Qualitative and quantitative evaluation of epoxy systems by Fourier transform infrared spectroscopy and the flexibilizing effect of mercaptans

Epoxy systems are widely applied as adhesives in the aerospace industry. They have excellent adhesion properties, however, being thermosetting, epoxy systems show fracture brittleness characteristics. Polysulfide and polymercaptans are good options to increase the flexibility of the epoxy adhesive. Thermal analysis techniques are generally used to evaluate the curing degree of epoxy systems. In most cases, when infrared (IR) analysis is used, it is employed qualitatively. This paper presents the reaction study of a DGEBA epoxy prepolymer with diethylenetriamine (DETA) and linear and branched dodecyl mercaptans as flexibilizers. Conversion data and curing time were assessed qualitatively and quantitatively by Fourier Transform Infrared Spectroscopy (FT-IR) in the medium infrared region (MIR) and in the near infrared region, using near infrared reflectance accessory (NIRA). NIRA methodology showed satisfactory results, with errors between 3 and 7%, especially in samples with lower amine contents. Mechanical tests confirmed the flexibilization of the cured epoxy system by the addition of mercaptans, indicating a lower crosslinking degree in the matrix. Young’s modulus (E) significantly decreased from 2017 MPa to 578 MPa with the addition of approximately 20 wt% of normal dodecyl mercaptan to the epoxy system.

Key words
epoxy resin; FT-MIR; mechanical properties; mercaptans; NIRA