroscopic fire phenomena of physicochemical nature to fire performance. Thought-provoking impulses are given how the scientific understanding of the pyrolysis in the condensed phase can be used for research and evidenced-based development of future flame-retardant polymeric materials.
Acknowledgement: The talk uses results from distinct projects; thus, thanks go to the German Research Foundation DFG SCHA 730/6-1, SCHA 730/8, SCHA 730/10-1, and Scha 730/19-1, Bayer MaterialScience AG, and the BMWi (BMWK) AiF: IGF No.: 19078 N/2 for financial support. Many thanks to former working group members U. Braun, Y. Y. Chan, B. Perret, S. Rabe, K. H. Richter, A. Weiß, and G. Wu, and to our co-operation partners A. Hartwig (IFAM), M. Döring and M. Ciesielski (at that time KIT), and J. M. Marti (CIMNE) as well.
Forschungsprojekt "INSIST"
(2024)
Der Vortrag zeigt den Bearbeitungsstand des Forschungsvorhabens "Entwicklung eines Verfahrens zur in situ Bewertung des Feuerwiderstands von bestehenden Stahlkonstruktionen mit reaktiven Brandschutzsystem (RBS)" (INSIST). Die Entwicklung und der Bau eines Geräteprototyps wurden vorgenommen und ein Konzept zur Kalibration erarbeitet. Die bisherigen Untersuchungen belegen, dass das Verfahren Ergebnisse liefert, die denen konventioneller Brandversuche im untersuchten Parameterbereich gleichwertig sind.
Innovation and scientific progress are often located in the synthesis of new flame retardants or in the compounding of new composites. Thus, although nearly everyone applies fire tests to ascertain the flame retardancy achieved, regular, cost-efficient fire testing is preferred, sometimes its reliability and meaningfulness are questioned. The goal of this revised chapter is to inspire the exploitation of the potential of fire testing beyond a soulless pass-and-fail or isolated number rating. Recommendations are given as to how fire behaviour can be investigated and how data can be evaluated faithfully and meaningfully. Backgrounds and benchmarks are discussed as thought-provoking impulses which could allow bench-scale fire testing to be exploited as a vital basis and powerful tool for science-based development.
Applying synergistic multicomponent systems is often key to efficient flame retardancy. Different flame retardants are combined or used together with fillers, adjuvants, or synergists to enhance their efficiency, reduce the worsening of other properties, or reduce the costs. Further, fibres and other reinforcing fillers contribute to fire properties crucially. Although the main flame-retardant modes of action are known, the scientific understanding usually falls short, when it comes to complex multicomponent systems, the crucial tiny optimizations, or quantifying in terms of specific fire properties. This book chapter illuminates the need for the multicomponent approach, the concept of synergistic flame retardants, and the main phenomena. Multicomponent systems are discussed in their capacity as general powerful strategy for achieving and optimizing future flame retardant polymeric materials.
This book presents the proceedings of the Thirteenth International Conference Structures in Fire. The conference took place at the Department of Civil Engineering, University of Coimbra, Portugal, from 19 to 21 June 2024, under the auspices of the SIF movement. Structural fire safety is a crucial aspect of the design of buildings and infrastructures. Significant advances in research have increased the knowledge on this topic. However, until the 1990s, there were few forums for structural fire engineers to exchange ideas and share research findings. SIF (Structures in Fire) specialised workshop series was conceived in the late 1990s and the “First International SIF Workshop” was held in Copenhagen, Denmark in 2000, followed by workshops in Christchurch, New Zealand (2002), Ottawa, Canada (2004) and Aveiro, Portugal (2006). The series of workshops evolved into conferences and the 2008 event in Singapore was the fifth International Conference on Structures in Fire. This was followed by events in East Lansing, USA (2010), Zurich, Switzerland (2012), Shanghai, China (2014), New Jersey, USA (2016), Belfast, UK (2018), Brisbane, Australia (2020) and Hong Kong, China (2022). Information about previous conferences, including complete proceedings, can be found at www.structuresinfire.com. The main mission of SIF conferences is to provide an opportunity for researchers and engineers from the global structural fire engineering community to participate, share and discuss the recent findings, innovations and developments with their peers in an open and international forum. Following the great success of the previous International Conferences, the University of Coimbra was selected to host the 13th International Conference on Structures in Fire. As with most of the recent conferences, the number of papers submitted far exceeds the number of papers that can be accommodated in the three-day programme, even with two parallel sessions. SIF 2024 received 249 abstracts before the deadline and accepted 172 abstracts after the review process by at least three reviewers from the scientific committee. These proceedings represent 132 full papers, collectively representing the state of the art in fundamental knowledge and practical application of structures in fire. Forty-two countries from around the globe have contributed to them. The papers are grouped into the following research topics: Applications of Structural Fire Engineering, Composite Structures in Fire, Concrete Structures in Fire, Timber Structures in Fire, Masonry Structures in Fire, Steel Structures in Fire, Experimental Research of Structures in Fire, Numerical Modelling of Structures in Fire, Other Topics Related to Structures in Fire. Finally, the Organizing Committee would like to thank the continuous support from the SIF Steering Committee chaired by Prof Jean-Marc Franssen. We also would like to thank to the Scientific Committee chaired by Prof Paulo Vila Real, the authors and all the supporting staff (and volunteer team) from the Institute for Sustainability and Innovation in Structural Engineering (ISISE) in Coimbra, for making SIF 2024 a successful conference.
