Abstract
The synergistic flame retardant effects of AlPi and ATH in UPR were investigated. The flammability and thermal stability of UPR composites were evaluated with LOI, UL-94 vertical burning, MCC and TG. The structure and morphology of filler and char residues were examined with SEM and FTIR. The interaction between AlPi and ATH was observed when the mass ratio of AlPi and ATH was 3:2 and LOI value of flame-retarded UPR increased to 30 and UL-94 rating passed V-0; however, the SEM showed that AlPi and ATH have a good dispersion in UPR. The pHRR of UPR-15AlPi/10ATH was 241.6 Wg−1, decreasing by 30.4 % compared with pure UPR. The experimental TG curve of AlPi/ATH in N2 was lower than calculated one at the second stage and had lower char residue at 700 °C, demonstrating interaction of AlPi and ATH during thermal degradation. The char residue of UPR-15AlPi/10ATH at 700° suggested that the interaction between AlPi and ATH strengthened the char-formation ability and thermal stability of UPR, so the SEM showed a strong and dense char surface. The FTIR of char residues at different temperatures showed that AlPi and ATH interactions changed the type of aluminum phosphates, making char residue of UPR/AlPi/ATH system increased eventually.
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1007%2Fs10973-016-5459-x/MediaObjects/10973_2016_5459_Fig1_HTML.gif)
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1007%2Fs10973-016-5459-x/MediaObjects/10973_2016_5459_Fig2_HTML.jpg)
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1007%2Fs10973-016-5459-x/MediaObjects/10973_2016_5459_Fig3_HTML.gif)
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1007%2Fs10973-016-5459-x/MediaObjects/10973_2016_5459_Fig4_HTML.gif)
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1007%2Fs10973-016-5459-x/MediaObjects/10973_2016_5459_Fig5_HTML.gif)
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1007%2Fs10973-016-5459-x/MediaObjects/10973_2016_5459_Fig6_HTML.gif)
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1007%2Fs10973-016-5459-x/MediaObjects/10973_2016_5459_Fig7_HTML.jpg)
Similar content being viewed by others
References
Baudry A, Dufay J, Regneir N, Mortaigne B. Thermal degradation and fire behaviour of unsaturated polyesters with chain ends modified by dicyclopentadiene. Polym Degrad Stab. 1998;61:441.
Tibiletti L, Longuet C, Ferry L, Coutelen P, Mas A, Robin JJ, et al. Thermal degradation and fire behaviour of unsaturated polyesters filled with metallic oxides. Polym Degrad Stab. 2011;96(1):67–75.
Baskaran R, Sarojadevi M, Vijayakumar CT. Unsaturated polyester nanocomposites filled with nano alumina. J Mater Sci. 2011;46(14):4864–71.
Nazare′ S, Kandola BK, Horrocks AR. Flame-retardant unsaturated polyester resin incorporating nanoclays. Polym Adv Technol. 2007;17(4):294–303.
Ricciardi MR, Antonucci V, Zarrelli M, Giordano M. Fire behavior and smoke emission of phosphate-based inorganic fire-retarded polyester resin. Fire Mater. 2012;36:203–15.
Horold S. Phosphorus flame retardants in thermoset resins. Polym Degrad Stab. 1999;64:427–31.
Klinkows C, Zang L, Doring M. DOPO-based flame retardants: synthesis and flame retardant efficiency in polymers. Mater China. 2013;32(3):144–58.
Si M, Feng J, Hao J, Xu L, Du J. Synergistic flame retardant effects and mechanisms of nano-Sb2O3 in combination with aluminum phosphinate in poly (ethylene terephthalate). Polym Degrad Stab. 2014;100:70–8.
Braun U, Bahr H, Sturm H, Schartel B. Flame retardancy mechanisms of metal phosphinates and metal phosphinates in combination with melamine cyanurate in glass‐fiber reinforced poly (1, 4‐butylene terephthalate): the influence of metal cation. Polym Adv Technol. 2008;19:680.
Braun U, Shartel B, Fichera MA, Jager C. Flame retardancy mechanisms of AlPi in combination with melamine polyphosphate and zinc borate in glass-fibre-reinforced polyamide6,6. Polym Degrad Stab. 2007;92:1528–45.
Liu X, Liu J, Cai S. Comparative study of Aluminum Diethylphosphinate and Aluminum Methylethylphosphinate-filled epoxy flame-retardant composites. Polym Compos. 2012;33:918–26.
Wang Y, Zhang L, Yang Y, Cai X. The investigation of flammability, thermal stability, heat resistance and mechanical properties of unsaturated polyester resin using AlPi as flame retardant. J Therm Anal Calorim. 2015;122:1331–9.
