TY - JOUR A1 - Langfeld, Kirsten A1 - Wilke, Antje A1 - Sut, Aleksandra A1 - Greiser, Sebastian A1 - Ulmer, B. A1 - Andrievici, V. A1 - Limbach, P. A1 - Bastian, Martin A1 - Schartel, Bernhard T1 - Halogen-free fire retardant styrene-ethylene-butylene-styrene-based thermoplastic elastomers using synergistic aluminium diethylphosphinate-based combinations N2 - Multicomponent flame retardant systems containing aluminum diethylphosphinate in thermoplastic styrene–ethylene–butylene–styrene elastomers are investigated (oxygen index, UL 94, cone calorimeter, and mechanical testing). Solid-state nuclear magnetic resonance, scanning electron microscopy, and elemental analysis illuminate the interactions in the condensed phase. Thermoplastic styrene–ethylene–butylene–styrene elastomers are a challenge for flame retardancy (peak heat release rate at 50 kW m-2 > 2000 kW m-2, oxygen index = 17.2 vol%, no UL-94 horizontal burn rating) since it burns without residue and with a very high effective heat of combustion. Adding aluminum diethylphosphinate results in efficient flame inhibition and improves the reaction to small flame, but it is less effective in the cone calorimeter. Its efficacy levels off for amounts >~25 wt%. As the most promising synergistic system, aluminum diethylphosphinate/melamine polyphosphate was identified, combining the main gas action of aluminum diethylphosphinate with condensed phase mechanisms. The protection layer was further improved with several adjuvants. Keeping the overall flame retardant content at 30 wt%, aluminum diethylphosphinate/melamine polyphosphate/titanium dioxide and aluminum diethylphosphinate/melamine polyphosphate/boehmite were the best approaches. An oxygen index of up to 27 vol% was achieved and a horizontal burn rating in UL 94 with immediate self-extinction; peak heat release rate decreased by up to 85% compared to thermoplastic styrene–ethylene–butylene–styrene elastomers, to <300 kW m-2. KW - Flame retardancy KW - Aluminium phosphinate KW - Thermoplastic elastomers KW - Cone calorimetry KW - Flammability PY - 2015 DO - https://doi.org/10.1177/0734904114565581 SN - 0734-9041 SN - 1530-8049 VL - 33 IS - 2 SP - 157 EP - 177 PB - Sage CY - London AN - OPUS4-32692 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Antje A1 - Langfeld, Kirsten A1 - Ulmer, B. A1 - Andrievici, V. A1 - Hörold, Andreas A1 - Limbach, P. A1 - Bastian, Martin A1 - Schartel, Bernhard T1 - Halogen-free Multicomponent Flame Retardant Thermoplastic Styrene-Ethylene-Butylene-Styrene Elastomers Based on Ammonium Polyphosphate – Expandable Graphite Synergy N2 - Developing flame retarded thermoplastic elastomers (TPES) based on styrene−ethylene−butylene−styrene, polypropylene, and mineral oil is a challenging task because of their very high fire loads and flammability. A promising approach is the synergistic combination of expandable graphite (EG) and ammonium polyphosphate (APP). Cone calorimetry, oxygen index, and UL 94 classification were applied. The optimal EG:APP ratio is 3:1, due to the most effective fire residue morphology. Exchanging APP with melamine-coated APPm yielded crucial improvement in fire properties, whereas replacing EG/APP with melamine polyphosphate did not. Adjuvants, such as aluminum diethyl phosphinate (AlPi), zinc borate, melamine cyanurate, titanium dioxide, dipentaerylthritol, diphenyl-2-ethyl phosphate, boehmite, SiO2, chalk, and talcum, were tested. All flame retardants reinforced the TPE-S. The combination with AlPi is proposed, because with 30 wt % flame retardants a maximum averaged rate of heat emission below 200 kW m−2 and a V-0 rating was achieved. Multicomponent EG/APP/adjuvants systems are proposed as a suitable route to achieve efficient halogen-free flame retarded TPE-S. KW - Thermoplastic elastomers KW - Amonium polyphosphate KW - Expandable graphite KW - Synergy PY - 2017 DO - https://doi.org/10.1021/acs.iecr.7b01177 SN - 0888-5885 VL - 56 IS - 29 SP - 8251 EP - 8263 PB - ACS Publications AN - OPUS4-41509 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - BOOK A1 - Schubert, Martina A1 - Schartel, Bernhard A1 - Lang, M. A1 - Yin, Huajie A1 - Dittrich, Bettina A1 - Heidemeyer, P. A1 - Bastian, Martin T1 - Wirkungsweise von halogenfreien Flammschutzmitteln in WPC N2 - Das Ziel des Forschungsvorhabens war die Untersuchung der Wirkungsweise von halogenfreien Flammschutzmitteln in WPC. Eine große Anzahl verschiedener Flammschutzmittel wurde hinsichtlich ihrer Wirkmechanismen umfassend untersucht, um ein Verständnis für die ablaufenden Prozesse zu entwickeln. Hierbei wurden verschiedene Brandtests eingesetzt, um die Materialien bezüglich verschiedener Applikationen (E&E, Transportwesen, Bauwesen) zu beleuchten. Die verschiedenen Untersuchungen liefern aber auch ein umfassendes Bild vom Brandverhalten in den verschiedenen