Journal of Thermal Analysis and Calorimetry

, Volume 103, Issue 1, pp 303–310 | Cite as

Synthesis and thermal properties of silicon-containing epoxy resin used for UV-curable flame-retardant coatings

  • Xi-e Cheng
  • Wenfang Shi


A novel silicon-containing trifunctional cycloaliphatic epoxide resin tri(3,4-epoxycyclohexylmethyloxy) phenyl silane (TEMPS) was synthesized and characterized by FTIR, 1H NMR, 13C NMR, and 29Si NMR spectroscopic analysis. A series of flame-retardant formulations by blending TEMPS with a commercial epoxide resin DGEBA (EP828) in different ratios were prepared, and exposed to a medium pressure lamp to form the cured films in the presence of diaryliodonium hexafluorophosphate salt as a cationic photoinitiator. The thermal degradation behaviors of the cured films were evaluated by thermogravimetric analysis. The char yields under nitrogen and air atmospheres increased along with the TEMPS content. The limiting oxygen index (LOI) value increased from 22 for EP828 to 30 for TEMPS80, demonstrating the improved flame retardancy. The data from the dynamic mechanical thermal analysis showed that TEMPS had good miscibility with EP828. The T s and T g both decreased from 93 and 138 to 78 and 118 °C, respectively. The crosslinking density (ν e) increased along with the TEMPS content. The mechanical property measurements indicated that the addition of TEMPS led to a decrease in the tensile strength and an increase in the elongation-at-break.


Cycloaliphatic epoxide resin Silicon Flame-retardant UV-curing 



The authors gratefully acknowledge the financial support of the National Natural Science Foundation of China (No. 50633010).


  1. 1.
    Calbo LJ. Handbook of coatings additives. New York: Marcel Dekker; 1986.Google Scholar
  2. 2.
    May CA, editor. Epoxy resins chemistry and technology. New York: Marcel Dekker, 1988.Google Scholar
  3. 3.
    Lin SC, Pearce PM. High-performance thermosets. New York: Hanser; 1994.Google Scholar
  4. 4.
    Sen AK, Mukheriee B, Bhattacharya AS, Sanghi LK, De PP, Bhowmick K. Preparation and characterization of low-halogen and nonhalogen fire-resistant low-smoke (frls) cable sheathing compound from blends of functionalized polyolefins and PVC. J Appl Polym Sci. 1991;43:1673–84.CrossRefGoogle Scholar
  5. 5.
    Hsiue GH, Wang WJ, Chang FC. Synthesis, characterization, thermal and flame-retardant properties of silicon-based epoxy resins. J Appl Polym Sci. 1999;73:1231–8.CrossRefGoogle Scholar
  6. 6.
    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.CrossRefGoogle Scholar
  7. 7.
    Wang WJ, Perng LH, Hsiue GH, Chang FC. Characterization and properties of new silicone-containing epoxy resin. Polymer. 2000;41:6113–22.CrossRefGoogle Scholar
  8. 8.
    Abad MJ, Barral L, Fasce DP, Williams RJJ. Epoxy networks containing large mass fractions of a monofunctional polyhedral oligomeric silsesquioxane (POSS). Macromolecules. 2003;36:3128–35.CrossRefGoogle Scholar
  9. 9.
    Mecado LA, Reina JA, Galià M. Flame retardant epoxy resins based on diglycidyloxymethylphenylsilane. J Polym Sci A: Polym Chem. 2006;44:5580–7.CrossRefGoogle Scholar
  10. 10.
    Mercado LA, Galià M, Reina JA. Silicon-containing flame retardant epoxy resins: synthesis, characterization and properties. Polym Degrad Stab. 2006;91:2588–94.CrossRefGoogle Scholar
  11. 11.
    Spontón M, Mercado LA, Ronda JC, Galià M, Cádiz V. Preparation, thermal properties and flame retardancy of phosphorus-and silicon-containing epoxy resins. Polym Degrad Stab. 2008;93:2025–31.CrossRefGoogle Scholar
  12. 12.
    Hsiue GH, Wei HF, Shiiao SJ, Kuo WJ, Sha YA. Chemical modification of dicyclopentadiene-based epoxy resins to improve compatibility and thermal properties. Polym Degrad Stab. 2001;73:309–18.CrossRefGoogle Scholar
  13. 13.
    Decker C. Photoinitiated crosslinking polymerisation. Prog Polym Sci. 1996;21:593–650.CrossRefGoogle Scholar
  14. 14.
    Fieberg A, Reis O. UV curable electrodeposition systems. Prog Org Coat. 2002;45:239–47.CrossRefGoogle Scholar
  15. 15.
    Wu S, Sears MT, Soucek MD, Simonsick WJ. Synthesis of reactive diluents for cationic cycloaliphatic epoxide UV coatings. Polymer. 1999;40:5675–86.CrossRefGoogle Scholar
  16. 16.
    Decker C, Viet TNT, Decker D, Weber-Koehl E. UV-radiation curing of acrylate/epoxide systems. Polymer. 2001;42:5531–41.CrossRefGoogle Scholar
  17. 17.
    Wang HL, Liu JH, Xu SP, Shi WF. Preparation and film properties of tri(3,4-epoxycyclohexylmethyl) phosphate based cationically UV curing coatings. Prog Org Coat. 2009;65:263–8.CrossRefGoogle Scholar
  18. 18.
    Kanai H, Sullivan V, Auerback A. Impact modification of engineering thermoplastics. J Appl Polym Sci. 1994;53:527–41.CrossRefGoogle Scholar
  19. 19.
    Hill LW. Structure/property relationships of thermoset coatings. J Coat Technol. 1992;64:29–42.Google Scholar

Copyright information

© Akadémiai Kiadó, Budapest, Hungary 2010

Authors and Affiliations

  1. 1.CAS Key Laboratory of Soft Matter Chemistry, Department of Polymer Science and EngineeringUniversity of Science and Technology of ChinaAnhuiPeople’s Republic of China

Personalised recommendations