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Abstract  

Differential scanning calorimetry (DSC) was applied to study the cure kinetics of an epoxy system containing both tetraglycidyl 4,4′-diaminodiphenylmethane (TGDDM) and a multifunctional Novolac glycidyl ether resin, cured with 4,4′-diaminodiphenylsulfone (DDS). The experimental data were analyzed in terms of a mechanistic model proposed by Cole, which includes the etherification reaction. The kinetics can be completely described in terms of three rate constants, which obey the Arrhenius relationship. This model gives a good description of the cure kinetics up to the onset of vitrification. The effect of diffusion control was incorporated to describe the cure in the later stages. By combining the model and a diffusion factor, it was possible to predict the cure kinetics over the whole range of conversion, including an analysis of the evolution of different chemical species during the curing process. Good agreement with the experimental DSC data was achieved with this mechanistic model over the whole range of cure when the etherification reaction was assumed to be of first order with respect to the concentrations of epoxide groups, hydroxy groups, and the tertiary amine groups formed in the epoxide amine reaction.

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Abstract  

The physical aging of a system containing tetraglycidyl-4-4′-diaminodiphenylmethane (TGDDM), with a multifunctional novolac glycidyl ether resin hardened by 4,4′-diaminodiphenylsulphone (DDS) has been investigated by differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA). Samples fully cured were aged at temperatures between 200 and 250C, during periods of time from 1 to a maximum of 336 h. Furthermore, the dynamic mechanical relaxation behaviour annealed at temperature of 220C, was studied, aging during 24 and 168 h. The effect of the enthalpy relaxation during DSC heating scan is shown by the presence of an endothermic peak whose position and intensity depends on the aging conditions, both temperature and time. DSC studies suggest that enthalpy relaxation increases gradually with aging time to a limiting value for each temperature where structural equilibrium is reached. DMA results show that the effect of aging is to cause chain stiffening and a decrease in the height of the peak value of the loss factor.

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Journal of Thermal Analysis and Calorimetry
Authors: L. Barral, J. Cano, J. López, I. López-Bueno, P. Nogueira, C. Ramírez, A. Torres, and M. Abad

Abstract  

Cure kinetics using a differential scanning calorimetry (DSC) technique were analyzed for a thermoplastic modified tetraglycidyl-4,4′-diaminodiphenylmethane (TGDDM) epoxy resin cured with diaminodiphenylsulphone (DDS), an aromatic diamine. The neat resin and its blends with the poly(styrene-co-acrylonitrile) (SAN) of various compositions were studied by applying a phenomenological model proposed by Kamal. Kinetic parameters were determined by fitting experimental data. This model gives a good description of cure kinetics up to the onset of vitrification. Diffusion control was incorporated to describe the cure in the latter stages of cure. The results showed that the addition of SAN did not alter the nature of the reaction, but the reaction rates and final conversions decreased when SAN contents increase, due to reduction of mobility of the reacting species.

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