Efficient recovery of carboxylic acids from fermentation broth is essential for improving the economic viability of bio-based production systems. In this study, we developed an integrated downstream process combining liquid–liquid extraction (LLE) and distillation for the recovery and purification of short-chain carboxylic acids, such as acetic acid (AA), produced via acetogenic fermentation of renewable feedstocks. Tri-octylamine (TOA) diluted in 1-octanol was selected as an effective extractant based on its high affinity for AA, stable phase separation, and compatibility with the distillation step. The LLE process enabled selective extraction of carboxylic acids from the aqueous broth into the organic phase. The resulting AA-rich organic phase was subjected to distillation, with operating conditions optimized to achieve high product purity, reduce energy consumption, and allow solvent recovery. The integrated process achieved an AA extraction efficiency of over 97% and a final purity exceeding 98%. Compared to conventional single-step recovery methods, this two-step approach offers enhanced selectivity, scalability, and energy efficiency. Moreover, the strategy is adaptable for recovering other volatile or semi-volatile organic acids from biological systems. These results support the feasibility of implementing this process in industrial biorefinery applications.
