The combination of organic and inorganic moieties resulted in advantageous materials with excellent physicochemical properties and reduced production costs. These organic-inorganic composites exhibited properties suitable for a large range of applications. This study introduces a simple strategy that combines Ni(OH)2 and Ag nanoparticles via thiol organic molecules. The obtained NiO–S(OH)2–Ag nanoparticles were fully characterized by FTIR, SEM, TEM, XPS, Raman, and ATG. The changes in morphology, covalent surface grafting, dispersion of silver nanoparticles, and thermal properties were investigated. NiO–S(OH)2–Ag exhibited an exceptional catalytic activity in reducing the pollutant 4-nitrophenol (4-NP). The kinetic rate constant was recorded as 0.388 cm-1, corresponding to a conversion uptake of 93.5 %. These values represent a significant improvement over metal-based catalysts of similar or identical compositions previously reported. Both Ag incorporation and S(OH)2 grafting appear to be, at least partly, responsible for the above results. Due to their outstanding catalytic properties and cost-effective production method, the synthesized NiO–S(OH)2–Ag is expected to exhibit excellent performance in the catalytic degradation of industrial pollutants.