Fire-induced spalling of normal strength concrete with different types of blended Portland cement
(2024)
The cement industry is looking to reduce its overall CO2 footprint. Greener manufacturing can be achieved by the introduction of more clinker-reduced cements. Concrete exposed to fire tends to show explosive spalling caused by thermomechanical and thermohydraulic processes. It is therefore essential to determine how concretes with clinker-reduced cements behave under fire exposure, especially for concretes containing calcined clays, as these are expected to be the supplementary cementitious material of the future.
In this paper, normal strength concretes with four different cements (CEM I, CEM II/A-LL, CEM III/A and CEM II/B-Q) were examined for their fire-induced spalling behaviour. In addition, a mix with PP fibres was investigated for each concrete. The experiments were conducted on ring-restrained cylindrical specimens exposed to the hydrocarbon fire curve. The results showed that the cement type influences spalling behaviour. Samples with CEM I spalled the least, followed by CEM II/A-LL and CEM III/A.
Finally, samples with CEM II/B-Q showed the most severe damage. It was found that the spalling behaviour of different concretes correlates with the moisture content before exposure to fire, meaning that higher moisture content leads to higher spalling susceptibility. The use of 2 kg/m³ PP fibres completely inhibited spalling regardless of the cement type used and therefore remains a successful avoidance strategy.
Considering the existing challenges involved in the transfer of flame retardant (FR) formulations from epoxy (EP) resins to glass fiber reinforced composites (GFRCs), obtaining data on the post-fire flexural properties of such composites is even more challenging as this involves balancing test parameters with potential composite delamination. In this study, solvent-free FR additives: ammonium polyphosphate (APP), and inorganic silicate (InSi) were added at 10, 30% and 50% w/w loading to a Bisphenol A diglycidyl ether (DGEBA)-dicyandiamide (DICY)-Urone resin matrix. These resin formulations were transferred to bidirectional (BD) glass fiber composites via prepregs. A novel, but facile approach was developed to prepare the composite samples for furnace tests at 400 oC. The composites were also subjected to fire exposure at different heat fluxes and times via a bench-scale test and subsequently tested via three-point bending. At approximately 3.5% P content, the FRs significantly improve the fire performance of both the resins and composites. However, they also degrade the systems’ pre- and postfire flexural modulus and strength. Therefore, improving the flame-retardant mode of action of the FRs in the composites, contrastingly reduces their structural integrity post-fire leading to a trade-off effect.
Considering the existing challenges involved in the transfer of flame retardant (FR) formulations from epoxy (EP) resins to glass fiber reinforced composites (GFRCs), obtaining data on the post-fire flexural properties of such composites is even more challenging as this involves balancing test parameters with potential composite delamination. In this study, solvent-free FR additives: ammonium polyphosphate (APP), and inorganic silicate (InSi) were added at 10, 30% and 50% w/w loading to a Bisphenol A diglycidyl ether (DGEBA)-dicyandiamide (DICY)-Urone resin matrix. These resin formulations were transferred to bidirectional (BD) glass fiber composites via prepregs. A novel, but facile approach was developed to prepare the composite samples for furnace tests at 400 oC. The composites were also subjected to fire exposure at different heat fluxes and times via a bench-scale test and subsequently tested via three-point bending. At approximately 3.5% P content, the FRs significantly improve the fire performance of both the resins and composites. However, they also degrade the systems’ pre- and postfire flexural modulus and strength. Therefore, improving the flame-retardant mode of action of the FRs in the composites, contrastingly reduces their structural integrity post-fire leading to a trade-off effect.