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Polyesters with 9,10-dihydro-9-oxy-10-phosphaphenanthrene-10-oxide-containing comonomers are synthesized aiming to improve the flame retardancy of aliphatic polyesters such as poly(butylene succinate) and poly(butylene sebacate). The influence of the chemical structure on the thermal decomposition and pyrolysis is examined using a combination of thermogravimetric analysis (TGA), TGA-Fourier transform infrared (FTIR) spectroscopy, pyrolysis-gas chromatography/mass spectrometry, and microscale combustion flow calorimetry. Thermal decomposition pathways are derived and used to select suitable candidates as flame retardants for PBS. The fire behavior of the selected polymers is evaluated by forced-flaming combustion in a cone calorimeter. The materials show two modes of action for flame retardancy: strong flame inhibition due to the release of a variety of molecules combined with charring in the solid state.
Several expandable graphites (EGs), differing in Expansion volume but with the same mean size, are compared as flame retardants in polyurethane (PUR) foams. Not only common sulfur-intercalated graphites are investigated but also a new one intercalated with phosphorus. The main aim of this article is to understand which properties of EG are important for its flame retardancy effectiveness in PUR foams. Thermal stability, flammability, and fire behavior are analyzed through limiting oxygen index and cone calorimeter tests. Detailed characterization of the phosphorus-intercalated graphite is also provided as well as physical–mechanical characterization. The results show that the well-known sulfur-intercalated graphites and the one with phosphorus both enhance the residue yield, induce a protective layer, and thus efficiently flame-retard PUR foams. While the expansion volume of the EGs had a surprisingly limited influence on the performance of the foams, at least in the range tested, the most important feature Controlling the effectiveness of EG in terms of flame retardant PUR foams was the type of intercalant. The presence of EG affected the physical–mechanical properties of the foams; however, no significant effect of the expansion volume or intercalant type has been revealed on the physical–mechanical properties of the foams.
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.
The functionalization of a natural sodium montmorillonite (MMT) with (3-glycidyloxypropyl)trimethoxysilane by a silylation procedure is presented, and its use as nanofiller in the melt compounding of low density polyethylene (LDPE) nanocomposites. In particular, the effects on the thermal stability and flame retardant properties of melt compounded LDPE nanocomposites are analyzed, with and without magnesium hydroxide (MH) as an additional conventional flame retardant. The purpose was to investigate possible synergistic effects between the two inorganic fillers on fire behavior. The obtained organosilylated clay showed higher interlayer spacing than the original MMT and good thermal stability, higher than that of many commercial organoclays modified with alkylammonium salts. Its addition to LDPE allowed the production of hybrids with nanoscale dispersion of the filler, as demonstrated by X-ray diffraction. The simultaneous presence of MH, which strongly interacts with the nanoclay, hindered intercalation of the polymer chains between the clay galleries and clay layer exfoliation within the LDPE resin.
The investigation of the thermal and burning behavior of the LDPE nanocomposites indicated that the organosilylated clay alone shows only a limited residual protection layer effect. In combination with MH the nanocomposites have a small adverse effect on the reaction to small flame as measured by the Oxygen index and UL 94 testing, and, surprisingly, no effect on the peak heat release rate in the cone calorimeter. The quality of the fire residue was lacking on the microscopic scale. The ternary LDPE/MH/ organoclay systems investigated did not open the door to reducing MH content in halogen-free flame retardant LDPE yet, but demand further research.
Condensed-phase mechanisms play a major role in fire-retardant polymers. Generations of development have followed the concept of charring to improve fire properties. Whereas the principal reactions are believed to be known, the specific description for multicomponent systems is lacking, as is the picture across different systems. A two-step approach is proposed in general, and also presented in greater detail. The second step covers the specific reactions controlling charring, whereas the actual reactants are provided in the preceding step. This model consistently incorporates the variety of structureproperty relationships reported. A comprehensive case study is presented on seven phosphorus flame retardants in two epoxy resins to breathe life into the two-step approach.
The influence of distinct carbon based nanofillers: expanded graphite (EG), conducting carbon black (CB), thermally reduced graphene oxide (TRGO) and multi-walled carbon nanotubes (CNT) on the thermal, dielectric, electrical and rheological properties of polybutylene terephthalate (PBT) was examined. The glass transition temperature (Tg) of PBT nanocomposites is independent of the filler type and content. The carbon particles act as nucleation agents and significantly affect the melting temperature (Tm), the crystallization temperature (Tc) and the degree of crystallinity of PBT composites. PBT composites with EG show insulating behaviour over the tested concentration range of 0.5 to 2 wt.-% and hardly changed rheological behaviour. CB, CNT and TRGO induce electrical conductivity to their particular PBT composites by forming a conducting particle network within the polymer matrix. CNT reached the percolation threshold at the lowest concentration (<0.5 wt.-%), followed by TRGO (<1 wt.-%) and CB (<2 wt.-%). With the formation of a particle network, the flow behaviour of composites with CB, CNT and TRGO is affected, i.e., a flow limit occurs and the melt viscosity increases. The degree of influence of the carbon nanofillers on the rheological properties of PBT composites follows the same order as for electrical conductivity. Electrical and rheological results suggest an influence attributed to the particle dispersion, which is proposed to follow the order of EG<< CB<TRGO<CNT.
The characteristic influences of increasing concentrations of graphene, expanded graphite (EG), carbon black (CB), and multiwall carbon nanotubes (MWNT) are investigated on pyrolysis, reaction to small flame, burning behavior, and on electrical, thermal, and rheological properties of flame retarded polypropylene (PP-FR). The property-concentration dependency is different for the various material properties, as threshold, linear, and leveling off functions were observed. Increasing concentrations of carbon nanoparticles resulted in a decrease in the electrical resistivity of the polymer by crossing the percolation threshold. The developing nanoparticle network changes melt flow behavior for small shear rates, increases thermal conductivity and therefore, affects the UL 94 classification and oxygen index. The onset temperature of PP decomposition is shifted to temperatures up to 37°C higher; the peak heat release rate is reduced by up to 74% compared to PP-FR. Both effects leveled off with increasing particle concentration. Among the four carbon nanomaterials tested, graphene presents superior influence on composite properties over the tested concentration range and outperforms commercial CB, MWNT, and EG. POLYM. COMPOS., 36:12301241, 2015.
Thermally reduced graphite oxide (TRGO), containing only four single carbon layers on average, was combined with ammonium polyphosphate (APP) and magnesium hydroxide (MH), respectively, in polypropylene (PP). The nanoparticle's influence on different flame-retarding systems and possible synergisms in pyrolysis, reaction to small flame, fire behavior and mechanical properties were determined. TRGO has a positive effect on the yield stress, which is decreased by both flame-retardants and acts as a synergist with regard to Young's modulus. The applicability and effects of TRGO as an adjuvant in combination with conventional flame-retardants depends strongly on the particular flame-retardancy mechanism. In the intumescent system, even small concentrations of TRGO change the viscosity of the pyrolysing melt crucially. In case of oxygen index (OI) and UL 94 test, the addition of increasing amounts of TRGO to PP/APP had a negative impact on the oxygen index and the UL 94 classification. Nevertheless, systems with only low amounts (≤1 wt%) of TRGO achieved V-0 classification in the UL 94 test and high oxygen indices (>31 vol%). TRGO strengthens the residue structure of MH and therefore functions as a strong synergist in terms of OI and UL 94 classification (from HB to V-0).