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Polymethoxy butyl ether (BTPOM_n), a novel diesel additive developed for suppressing incomplete combustion emissions, was synthesized via an optimized batch slurry method employing n-butanol and trioxane (TOX) over NKC-9 acid cation-exchange resin (90–110 °C). A comprehensive kinetic model elucidated the reaction mechanism, addressing competitive pathways governing both main product formation and key side reactions—specifically polyoxymethylene hemiformals (HD_n) and polyoxymethylene glycols (MG) generation. As the first detailed kinetic investigation of BTPOM_n synthesis, this work provides a fundamental dataset and a robust predictive model that are crucial for process intensification and reactor design. Hybrid optimization integrating genetic algorithms with nonlinear least-squares regression achieved robust parameter estimation, with model predictions showing excellent agreement with experimental data. Thermal effects significantly influenced reaction rates, enhancing decomposition and propagation processes with increasing temperature. Optimal catalyst loading was identified at 3 and 6 wt.%, balancing reaction acceleration and byproduct suppression. Temperature-dependent equilibrium revealed chain length regulation through growth and depolymerization processes. This mechanistic understanding enables predictive reactor design for cleaner fuel additive synthesis. It provides critical insights for developing emission-control technologies in diesel engine systems. Full article