In this work, novel organic-inorganic hybrid nanocomposites M + /PO 3 − (M = 2,2′-dibenzimidazolyl butane) were prepared by soft chemistry method. The synthesis was done by ion exchange method between sodium metaphosphate anions (yNaPO 3 ) and 2,2′-dibenzimidazolyl butane dichlorhydrates cations (xMCl 2 ) in aqueous media. The MCl 2 organic salt and the M + /PO 3 − hybrid nanocomposites were characterized by using spectroscopic and microscopic analyses. The FTIR and Raman spectroscopy are showed new bands in the hybrid nanocomposites structure, which proved the interactions between PO 3 and NH of MCl 2 molecules. The UV-Vis results of MCl 2 and M + /PO 3 − materials showed a broad absorption band in 200-300 nm regions, originating from phosphate and benzimidazole molecules. The X-ray diffraction was showed the appearance of new peaks attributed to the phosphate (PO 3 ) and a reduction of the intensity of the benzimidazole peaks. The TEM images are showed changes in appearance and size of hybrid materials. Moreover, the surface of hybrids became less dark and the size of M + /PO 3 − nanocomposites diameter was < 50 nm. The EDX analysis results revealed the presence of carbon, oxygen, and phosphate, confirming the interactions between phosphate and MCl 2 organic salt.