This work aims to optimize the recovery of methyl methacrylate (MMA) by depolymerization of polymethyl methacrylate (PMMA) dental resins fragments/residues. In order to pilot the experiments at technical scale, the PMMA dental resins scraps were submitted by thermogravimetric analysis (TG/DTG/DTA). The experiments were conducted at 345, 405, and 420 °C, atmospheric pressure, using a pilot scale reactor of 143 L. The liquid phase products obtained at 420 °C, atmospheric pressure, were subjected to fractional distillation using a pilot scale column at 105 °C. The physicochemical properties (density, kinematic viscosity, and refractive index) of reaction liquid products, obtained at 345 °C, atmospheric pressure, were determined experimentally. The compositional analysis of reaction liquid products at 345 °C, 30, 40, 50, 60, 70, 80, and 110 min, at 405 °C, 50, 70, and 130 min, and at 420 °C, 40, 50, 80, 100, 110, and 130 min were determined by GC-MS. The morphology of PMMA dental resins fragments before and after depolymerization was performed by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDX). The experiments show that liquid phase yields were 55.50%, 48.73%, and 48.20% (wt.), at 345, 405, and 420 °C, respectively, showing a first order exponential decay behavior, decreasing with increasing temperature, while that of gas phase were 31.69%, 36.60%, and 40.13% (wt.), respectively, showing a first order exponential growth, increasing with temperature. By comparing the density, kinematic viscosity, and refractive index of pure MMA at 20 °C with those of liquid reaction products after distillation, one may compute percent errors of 1.41, 2.83, and 0.14%, respectively. SEM analysis showed that all the polymeric material was carbonized. Oxygenated compounds including esters of carboxylic acids, alcohols, ketones, and aromatics were detected by gas chromatography/mass spectrometry (GC-MS) in the liquid products at 345, 405, and 420 °C, atmosphere pressure. By the depolymerization of PMMA dental resins scraps, concentrations of methyl methacrylate between 83.454 and 98.975% (area.) were achieved. For all the depolymerization experiments, liquid phases with MMA purities above 98% (area.) were obtained between the time interval of 30 and 80 min. However, after 100 min, a sharp decline in the concentrations of methyl methacrylate in the liquid phase was observed. The optimum operating conditions to achieve high MMA concentrations, as well as elevated yields of liquid reaction products were 345 °C and 80 min.