Nickel zinc aluminum layered double hydroxides (NiZnAl-LDH) were synthesized by co-precipitation and co-formation methods using urea in polyvinyl alcohol (PVA) solution. On the obtained nanocomposites nickel-zinc sulfide (NixZn1-xS; x=0.25, 0.5, 0.75) nanoparticles were synthesized by successive ionic layer adsorption and reaction (SILAR) method at room temperature (25°C). The photocatalytic degradation of Ponceau 4R (P4R) and Rhodamine 6G (R6G) with obtained LDH and sulphide nonmaterials were studied under visible light source (150W). NiZnAl-LDH and NixZn1-xS/NiZnAl-LDH (x=0.25, 0.5, 0.75) nanocomposites were characterized by Ultraviolet (UV) spectratrometer, X-ray diffractometer (XRD), Energy-dispersive X-ray (EDX), Fourier transform infrared (FTIR) spectratrometer and Scanning electron microscopy (SEM).