7.5 Technische Eigenschaften von Polymerwerkstoffen
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Poly(limonene carbonate) (PLimC) is a green polymer produced from renewable limonene oxide and CO₂ as a green carbon feedstock. Previous fire-behavior results showed that PLimC responds best to flame retardants (FRs) typically used in polyolefin systems. To develop a sustainable formulation, we evaluated melem phytate, biochar, phosphorylated lignin, and aluminum hydroxide (ATH) individually, and subsequently combined melem phytate with each of the three environmentally friendly adjuvants.
Techniques including cone calorimetry were used to understand the thermal stability and fire behavior of all formulations. Figure 1, using the biochar system as an example, demonstrates a stepwise reduction in pHRR for melem phytate and biochar alone, with their combination yielding the greatest shift toward the origin in the Petrella diagram. This result highlights a sustainable FR strategy, as combining melem phytate and biochar, as well as with ATH and phosphorylated lignin, improves fire performance using renewable, low-hazard compounds.
This study examines two comprehensive approaches to reducing the amount of antimony trioxide (ATO) in brominated flame retardant (tris(2,4,6‐tribromophenoxy)‐s‐triazine bromine) (Br) in acrylonitrile–butadiene–styrene (ABS). One approach systematically substitutes Br/ATO with magnesium hydroxide (MH), while the other substitutes ATO with calcium borate, zinc borate, zinc oxide, zinc sulfide, and zinc stannate. We investigated the pyrolysis (thermogravimetry), flammability (limiting oxygen index and UL 94 tests), smoldering (smoke density chamber), and fire behavior (cone calorimeter). The study reveals that the synergism between Br and ATO is essential and sensitive to any changes. None of the additives fully replaced the Br/ATO mixture or ATO alone while maintaining the same level of flame retardancy. Replacing the Br/ATO mixture with MH reduces smoke emission during burning but increases flammability in the ignition scenario. Zinc and calcium salts considerably lower the peak of heat release rate due to the enhanced formation of a protective char layer. The residual protective layer hinders mass and heat transfer, and prolonged residence time of the decomposition products in the pyrolytic zone results in smoke reduction. This systematic investigation illustrates the challenges of replacing Br/ATO or ATO in ABS, but it also emphasizes the relevant benefits and remarkable potential of partial replacement.
Poly(lactic acid) (PLA) is the most important player in the biopolymer market. So far competing with commodity plastics for packaging dominates PLA consumption. Developing flame retardant PLA composites enables the replacement of higher-priced technical polymers in electrical engineering. Sustainable, bio-based, and compostable PLA composites are the ultimate goal, thus using natural fibres and eco-friendly/bio-based flame retardants are on the short list of the current and urgent research tasks. Some opportunities and tasks, milestones and innovations are adumbrated using different examples taken from our recent research projects [1-6]. The challenge to maintain the molecular weight during processing is underlined as well as the impact of viscosity on the flammability. Natural fibres are discussed with respect to their impact on the mechanical performance and fire behaviour of PLA composites. Innovative bio-derived adjuvants and flame retardants such as biochar, cork, in wastewater P-enriched microalgae, phosphorylated lignin, and different phytates are proposed.
Reference materials are indispensable for obtaining reliable measurement results. Incorrect values cost time and money, because at best they lead to measurements having to be re-peated and at worst they can cause wrong decisions with far-reaching consequences. To achieve a meaningful comparison between results obtained by different laboratories using the Friction After Polishing (FAP) test method, it is therefore essential to use elastomer materials with similar properties.
The Federal Institute for Materials Research and Testing (BAM) has been working on the de-velopment of reference materials for more than 100 years. A comprehensive quality manage-ment system ensures that the production of such materials meets the requirements of DIN EN ISO 17034. BAM currently offers over 400 reference materials for various applications. This also includes more than 20 elastomer reference materials.
At the moment, a team from the elastomer group of BAM division 7.5 is working in coopera-tion with the Federal Highway Research Institute (BASt) on the development of rubber sliding blocks and polishing rollers that can serve as reference materials for FAP devices in the fu-ture. This presentation describes the hurdles that have already been overcome and outlines the next steps.
Major fire disasters continue to cause substantial loss of life, economic damage, and social disruption worldwide. Although investigations occur in most countries, lessons learned are often fragmented, published in incompatible formats, or not published at all. Therefore, it is recommended that a group be set up of experts to investigate national and international fire incidents in a structured manner and to determine specifically what lessons can be learned for the future.