Eigenschaften, wie Entflammbarkeit und Brandausbreitung. Die prinzipiellen Ansätze wurden anhand von verschiedenen Flammschutzmitteln beleuchtet, ihre Pyrolyse und ihre Performance in verschiedenen Brandtests gegenübergestellt. Bei der angestrebten geringen Zusatzmenge ist durch den Zusatz eines einzigen Flammschutzmittels keine zufriedenstellende Reduktion der Brandeigenschaften zu erwarten. Multikomponentensysteme zur Steigerung der Effizienz sind angezeigt. Einige prinzipielle Kombinationsmöglichkeiten wurden für alle Hauptflammschutzmittel durchgespielt. Die teilweise deutlichen Verbesserungen zeigen Wege zur erfolgreichen Produktentwicklung auf. So konnten bei den Spritzgießcompounds Eigenschaften erzielt werden, die eine UL 94 V0 Klassifizierung ermöglichen. Ein Einsatz der im Forschungsvorhaben hergestellten Compounds als Baustoff ist aufgrund des Brandverhaltens in den baustoffspezifischen Prüfungen nicht möglich. Hier sind weitere Flammschutz-Konzepte zu erproben. Gleitmittel nehmen bei den untersuchten Extrusionscompounds keinen Einfluss auf das Brandverhalten. Haftvermittler nehmen ebenfalls keinen signifikanten Einfluss auf das untersuchte Brandverhalten, können aber zu einer veränderten Verteilung der Füllstoffe und damit zur Ausbildung einer effektiveren Schutzschicht führen. Feinere Holzpartikel schneiden bei den Brandprüfungen besser ab als grobe Holzpartikel. Bei Einsatz von grobem Holz wird eine schlechtere Rückstandsstruktur ausgebildet, was das Brandverhalten negativ beeinflusst. Der Einsatz von vorbehandeltem Holz brachte nicht die erwartete Verbesserung. Die neu konzipierte Aufbereitungsanlage auf Basis des Planetwalzenextruders konnte erfolgreich in Betrieb genommen werden. Vergleichende Versuche mit dem Doppelschneckenextruder zeigten, dass der PWE-Aufbau eine gute Alternative zur etablierten DSE-Aufbereitung darstellt. Zusätzlich wurden an Compounds vielversprechender Flammschutzansätze weitere Materialprüfungen (Biegeversuch, Schlagversuch, Wasseraufnahme) durchgeführt, um den Einfluss der FSM auf die spezifischen Eigenschaften der WPC zu beleuchten. N2 - The objective of the research project was to investigate the effect of halogen-free flame retardants in WPC. A large number of different flame retardants was thoroughly examined regarding their effect mechanisms to develop an understanding for the processes taking place. Different fire tests were used to examine the materials with respect to the different applications (E&E, transportation, construction). Additionally, the different investigations provide a comprehensive picture of the fire behavior regarding the different properties, such as flammability and fire spread. The fundamental approaches were examined by means of different flame retardants and their pyrolysis and performance were compared in different fire tests. A satisfactory reduction of the fire properties by adding only one flame retardant cannot be expected with the intended low added amount. Multi-component systems to increase the efficiency are indicated. Some basic combination options were tried out for all main flame retardants. The partially considerable improvements illustrate ways for successful product development. This way, properties could be achieved in injection molding compounds, which allow for a UL 94 V0 classification. It is not possible to use the compounds introduced in the research project as building material due to the fire behavior in the building material specific tests. Further flame protection concepts need to be tested in this area. Slip agents do not have an influence on the fire behavior of the examined extrusion compounds. Adhesion promoters also do not have a significant influence on the examined fire behavior but can lead to a change in the distribution of the fillers and thus to the formation of a more effective protective layer. Finer wood particles performed better in the fire tests than coarse wood particles. When using coarse wood, an inferior residual structure is formed, which has an adverse effect on the fire behavior. The use of pretreated wood fibers did not bring the expected improvement. The newly conceived processing technique based on a planetary roller extruder (PRE) was successfully put into operation. Comparative tests with twin-screw extruders (TSE) showed that the PRE configuration is a good alternative to the established TSE processing. Additionally, further material testing (bending test, impact test, water absorption) was performed on promising flame retarded compounds to examine the influence of the fire retardants on the specific properties of the WPC. KW - Wood plastic composite KW - Halogen free KW - Flame retardancy PY - 2016 SN - 978-3-8440-4645-8 SN - 2364-754X SP - 1 EP - 88 PB - Shaker Verlag CY - Aachen AN - OPUS4-37482 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -