Additive manufacturing (AM) or 3D printing offers a new paradigm for designing and developing chemical reactors, in particular, prototypes. The use of 3D printers has been increasing, their performance has been improving, and their price has been reducing. While the general trend is clear, particular applications need to be assessed for their practicality. This study develops and follows a systematic approach to the prototyping of Advanced Oxidation Processes (AOP) reactors. Specifically, this work evaluates and discusses different printable materials in terms of mechanical and chemical resistance to photo-Fenton reactants. Metallic and ceramic materials are shown to be impracticable due to their high printing cost. Polymeric and composite materials are sieved according to criteria such as biodegradability, chemical, thermal, and mechanical resistance. Finally, 3D-printed prototypes are produced and tested in terms of leakage and resistance to the photo-Fenton reacting environment. Polylactic acid (PLA) and wood–PLA composite (Timberfill®) were selected, and lab-scale raceway pond reactors (RPR) were printed accordingly. They were next exposed to H2O2/Fe(II) solutions at pH = 3 ± 0.2 and UV radiation. After 48 h reaction tests, results revealed that the Timberfill® reactor produced higher Total Organic Carbon (TOC) concentrations (9.6 mg·L−1) than that obtained for the PLA reactor (5.5 mg·L−1) and Pyrex® reactor (5.2 mg·L−1), which suggests the interference of Timberfill® with the reaction. The work also considers and discusses further chemical and mechanical criteria that also favor PLA for 3D-printing Fenton and photo-Fenton reactors. Finally, the work also provides a detailed explanation of the printing parameters used and guidelines for preparing prototypes.