Zirconium tetrachloride was produced in a pilot plant fluidized bed reactor via the carbochlorination reaction of zirconia. Minitab software 17 was used for the design of experiment with response surface methodology (RSM) for both semi batch and continuous processes. The operating temperature (800-1200 °C), reaction time (30-90 min) and mean particle size (MPS) (70-130µm) were chosen as the range of operating conditions at semi-batch mode. Also, the ranges of operating variables at the continuous mode were chosen to be the operating temperature(1000-1400°C), chlorine concentration (3-5mol/m 3 ) and mean particle size (MPS) (70-130µm). The coefficients of determination (R 2 ) for semi-batch and continuous modes by RSM analysis were 99.54% and 99.94%, respectively. The optimal operating conditions was predicted to be the Cl 2 concentration of 3mol/m 3 , temperature of 1380 °C and the mean particle size of 70µm in which the maximum chlorine conversion of 98.26% was obtained at continuous process. The optimum operating conditions for semi-batch process were found by using RSM modelling to be 1200°C, 90 min and 70 µm, in which the maximum zirconia conversion of 92.7% was obtained.