The study aimed to improve the effectiveness of dyes and pigments wastewater treatment. Hybrid system of adsorption and coagulation was applied for the reduction of COD, color, turbidity and TSS. Activated carbon adsorbent was prepared from a waste of sugar industry boiler. It was processed through physicochemical treatment with sulfuric acid following grinding, sieving, washing and drying unit operations. Combined wastewater of dyes and pigments manufacturing plant was treated with a hybrid process of coagulation and adsorption. FeCl 3, FeSO 4and Alum coagulants were tested individually and found them less effective. It was revealed that FeCl 3 coagulation, adsorption and hybrid process reduced COD (41, 51 and 54%), Color (67, 70 and 89%), turbidity (69, 71 and 90%) and TSS (82, 93 and 97%) respectively. Combination of FeCl3 -SBFA (Sugarcane Bagasse Fly Ash) proved 90% efficient in removal than coagulation as an individual process. 4g adsorbent dose was optimized for this hybrid process