The effective separation of short-chain fatty acids (SCFAs) from acidic fermentation broth of organic solid wastes is difficult because of its complicated composition. The combination of tributyl phosphate (TBP) reactive extraction with vacuum evaporation stripping was investigated and its performance evaluated in this manuscript. The selection of vacuum evaporation as the stripping of SCFAs was mainly based on the "temperature swing effect" of reactive extraction. Under 15 min of extraction, room temperature, and a 1:1 extraction phase ratio (v/v), the extraction efficiency (E) of SCFAs by TBP amounted to 98.47 % after the third extraction. In view of SCFAs' stripping, the stripping efficiency (E') of 100 degrees C vacuum evaporation was up to 94.74 % under 0.095 MPa vacuum, a 1:1 stripping phase ratio (v/v), and 30 min of stripping. Finally, 93.29 % SCFAs and 98.21 % acetic acid could be separated and recovered from synthetic acidic fermentation broth of municipal sewage sludge. TBP could be regenerated after SCFAs were stripped from it three times.