In this study, syntactic composite foams were developed by incorporating cenosphere (CS) particles recovered from recycled fly ash into a one-component polyurethane (PU) foam system. During production, CS was added to the spray-applied PU foam at specific ratios, and the foaming reaction was simultaneously initiated via manual mixing. This approach minimized particle settling caused by the filler–matrix density difference and promoted a more homogeneous structure. Two types of CS, with mean sizes of approximately 70 µm and 130 µm, were incorporated at five loadings ranging from 5 wt% to 15 wt%. The resulting composites were evaluated for their acoustic, mechanical, and thermal performance. Thermal analyses revealed that CS addition increased the glass-transition temperature (Tg) by ≈12 °C and delayed the 5% mass-loss temperature (T5%) by ≈30–35 °C compared with the neat N2 foam, confirming the stabilizing role of cenospheres. The refoaming process with manual mixing promoted finer cell diameters and thicker walls, enhancing the sound absorption coefficient (α), particularly at medium and high frequencies. Moreover, increasing the filler content improved both the sound transmission loss (STL) and compressive strength, alongside density, although further gains in α and STL were limited beyond a 10 wt% filler content. Significant enhancements in compressive strength were achieved at filler ratios above 12.5 wt%. Unlike conventional two-component PU foams, this study demonstrates a sustainable one-component PU system reinforced with recycled cenospheres that simultaneously achieves acoustic, mechanical, and thermal multifunctionality. To the best of our knowledge, this is the first report on incorporating recycled cenospheres into a one-component PU foam system, overcoming dispersion challenges of conventional two-component formulations and presenting an environmentally responsible route for developing versatile insulation materials.