Analysis of nanomaterial (NM) surface chemistry is essential for understanding and controlling NM properties relevant for NM functionality, stability, and safety. In this work, we present a multimethod study of the quantification of the frequently used, biocompatible surface ligand citrate for lanthanide-based upconversion nanoparticles (UCNPs) and iron oxide nanoparticles (IONPs). Methods applied that address different yet correlated measurands with varying chemo-selectivity and rely on different sample preparation workflows include chemo-selective reversed-phase high-performance liquid chromatography (RP-HPLC) with photometric detection measuring liquid samples and dissolved NMs as well as non-selective thermogravimetric analysis (TGA) and chemo-selective pyrolysis-gas chromatography-mass spectrometry (PyGC-MS) analyzing dried NMs. Thereby, we demonstrate the applicability of the RP-HPLC method, recently developed for citrate quantification on IONPs, for UCNPs as another application-relevant NM class. In addition, the feasibility of PyGC-MS, emerging for material characterization at the trace level due to the consumption of very small sample amounts and minimum sample preparation, for NM ligand quantification is assessed. This method, which has not been applied before for NM surface analysis, indirectly quantifies citrate via the amount of acetone formed during citrate decomposition. For UCNPs, PyGC-MS measurements led to a good agreement with the TGA and RP-HPLC results within the respective measurement uncertainties. However, quantifying citrate on IONPs with PyGC-MS resulted in an overestimation of citrate, which is tentatively ascribed to IONP catalytic activity. Overall, our method cross-comparison underlines the importance of multimethod characterization schemes to assure a reliable and precise ligand quantification and to identify method- and NM-specific effects.
Poly(limonene carbonate) (PLimC) is an emerging bio-based polymer produced from renewable limonene and carbon dioxide. To enable its use in technical applications, its fire performance must be improved through meffective and environmentally compatible flame-retardant (FR) strategies. Bio-based FRs—melem phytate, phosphorylated lignin (P-lignin), and biochar—were valorized through investigation of thermal and mechanical properties, flammability, and fire behavior, with aluminum trihydroxide (ATH) included as an environmentally benign mineral FR. Individual effects were assessed using formulations containing 5 wt% melem phytate or 20 wt% of P-lignin, biochar, or ATH. Potential synergistic interactions were subsequently examined by combining melem phytate with each adjuvant at a total loading of 25 wt%. Each additive alone reduced key fire properties, including fire load and peak heat release rate. When melem phytate was combined with an adjuvant, these reductions became even more pronounced—as seen in the Petrella diagram—demonstrating that the mixed formulations provide enhanced FR performance. These enhancements highlight the complementary roles of phosphorus-rich and charring agents in promoting condensed-phase protection. Overall, the results demonstrate a viable pathway toward sustainable, flame-resistant PLimC materials and confirm the effectiveness of bio-based FR systems for meeting fire safety requirements.
Flame retardant polyurethane (PU) foams and thermoplastic PU are proposed for insulation, seat cushioning, or cable jackets. PU consists of alternating segments that tailor the material properties while also determining the pyrolysis and fire behavior. Most PU materials are highly flammable and tend to form pool fires or burning drops; although rigid and flexible PU foams are two different stories, their low thermal inertia results in short ignition times and intensive flame spread. The important PU markets are dying for developing novel flame-retardant PU materials that outperform the existing ones. This work delivers detailed insight into the complex burning behavior of PU-materials. The comprehensive understanding of the physical and chemical processes and their complex interplay, respectively, is presented as the foundation of customized development of future PU materials.
Flame retarded bioplastics: The flame retardancy of three cork particle sizes was investigated in polylactide acid (PLA) and combined with barrier forming ammonium polyphosphate (APP), flamepoisoning 9,10-dihydro-9-oxa-10-phosphaphenanthren-10-oxid (DOPO) and the newly synthesized bio-flame retardant melem phytate. V0 was achieved with only 10wt.% APP, DOPO, and melem phytate, respectively. With increasing particle size, cork composites reduced peak heat release rate (pHRR) from 703 kW/m² (PLA) to 280 kW/m² in PLA with 20 wt.% cork. Combining flame retardants and cork resulted in a crucial reduction in fire load up to 43% and pHRR up to 64%. Maximum tensile strength remained constant across the cork particle sizes. Injection molding and 3D printing were successful.
Für ein Prüflaboratorium ist die richtige Anwendung von Prüfnormen von grundlegender Bedeutung. Um die Kompetenz des Labors zu belegen, sind Ringversuche ein wichtiges Mittel. In dem Vortrag wurde gezeigt, wie ein Prüflaboratorium die Teilnahme an Ringversuchen zu diesem Zweck nutzen kann. Welche aktuellen Anforderungen gibt es bei einer Akkreditierung als Prüflaboratorium? Wie kann die Beteiligung an einem Ringversuch nach ISO 4649 genutzt werden, um die Unsicherheit der Ergebnisse des Verfahrens für das Prüflaboratorium zu ermitteln?