Multiwalled carbon nanotubes (MWNT) modified by 2.2′-azoiso- butyronitrile (AIBN) were incorporated into methyl methacrylate (MMA) by sonochemistry method, resulting in homogenous dispersion of MWNT, which makes possible to obtain flexible conductive polymer-matrix nanocomposites films of PMMA, with MWNT concentrations ranging from 0 to 0.5 wt%. Modified MWNT (AIBN-MWNT) were studied by Fourier transform infrared (FT-IR), Raman spectroscopy, X-ray Photoelectron Spectroscopy (XPS) and through visual observations in order to compare the dispersion in 2-propanone and toluene with that of pristine MWNT. Synthesized PMMA-AIBN-MWNT films were studied by FT-IR and Raman spectroscopy. Using FT-IR for the AIBN-MWNT it was not possible to identify any group or groups attached to the nanotubes. Raman spectroscopy shows a small modification in the Lorentzian peaks ratio ID/G of AIBN-MWNT, meanwhile XPS showed that atomic compositions does not change for AIBN-MWNT compared to the pristine nanotubes. Also by impedance it was analyzed the conductivity of PMMA-MWNT films and the results showed a threshold percolation at 0.5 wt%. FT-IR and Raman analyses for PMMA-AIBN-MWNT composite indicate a covalent bonding between PMMA and MWNT due to the opening of π-bonds of the nanotubes, which is related with a possible proposed reaction scheme.