A series of surfactants utilizing various molecular weight allyloxy(poly(ethylene oxide)s (PEOs) and siloxanes were successfully synthesized via iridium-catalyzed hydrosilylation. The iridium (Ir) catalytic process highlights a rapid transformation in producing siloxane-based surfactants without the harsh reaction conditions of a traditional platinum (Pt) catalytic system. Furthermore, direct hydrosilylation of two anionic modified PEO molecules with a sulfate termination (SO4) was achieved with the Ir catalytic system previously not accessible via traditional Pt-catalyzed reactions. The siloxane polyether surfactants were characterized by 1H nuclear magnetic resonance (NMR) and high-resolution mass spectrometry (HRMS). The surfactants described are considered promising additives for fluorine-free foams (FFF).