The effect of a microwave (MW) pre-treatment on two-phase olive mill solid residue (OMSR) or alperujo with a view to enhancing its anaerobic digestibility was studied. The MW pre-treatment was carried out at a power of 800 W and at a targeted temperature of 50 °C using different heating rates and holding times. The following specific energies were applied: 4377 kJ·kg TS-1 (MW1), 4830 kJ·kg TS-1 (MW2), 7170 kJ·kg TS-1 (MW3) and 7660 kJ·kg TS-1 (MW4). The maximum methane yield, 395±1 mL CH4·g VSadded-1, was obtained for MW4. The effect of the pre-treatment on the kinetics of the process was also studied. The methane production curves generated during the batch tests showed a first exponential stage and a second sigmoidal stage for all the cases studied. In the first stage, the kinetic constant for the pre-treatment MW1 was 54.8% higher than that obtained for untreated OMSR.