In this research, a new facile and efficient route has been employed to prepare poly(3,4-ethylenedioxythiophene)/titanium dioxide (PEDOT/TiO2) nanocomposites using chloroform-acetonitrile binary solvents. Two homogenized and stabilized chloroform-based nanofluids were separately prepared with titanium dioxide nanoparticles in the presence of two anionic and cationic surfactants, i.e. sodium dodecylbenzene sulfonate (SDBS) and tetradecyltrimethylammonium bromide (TTAB) by sonication. Next, 3,4-ethylenedioxythiophene (EDOT) monomer was added to these nanofluids. A solution of iron (III) chloride oxidant in acetonitrile was then slowly poured into the previous mixture. The chemical oxidative polymerizations resulted in the preparation of PEDOT/TiO2 in a medium of the two mentioned miscible organic solvents. To compare the results obtained, pure PEDOT as a reference was also prepared by a similar manner to that of used to prepare PEDOT/TiO2 nanocomposites. UV–vis diffuse reflectance spectra (DRS) were utilized to investigate the effect of the incorporated nano-TiO2 particles on optical properties of PEDOT. X-ray diffraction (XRD) patterns obviously showed the characteristic peaks of embedded TiO2 nanoparticles on the diffractogram of the resulting PEDOT. Surface morphology of the nanocomposites was evaluated by scanning electron microscopy (SEM) analyses. Transmission electron microscopy (TEM) images demonstrated that the TiO2 nanoparticles were uniformly dispersed in both PEDOT bulks. Thermogravimetric analysis (TGA/DTG) clearly showed that both PEDOT/TiO2 nanocomposites are more stable toward heat compared with the pure PEDOT sample.