A nanocomposite consisting of Fe3O4 and MWCNT was produced via sol-gel technique using FeCl3 along with MWCNT by calcination at 300℃. The degradation effect of rhodamine B dye has been investigated under UV illumination in a darkroom. The degradation reaction was studied by monitoring the discoloration of dye as a function of irradiation time using UV-visible spectrophotometeric technique. The Fe3O4-MWCNT samples have continuous degradation ability under the UV illumination with the first order kinetics and the dye removal was better than in the pristine Fe3O4. The resultant composite catalyst was found to be efficient for the photo-Fenton reaction of the dye.