In this study, the effect of operational parameters, such as solids retention time (SRT), pH, and substrate total solids (TS) concentration, on acid fermentation efficiency was investigated. From batch tests, it was shown that the appropriate pH range for thermophilic acidogens was around 6–7 and that the optimum pH condition was 6. From the continuous experiment, pH and SRT were shown to be the most important operational parameters for solubilization and organic acid production. In contrast, TS concentration did not show any obvious effect on chromium chemical oxygen demand (CODcr) solubilization when TS was in the range 3.5%–10%. The optimum operational conditions for thermophilic acid fermentation were an SRT of 2 days and a pH of 6.