The behavior of p-methoxybenzoyldiphenylphosphine oxide, previously synthesized, as a photoinitiator for the polymerization of diacrylate monomer, in the presence of 3% (w/w) tertiary amine (triethyl amine) as synergist additive, was studied. The influence of temperature in the range 30–90°C at 3% (w/w) photoinitiator concentration and the influence of the photoinitiator concentration in the range 0.5–3.5% (w/w) at 30°C was investigated by differential scanning photocalorimetry (photo-DSC). In all experiments the photopolymerization was performed at constant light intensity (3 mW cm−2). The maximum conversion was obtained at temperature of 90°C at 3% (w/w) photoinitiator concentration and 3% (w/w) triethyl amine. The optimal concentration of photoinitiator to obtain maximum conversion was 3% (w/w), at 30°C. No thermal polymerization occurred at higher temperature.