Skip to main content
SpringerLink
Log in

Non-isothermal cure and decomposition kinetics of epoxy–imidazole systems

  • Published:
Journal of Thermal Analysis and Calorimetry Aims and scope Submit manuscript

Abstract

Non-isothermal curing kinetics of a tetra functional epoxy resin with imidazole-based curing agents was investigated by differential scanning calorimetry (DSC), and decomposition of the cured compounds was studied by thermogravimetric analysis. N,N,N′,N′-tetraglycidyl-4, 4′diaminodiphenylmethane (TGDDM) was cured with three types of tertiary amine curing agents including 1-methyl imidazole (MI), 2-methyl imidazole (2MI) and 2-ethyl 4-methyl imidazole (EMI). These systems exhibited cure initiation at around 70–90 °C by DSC. 2-methyl imidazole and 2-ethyl 4-methyl imidazole showed two cure initiation profiles, while the 1-substituted counterpart, MI, showed a single cure initiation profile by DSC. The Kissinger equation was applied to calculate the apparent activation energy for epoxy–imidazole cure reactions. The rate constants and the pre-exponential factor were also determined. The activation energy varied from 59 to 65 kJ mol−1 for the systems. The Flynn–Wall–Ozawa iso-conversional approach was used to elucidate the activation energies at different extents of conversion during the cure reactions. The cured systems are found thermally stable up to 250 °C. Decomposition kinetics of cured networks was studied using Kissinger equation and Flynn–Wall–Ozawa iso-conversional approach. The cured resins were analyzed for the glass transition temperature and compared with that of a conventional amine-cured system.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8
Fig. 9

Similar content being viewed by others

References

  1. Jin FL, Li X, Park SJ. Synthesis and application of epoxy resins: a review. J Ind Eng Chem. 2015;29:1–11.

    Article  CAS  Google Scholar 

  2. Weil ED, Levchik S. A review of current flame retardant systems for epoxy resins. J Fire Sci. 2004;22:25–40.

    Article  CAS  Google Scholar 

  3. Sprenjer S. Epoxy resin composites with surface-modified silicon dioxide nanoparticles: a review. J Appl Polym Sci. 2013;130(3):1421–8.

    Article  Google Scholar 

  4. Rafique I, Kausar A, Anwar Z, Muhammad B. Exploration of epoxy resins, hardening systems, and epoxy/carbon nanotube composite designed for high performance materials: a review. Polym Plast Technol. 2016;55(3):312–33.

    Article  CAS  Google Scholar 

  5. Mustata F, Bicu I. Multifunctional epoxy resins: synthesis and characterization. J Appl Polym Sci. 2000;77(11):2430–6.

    Article  CAS  Google Scholar 

  6. May CA. Epoxy resins, chemistry and technology. New York: Marcel Dekker; 1988.

    Google Scholar 

  7. Cheng J, Li J, Zhang JY. Curing behavior and thermal properties of trifunctional epoxy resin cured by 4, 4′-diaminodiphenyl sulfone. Expr Polym Lett. 2009;3(8):501–9.

    Article  CAS  Google Scholar 

  8. Qiu SL, Wang CS, Wang YT, Liu CG, Chen XY, Xie HF, Huang YA, Cheng RS. Effects of graphene oxides on the cure behaviors of a tetrafunctional epoxy resin. Expr Polym Lett. 2011;5(9):809–18.

    Article  CAS  Google Scholar 

  9. Yu M, Feng B, Xie W, Fang L, Li H, Liu L, Ren M, Zhnag J, Sun J, Hu H. The modification of a tetrafunctional epoxy and its curing reaction. Materials. 2015;8(6):3671–84.

    Article  Google Scholar 

  10. Unnikrishnan KP. Doctoral Dissertation, Cochin University of Science and Technology, India 2006.

  11. Prolongo SG, Prolongo G. Epoxy/poly (4-vinylphenol) blends crosslinked by imidazole initiation. J Therm Anal Calorim. 2007;87(1):259–68.

    Article  CAS  Google Scholar 

  12. Potter WG. Epoxide resins. New York: Springer; 1970.

    Google Scholar 

  13. Kissinger HE. Reaction kinetics in differential thermal analysis. Anal Chem. 1957;29:1702–6.

    Article  CAS  Google Scholar 

  14. Flynn J, Wall L. A quick, direct method for the determination of activation energy from thermogravimetric data. J Polym Sci Polym Lett. 1966;4(5):323–8.

    Article  CAS  Google Scholar 

  15. Barton JM, Shepherd PM. The curing reaction of an epoxide resin with 2-ethyl-4-methylimidazole, a calorimetric study of the kinetics of formation of epoxide-imidazole adducts. Makromol Chem. 1975;176:919–30.

    Article  CAS  Google Scholar 

  16. Vogt J. Thermoset matrices for structural adhesives: imidazole-catalysed curing of epoxy resins. J Adhesion. 1987;22:139–51.

    Article  CAS  Google Scholar 

  17. Dearlove TJ. A comparison of some imidazole catalysts as epoxy curing agents. J Appl Polym Sci. 1970;14:1615–26.

    Article  CAS  Google Scholar 

  18. Yang BK, Gu M. Fabrication. Morphology and cure behavior of triethylenetetramine-grafted multiwalled carbon nanotube/epoxy nanocomposites. Polym J. 2009;41(9):752–63.

    Article  CAS  Google Scholar 

Download references

Acknowledgements

The authors thank Director, Vikram Sarabhai Space Centre and Deputy Director, VSSC (PCM) for their permission to publish this work.

Author information

Authors and Affiliations

  1. Polymers and Special Chemicals Division, Vikram Sarabhai Space Centre, Thiruvananthapuram, Kerala, 695 022, India

    K. Leena, Monisha Baby, S. Suraj & Dhanya S. Mohan

  2. Analytical and Spectroscopy Division, Vikram Sarabhai Space Centre, Thiruvananthapuram, Kerala, 695 022, India

    P. B. Soumyamol & R. Rajeev

Authors
  1. K. Leena
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. P. B. Soumyamol
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Monisha Baby
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. S. Suraj
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. R. Rajeev
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Dhanya S. Mohan
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to K. Leena.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Leena, K., Soumyamol, P.B., Baby, M. et al. Non-isothermal cure and decomposition kinetics of epoxy–imidazole systems. J Therm Anal Calorim 130, 1053–1061 (2017). https://doi.org/10.1007/s10973-017-6410-5

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10973-017-6410-5

Keywords

Search

Navigation