Influence of Post-curing on Solid State 13C NMR Spectra of Electron Beam-irradiated Epoxy Resins

Soo-Jin Park; Gun-Young Heo; Fan-Long Jin

Journal of Industrial and Engineering Chemistry, Vol.12, No.6, 972-975, November, 2006

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Influence of Post-curing on Solid State 13C NMR Spectra of Electron Beam-irradiated Epoxy Resins

Soo-Jin Park^†, Gun-Young Heo , and Fan-Long Jin¹

Department of Chemistry, Inha University, Nam-gu, Incheon 402-751, Korea
¹Department of Chemical Engineering, Jilin Institute of Chemical Technology, Jilin City 132022, China

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In this work, difunctional epoxy resins were cured using electron beam (EB) irradiation. After EB curing, the specimens were cured thermally and the effect of post-curing on the network structure was investigated using nuclear magnetic resonance (NMR) spectroscopy. Decreases in the abundances of extant oxirane and secondary alcohol groups after post-curing were confirmed from analyses of solid-state 13C NMR spectra. These phenomena could be explained by the fact that the crosslinking density increased through the re-crosslinking that occurred during post-curing. In terms of the cure mechanism we believe that the main cure reactions during EB curing were the reactions mediated by the protonic acids and oxonium cations.

Keywords:electron-beam;post-curing;solid-state 13C NMR;protonic acids;oxonium cations

[References]

Mehnert R, Pincus A, Janorsky I, Stowe R, Berejka A, UV & EB Curing Technology & Equipment, 2nd Edn. John Willey & Sons, London, Chapter 1 (1998)
Charlesby A, Atomic Reaction and Polymer, Pergamon Press, Oxford (1960)
Lim YM, Kang PH, Lee SM, Kim SS, Jeun JP, Jung CH, Choi JH, Lee YM, Nho YC, J. Ind. Eng. Chem., 12(4), 589 (2006)
Glauser T, Johansson M, Hult A, Macromol. Mater. Eng., 274, 20 (2000)
Crivello JV, Walton TC, Malik R, Chem. Mater., 9, 1273 (1997)
Ju X, Ha H, Jiang B, Zhou Y, Radiat. Phys. Chem., 56, 573 (1999)
Sui G, Zang ZG, Chen CQ, Zhong WH, Mater. Chem. Phys., 78, 349 (2003)
Pappas SP, Radiation curing, Plenium Press, New York (1992)
Crivello JV, Ahn J, J. Polym. Sci. A: Polym. Chem., 41(16), 2570 (2003)
Yagci Y, Reetz I, Prog. Polym. Sci, 23, 1485 (1998)
Kim MS, Lee KW, Endo T, Lee SB, Macromolecules, 37(15), 5830 (2004)
Sundell PE, Ph. D. Thesis, Royal Institute of Technology, Stockholm (1990)
Rath S, Boey F, Abadie M, Polym. Int., 53, 857 (2004)
Glauser T, Hult A, Johansson M, Kornmann X, Berglund L, Macromol. Mater. Eng., 280, 20 (2000)
Park SJ, Jin FL, Lee JR, Shin JS, Eur. Polym. J., 41, 231 (2005)
Park SJ, Lee HY, Lee JR, J. Ind. Eng. Chem., 11(5), 726 (2005)
Sojka S, Moniz W, J. Appl. Polym. Sci., 20, 1977 (1976)
Ngono-Ravache Y, Foray MF, Bardet M, Polym. Adv. Technol., 12, 515 (2001)
Kumar RN, Mehnert R, Scherzer T, Bauer F, Macromol. Mater. Eng., 286, 598 (2001)
Attias AJ, Bloch B, J. Polym. Sci., 28, 3445 (1990)
Finzel MC, Delong J, Hawley MC, J. Polym. Sci. A: Polym. Chem., 33, 673 (1995)
Park SJ, Heo GY, Suh DH, J. Polym. Sci. A: Polym. Chem., 41(15), 2393 (2003)
Xu LS, Schlup JR, J. Appl. Polym. Sci., 67(5), 895 (1998)
Park SJ, Kwak GH, Seo MK, Lee JR, J. Polym. Sci. B: Polym. Phys., 39(3), 326 (2001)

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[1] Mehnert R, Pincus A, Janorsky I, Stowe R, Berejka A, UV & EB Curing Technology & Equipment, 2nd Edn. John Willey & Sons, London, Chapter 1 (1998)

[2] Charlesby A, Atomic Reaction and Polymer, Pergamon Press, Oxford (1960)

[3] Lim YM, Kang PH, Lee SM, Kim SS, Jeun JP, Jung CH, Choi JH, Lee YM, Nho YC, J. Ind. Eng. Chem., 12(4), 589 (2006)

[4] Glauser T, Johansson M, Hult A, Macromol. Mater. Eng., 274, 20 (2000)

[5] Crivello JV, Walton TC, Malik R, Chem. Mater., 9, 1273 (1997)

[6] Ju X, Ha H, Jiang B, Zhou Y, Radiat. Phys. Chem., 56, 573 (1999)

[7] Sui G, Zang ZG, Chen CQ, Zhong WH, Mater. Chem. Phys., 78, 349 (2003)

[8] Pappas SP, Radiation curing, Plenium Press, New York (1992)

[9] Crivello JV, Ahn J, J. Polym. Sci. A: Polym. Chem., 41(16), 2570 (2003)

[10] Yagci Y, Reetz I, Prog. Polym. Sci, 23, 1485 (1998)

[11] Kim MS, Lee KW, Endo T, Lee SB, Macromolecules, 37(15), 5830 (2004)

[12] Sundell PE, Ph. D. Thesis, Royal Institute of Technology, Stockholm (1990)

[13] Rath S, Boey F, Abadie M, Polym. Int., 53, 857 (2004)

[14] Glauser T, Hult A, Johansson M, Kornmann X, Berglund L, Macromol. Mater. Eng., 280, 20 (2000)

[15] Park SJ, Jin FL, Lee JR, Shin JS, Eur. Polym. J., 41, 231 (2005)

[16] Park SJ, Lee HY, Lee JR, J. Ind. Eng. Chem., 11(5), 726 (2005)

[17] Sojka S, Moniz W, J. Appl. Polym. Sci., 20, 1977 (1976)

[18] Ngono-Ravache Y, Foray MF, Bardet M, Polym. Adv. Technol., 12, 515 (2001)

[19] Kumar RN, Mehnert R, Scherzer T, Bauer F, Macromol. Mater. Eng., 286, 598 (2001)

[20] Attias AJ, Bloch B, J. Polym. Sci., 28, 3445 (1990)

[21] Finzel MC, Delong J, Hawley MC, J. Polym. Sci. A: Polym. Chem., 33, 673 (1995)

[22] Park SJ, Heo GY, Suh DH, J. Polym. Sci. A: Polym. Chem., 41(15), 2393 (2003)

[23] Xu LS, Schlup JR, J. Appl. Polym. Sci., 67(5), 895 (1998)

[24] Park SJ, Kwak GH, Seo MK, Lee JR, J. Polym. Sci. B: Polym. Phys., 39(3), 326 (2001)