Cationic Cure of Epoxy Resin by an Optimum Concentration of N-benzylpyrazinium Hexafluoroantimonate

  • Lee, Jong-Keun (Department of Polymer Science and Engineering, Kumoh National University of Technology) ;
  • Park, Yusong (Department of Polymer Science and Engineering, Kumoh National University of Technology) ;
  • Jae-Rock lee (Advanced Materials Division, Korea Research Institute of Chemical Technology) ;
  • Park, Jaekyeung (Department of Chemical Engineering, Sangju National University)
  • Published : 2002.02.01

Abstract

Cure behavior of an epoxy resin was investigated at different cure temperatures (110, 120, 130, 140, and 150 $^{\circ}C$) and cure times in the presence of 2 wt% of an N-benzylpyrazinium hexafluoroantimonate (BPH) cationic catalyst by means of differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA). The glass transition temperature ( $T_{g}$) and chemical conversion (x) at the different temperatures were determined from DSC thermograms. The $T_{g}$ and x vs. In time data were superposed up to $T_{g}$ = 10$0^{\circ}C$ and x = 0.70 by shifting horizontally at a reference temperature of $T_{g}$ = 13$0^{\circ}C$. It is interesting that the $T_{g}$ and x of the superposed data increase rather slowly in the early stage of cure and rapidly thereafter. Therefore, the increase of the $T_{g}$ and x can be divided into two regions; $R_{I}$= -18.4(= $T_{go}$ ) ~5$^{\circ}C$ and $R_{II}$ = 5 ~ 10$0^{\circ}C$ in $T_{g}$, and $R_{I}$ : 0~0.24 and $R_{II}$ : 0.24~0.70 in x. The $R_{I}$ is closely related to the initiation reactions between BPH and epoxy and between hydroxy group and epoxy in this epoxy/catalyst system. From the kinetic analysis of the $T_{g}$-shift, activation energy was 12.5 kcal/mol. The relationship between $T_{g}$ and x was also considered. The gelation and vitrification times for different cure temperatures were obtained from DMA curves.urves. DMA curves.urves.

Keywords

References

  1. O. Shimomura, I. Tomita, and T. Endo, J. Polym. Sci., Part A: Polym. Chem. , 39,868 (2001)
  2. K. Morio, H. Murase, and H. Tsuchiya, J. Appl. Polym. Sci., 32, 5727 (1986)
  3. S. Murai, Y. Nakano, and S. Hayase, J. Appl. Polym. Sci., 80, 181 (2001),
  4. A. P. Pappas and L. H. Hill, J. Coating Tech., 53, 43 (1981)
  5. T. Endo, A. Kikkawa, H. Uno, and H. Sato, J. Polym. Sci., Polym. Lett, Ed, , 27, 73 (1989)
  6. J. Gu, S. C. Narang, and E. M. Pearce, J. Appl. Polym. Sci., 30, 2997 (1985)
  7. J. Park, Korea Polym. J., 9, 206 (2001)
  8. Y.C. Kim, S.-J. Park, and J. -R. Lee, Polym. J., 29, 759 (1997)
  9. S, -J, Park, T. -J. Kim, and J. -R. Lee, J., Polym. Sci.: Part B:Polym. Phys., 38, 2114 (2000)
  10. G. -H. Kwak, S. -J. Park, and J. -R. Lee, J. Appl, Polym. Sci., 78, 290 (2000),
  11. S. -J. Park and H. -C. Kim, J. Polym. Sci, :Part B:Polym. Phys., 39, 121 (2001),
  12. G. Wisanrakkit and J. K. Gillham, J. Coating Tech., 62, 35 (1990)
  13. A. Osei-Owusu, G. C. Martin, and J. T. Grotto, Polym. Eng, Sci., 31,1604 (1991)
  14. V. Micro, Z. Q. Cao, F. Mechin, and J. P. Pascault, Am. Chem. Soc.,., Polym. Mater, Sci., Eng. Prepr., 66, 451 (1992)
  15. P. A. Oyanguren and R. J. J. Williams, J. Appl, Polym. Sci.,47, 1371 (1993)
  16. S. L. Simon and J. K. Gillham, J. Appl, Polym. Sci., 46, 1245 (1992)
  17. W. H. Park, J. K. Lee, and K. J. Kwon, Polym, J., 28, 407 (1996)
  18. R. B. Prime, Thermal Characterization of Polymeric Materials, E. A. Turi, Ed., Academic Press, New York, 1997, Vol, 2
  19. L. E. Nelson, J. Macromol. Sci. Rev. Macromol, Chem., C3, 69 (1969)