Multi-parameter effect consideration during metakaolin conversion gives the best optimum processing conditions. Kaolin deposits have different properties, which makes it vital to establish optimum conditions for a distinctive kaolin deposit. The Response Surface Methodology under Box-Behnken Design has been adopted in the current study to optimize the processing conditions for kaolin-to-metakaolin conversion. The temperature of 765.608 °C, the rate of 9.775°C/min, and 6.465 h of soaking were the optimum conditions for yielding the highly reactive (1382.15mg Ca (OH)2/g) metakaolin. The typical reflections at 2θ of 14.32 and 29.03°attested to the existence of kaolinite in the kaolin sample, which then disappeared in the optimized metakaolin as confirmed by X-ray diffraction. The Fourier-transformation infrared spectroscopy confirmed the existence of kaolinite in the sample with reflections at the bands 3692, 3650, and 3620 cm-1 which disappeared to form a broad band in this region, which validates the formation of reactive amorphous metakaolin.