A two-stage process consisting of anaerobic fermentation followed by sub-critical wet oxidation was used to generate acetic acid from sewage sludge at pilot scale. Volatile fatty acids, dominated by propionic acid, were produced over 4–6 days in the 2,000 L fermentation reactor, which also achieved 31% solids reduction. Approximately 96% of the carbon was retained in solution over the fermentation stage. Using a 200 L wet oxidation reactor operating in batch mode, the second stage achieved 98% volatile suspended solids (VSS) destruction and 67% total chemical oxygen demand (tCOD) destruction. Acetic acid produced in this stage was recalcitrant to further degradation and was retained in solution. The gross yield from VSS was 16% for acetic acid and 21% for volatile fatty acids across the process, higher than reported yields for wet oxidation alone. The pilot plant results showed that 72% of the incoming phosphorus was retained in the solids, 94% of the nitrogen became concentrated in solution and 41% of the carbon was converted to a soluble state, in a more degradable form. Acetic acid produced from the process has the potential to be used to offset ethanol requirements in biological nutrient removal plants.