The research of negative effect of calcination to catalytic performance of coal char-loaded TiO2 catalyst in styrene oxidation with hydrogen peroxide as oxidant has successfully done. The effects of calcination step to catalyst properties were characterized with Fourier Transform Infra Red (FTIR), X-ray Difraction (XRD), nitrogen adsorption, Field Emission Scanning Electron Microscopy (FESEM), and Transmission electron microscopy (TEM). The catalytic performance of the catalysts has been investigated in styrene oxidation with hydrogen peroxide as oxidant. The catalytic study showed the calcination step influenced to catalytic properties and could decrease the catalytic performance of coal char-loaded TiO2 catalyst in styrene oxidation.