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Synergistic effects between silicon-containing flame retardant and DOPO on flame retardancy of epoxy resins

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Abstract

A novel flame retardant, containing silicon and nitrogen (PSiN), was synthesized, and it was used together with 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) to prepare a flame-retardant system for epoxy resins (EP). Flammability and thermal behaviors of EP systems were estimated by limited oxygen index (LOI), vertical burning test (UL-94), microscale combustion calorimetry test and thermogravimetric analysis. The results showed that synergistic effects on the flame retardancy of EP composites existed between the DOPO and PSiN. When 3 % PSiN and 7 % DOPO were incorporated, the LOI value of EP was found to be 34 %, and the UL-94 test found to be class V-0. The microstructures observed by scanning electron microscopy and FTIR indicated that the surface of the char for EP/DOPO/PSiN system holds a more cohesive and denser char structure when compared to the pure EP and EP/DOPO systems.

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References

  1. Liu Q, Bao X, Deng SQ. The investigation of methyl phenyl silicone resin/epoxy resin using epoxy-polysiloxane as compatibilizer. J Therm Anal Calorim. 2014;118:247–54.

    Article  CAS  Google Scholar 

  2. Bao X, Cai XF. Synergistic effect of methyl phenyl silicone resin and DOPO on the flame retardancy of epoxy resins. J Therm Anal Calorim. 2014;118:369–75.

    Article  CAS  Google Scholar 

  3. Ahmada S, Gupta AP, Sharmin E, Alam M, Pandey SK. Synthesis, characterization and development of high performance siloxane-modified epoxy paints. Prog Org Coat. 2005;54:248–55.

    Article  Google Scholar 

  4. Wu CS, Liu YL, Chu YS. Epoxy resins possessing flame retardant elements from silicon incorporated epoxy compounds cured with phosphorus or nitrogen containing curing agents. Polymer. 2002;43:4277–84.

    Article  CAS  Google Scholar 

  5. Jiang J, Chen YB, Liu Y, Wang Q. Intergrowth charring for flame-retardant glass fabric-reinforced epoxy resin composites. J Mater Chem A. 2015;3:4284–90.

    Article  CAS  Google Scholar 

  6. Yuan DD, Yin HQ, Cai XF. Synergistic effects between silicon-containing flame retardant and potassium-4-(phenylsulfonyl)benzene-sulfonate (KSS) on flame retardancy and thermal degradation of PC. J Therm Anal Calorim. 2013;114:19–25.

    Article  CAS  Google Scholar 

  7. Chen XL, Jiao CM. Synergistic effects of hydroxy silicone oil on intumescent flame retardant polypropylene system. Fire Saf J. 2009;44:1010–4.

    Article  CAS  Google Scholar 

  8. Lu SY, Hamerton I. Recent developments in the chemistry of flame retardant composites matrices. Prog Polym Sci. 2002;27:1661–712.

    Article  CAS  Google Scholar 

  9. Shen H, Wang YH, Mai KC. Non-isothermal crystallization behavior of PP/Mg(OH)2 composites modified by different compatibilizers. Thermochim Acta. 2007;457:27–34.

    Article  CAS  Google Scholar 

  10. Wang WJ, Perng LH, Hsiue GH, Chang FC. Characterization and properties of new silicone-containing epoxy resin. Polymer. 2000;41:6113–22.

    Article  CAS  Google Scholar 

  11. Liu SM, Lang XM, Ye H. Preparation and characterization of copolymerized aminopropyl/phenylsilsesquioxane microparticles. Eur Polym J. 2005;41:996–1001.

    Article  CAS  Google Scholar 

  12. Chiang CL, Ma CCM. Synthesis, characterization, thermal properties and flame retardance of novel phenolic resin/silica nanocomposites. Polym Degrad Stab. 2004;83:207–14.

    Article  CAS  Google Scholar 

  13. Qian XD, Song L, Yuan BH, Yu B. Organic/inorganic flame retardants containing phosphorus, nitrogen and silicon: preparation and their performance on the flame retardancy of epoxy resins as a novel intumescent flame retardant system. Mater Chem Phys. 2014;143:1243–52.

    Article  CAS  Google Scholar 

  14. Hsiue GH, Liu YL, Tsiao J. Phosphorus-containing epoxy resins for flame retardancy V: synergistic effect of phosphorus–silicon on flame retardancy. J Appl Polym Sci. 2000;78:1–7.

    Article  CAS  Google Scholar 

  15. Lin CH, Feng CC, Hwang TY. Preparation, thermal properties, morphology, and microstructure of phosphorus containing epoxy/SiO2 and polyimide/SiO2 nanocomposites. Eur Polym. 2007;43:725–42.

