Wastewater generated from the coking processes has high load of organic as well as inorganic pollutants which requires the application of effective treatment techniques. In the present work, treatment of coking wastewater (CWW) through catalytic thermolysis has been carried out in batch mode with varying parameters such as type of catalyst, catalyst mass loading, pH, temperature and time. This process was followed by adsorption as second stage treatment process. The final parameters obtained are as Chemical Oxygen Demand (COD) 20 mg/L, cyanide 0.42 mg/L and nil amount of phenol from the high initial organic and inorganic load. The study aims reduction of COD, phenol, and cyanide content in the wastewater to the permissible limits. The mechanism and kinetics of thermolysis process have been also presented in this study.