In this study, we have synthesized nano Aluminum Fluoride (nAF) nanoparticles by the sol-gel method and studied the nano-sized morphology of crystals. In the other section, the PVC/NiAl2O3/AlF3 (nPNA) nanocomposite was successfully prepared and characterized by FT-IR, and HRTEM techniques. FTIR peaks of the PVC and nPNA have been shown spherical shape of PVC and also spherical shapes nanoparticles of nPNA loaded on PVC. A solvothermal method has been successfully introduced and applied for catalyst efficiency. This nanocomposite was used for the removal of Congo red dye. For this purpose, the morphology and the structure of crystals have been changed by modification on precursor gel. Meanwhile, precursor gel preparation and the interaction on the nano-sized area have been studied. This study exhibited that PVC/NiAl2O3/AlF3 (nPNA) nanocomposite is an effective catalyst for the synthesis of some organic derivatives. The results show that the as-prepared nanocomposite is an efficient catalyst and that PVC/NiAl2O4/AlF3 nanocomposite can be used in the next-generation of some organic reactions and faster production of various materials. Manuscript profile