    Article  CAS  Google Scholar 

  16. Wang XD, Zhang Q. Synthesis, characterization, and cure properties of phosphorus-containing epoxy resins for flame retardance. Eur Polym. 2004;40:385–95.

    Article  CAS  Google Scholar 

  17. Lin CH, Wu CY, Wang CS. Synthesis and properties of phosphorus-containing advanced epoxy resins. II. J Appl Polym Sci. 2000;78:228–35.

    Article  CAS  Google Scholar 

  18. Wang CS, Shieh JY. Synthesis and properties of epoxy resins containing 2-(6-oxid-6H-diben <c,e> <1,2> oxa-phosphorin-6-yl)1,4-benzenediol. Polymer. 1998;39:5819–26.

    Article  CAS  Google Scholar 

  19. Cho CS, Fu SC, Chen LW, Wu TR. Aryl phosphinate anhydride curing for flame retardant epoxy networks. Polym Int. 1998;47:203–9.

    Article  CAS  Google Scholar 

  20. Liu YL, Wu CS, Hsu KY, Chang TC. Flame-retardant epoxy resins from o-cresol novolac epoxy cured with a phosphorus containing aralkyl novolac. J Polym Sci Polym Chem. 2002;40:2329–39.

    Article  CAS  Google Scholar 

  21. Wang CS, Lin CH. Properties and curing kinetic of diglycidyl ether of bisphenol A cured with a phosphorus-containing diamine. J Appl Polym Sci. 1999;74:1635–45.

    Article  CAS  Google Scholar 

  22. Levchik SV, Weil ED. Thermal decomposition, combustion and flame retardancy of epoxy resins—a review of the recent literature. Polym Int. 2004;53:1901–29.

    Article  CAS  Google Scholar 

  23. Hsiue GH, Liu YL, Liao HH. Flame retardant epoxy resins: an approach from organic-inorganic hybrid nanocomposites. J Polym Sci A Polym Chem. 2001;39:986.

    Article  CAS  Google Scholar 

  24. Gu AJ, Liang GZ. Thermal degradation behaviour and kinetic analysis of Epoxy/montmorillonite nanocomposites. Polym Degrad Stab. 2003;80:383–91.

    Article  CAS  Google Scholar 

  25. Kanai H, Sullivan V, Auerback A. Impact modification of engineering thermoplastics. J Appl Polym Sci. 1994;53:527–41.

    Article  CAS  Google Scholar 

  26. Kambour RP, Ligon WV, Russell RP. Enhancement of the limiting oxygen index of an aromatic polycarbonate by the incorporation of silicone blocks. J Polym Sci C Polym Lett. 1978;16:327–33.

    Article  CAS  Google Scholar 

  27. Durga G, Narula AK. Curing and thermal behaviour of diamide–diimide–diamines based on l-phenylalanine with epoxy blends containing phosphorus/silicon. J Therm Anal Calorim. 2012;109:345–53.

    Article  CAS  Google Scholar 

  28. Chen YJ, Zhan J, Zhang P, Nie SB, Lu HD, Song L, Hu Y. Preparation of intumescent flame retardant poly(butylene succinate) using fumed silica as synergistic agent. Ind Eng Chem Res. 2010;49:8200–8.

    Article  CAS  Google Scholar 

  29. Morgan AB, Harris RH, Kashiwagi T, et al. Flammability of polystyrene layered silicate (clay) nanocomposites: carbonaceous char formation. Fire Mater. 2002;26:247–53.

    Article  CAS  Google Scholar 

  30. Bugajny M, Bourbigot S, Le Bras M, et al. The origin and nature of flame retardance in ethylene vinyl acetate copolymers containing hostaflam AP 750. Polym Int. 1999;48:264–70.

    Article  CAS  Google Scholar 

  31. Wang ZZ, Lv P, Hu Y, Hu KH. Thermal degradation study of intumescent flame retardants by TG and FTIR: melamine phosphate and its mixture with pentaerythritol. J Anal Appl Pyrol. 2009;86:207–14.

    Article  CAS  Google Scholar 

Download references

Acknowledgements

We would like to thank the generous financial support by the following grant: Applied basic research project of Sichaun Technology Department, Grant No. 2014JY0138.

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Correspondence to Xufu Cai.

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Zhang, L., Wang, Y., Liu, Q. et al. Synergistic effects between silicon-containing flame retardant and DOPO on flame retardancy of epoxy resins. J Therm Anal Calorim 123, 1343–1350 (2016). https://doi.org/10.1007/s10973-015-5046-6

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  • DOI: https://doi.org/10.1007/s10973-015-5046-6

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