Duquesne S, Fontaine G, Cérin-Delaval O, Gardelle B, Tricot G, Bourbigot S. Study of the thermal degradation of an aluminium phosphinate–aluminium trihydrate combination. Thermochim Acta. 2013;551:175–83.
Gallo E, Braun U, Schartel B, Russo P, Acierno D. Halogen-free flame retarded poly (butylene terephthalate) (PBT) using metal oxides/PBT nanocomposites in combination with aluminium phosphinate. Polym Degrad Stab. 2009;94(8):1245–53.
Gallo E, Schartel B, Acierno D, Russo P. Flame retardant biocomposites: synergism between phosphinate and nanometric metal oxides. Eur Polym J. 2011;47(7):1390–401.
Gallo E, Schartel B, Braun U, Russo P, Acierno D. Fire retardant synergisms between nanometric Fe2O3 and aluminum phosphinate in poly (butylenes terephthalate). Polym Adv Technol. 2011;22(12):2382–91.
Mehmet D, Aysen Y, Erdal B. Synergistic effect of boron containing substances on flame retardancy and thermal stability of intumescent polypropylene composites. Polym Degrad Stab. 2010;95(12):2584–8.
Zhang H, Westmoreland PR, Farris FJ, Coughlin EB, Plichta A, Brzozowski ZK. Thermal decomposition and flammability of fire-resistant, UV/visible-sensitive polyarylates, copolymers and blends. Polymer. 2002;43:5463–72.
Zhang HQ, Farris RJ, Westmoreland PR. Low flammability and thermal decomposition behavior of poly (3,3′-dihydroxybiphenylisophthalamide) and its derivatives. Macromolecules. 2003;36:3944–54.
Benin V, Durganala S, Morgan AB. Synthesis and flame retardant testing of new boronated and phosphonated aromatic compounds. J Mater Chem. 2012;22(3):1180–90.
Levchik SV, Weil ED. A review of recent progress in phosphorus-based flame retardants. J Fire Sci. 2006;24(5):345–64.
Cinausero N, Azema N, Cochez M, Ferriol M, Essahli M, Ganachaud F, et al. Influence of the surface modification of alumina nanoparticles on the thermal stability and fire reaction of PMMA composites. Polym Adv Technol. 2008;19(6):701–9.
Samyn F. Compréhension des procédés d’ignifugation du polyamide 6-Apport des nanocomposites aux systèmes retardateurs de flamme phosphorés, Ph.D. Thesis, Université de Lille1, 2007. http://ori.univ-lille1.fr/notice/view/univ-lille1-ori-5598.
Braun U, Schartel B. Flame retardancy mechanisms of AlPi in combination with melamine cyanurate in glass-fibre-reinforced poly (1,4-butylene terephthalate). Macromol Mater Eng. 2008;293:206–17.
Sullalti S, Colonna M, Berti C, Fiorini M, Karanam S. Effect of phosphorus based flame retardants on UL-94 and comparative tracking index properties of poly (butylene terephthalate). Polym Degrad Stab. 2012;97(4):566–72.
Tjong SC, Bao SP. Preparation and nonisothermal crystallization behavior of polyamide 6/montmorillonite nanocomposites. J Polym Sci, Part B: Polym Phys. 2004;42(15):2878–91.
Holland BJ, Hay JN. The thermal degradation of PET and analogous polyesters measured by thermal analysis–Fourier transform infrared spectroscopy. Polymer. 2002;43(6):1835–47.
Balabanovich AI. Thermal decomposition study of intumescent additives: pentaerythritol phosphate and its blend with melamine phosphate. Thermochim Acta. 2005;435(2):188–96.
Li H, Ning N, Zhang L, Wang Y, Liang W, Tian M. Different flame retardancy effects and mechanisms of aluminium phosphinate in PPO, TPU and PP. Polym Degrad Stab. 2014;105(105):86–95.
Acknowledgements
We would like to thank the generous supports by the following: National Natural Sciences Foundation of China, Grant No. 50973066; the Experiment center of Polymer science and engineering academy, Sichuan University; Tiannan Zhou doctor; Xinhui Science and Technology Co, LTD.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Wang, Y., Zhang, L., Yang, Y. et al. Synergistic flame retardant effects and mechanisms of aluminum diethylphosphinate (AlPi) in combination with aluminum trihydrate (ATH) in UPR. J Therm Anal Calorim 125, 839–848 (2016). https://doi.org/10.1007/s10973-016-5459-x
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10973-016-5459-x