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Cure process and reaction-induced phase separation in a diepoxy–diamine/PMMA blend. Monitoring by steady-state fluorescence and FT-IR (near and medium range)

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Abstract

Poly(methyl methacrylate), PMMA, was chosen as an additive for an epoxy system based on the cured product of (a) diglycidyl ether of bisphenol A labeled with 5-dimethylaminonaphthalene-1-(2-aminoethyl) sulfonamide and (b) 1,5-diamino-2-methylpentane. Fourier transformed infrared spectroscopy (near, FT-NIR, and medium, FT-MIR, ranges) and steady-state fluorescence spectroscopy were used to monitor the epoxy cure reaction and the induced phase separation. The PMMA seems to exert a change in the mechanism of the epoxy cure reaction by means of a slight enhancement of the secondary amino group reactivity. It has been demonstrated that following the fluorescence response of the dansyl chromophore chemically bonded to the epoxy component is a way to monitor the cure process in a general sense, not only accounting for the chemical changes but also being additionally possible to detect the reaction-induced phase separation at a molecular scale. The fluorescence results, in terms of the first moment of the emission band, point out that the dilution effect is affecting the physicochemical changes of the modified epoxy system quite more exclusively than the chemical changes. Finally, a semiempirical model to explain the behavior of the dansyl fluorescence during the curing of a PMMA/diepoxy–diamine blend showing a reaction-induced phase separation has been proposed. The proposed model allows estimating the composition of the phases after nearly complete cure.

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Acknowledgements

This work has been funded by the project GR/MAT/0499/2004 of the CAM (Spain). On the other hand, the authors acknowledge the Secretaría de Estado de Universidades e Investigación del Ministerio de Educación y Ciencia of Spain for supporting the short research stay of Dr. J. González-Benito at the Department of Materials (Engineering II) of the University of California, Santa Barbara. At the same time, we would like to thank Dr. E.J. Kramer and the University of California, Santa Barbara, for all the facilities supplied for the elaboration of this article.

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Authors and Affiliations

  1. Departamento de Ciencia e Ingeniería de Materiales e Ingeniería Química, Universidad Carlos III de Madrid, Avda. Universidad 30, 28911, Leganés, Madrid, Spain

    D. Olmos & J. González-Benito

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  1. D. Olmos
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  2. J. González-Benito
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Correspondence to J. González-Benito.

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Olmos, D., González-Benito, J. Cure process and reaction-induced phase separation in a diepoxy–diamine/PMMA blend. Monitoring by steady-state fluorescence and FT-IR (near and medium range). Colloid Polym Sci 284, 654–667 (2006). https://doi.org/10.1007/s00396-005-1434-y

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  • DOI: https://doi.org/10.1007/s00396-005-1434-y

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