Compared to a batch reactor, where all reactants are initially charged to the reactor, the semi-batch reactor presents serious advantages. The feed of at least one of the reactants provides an additional way of controlling the reaction course, which represents a safety factor and increases the constancy of the product quality. The aim of this study was to investigate the characteristics of thermal hazard such as a feed time, catalysis concentration and solvent concentration in methylthioisocyanate(MTI) synthesis reaction process. The experiments were carried out by the Multimax reactor system and Accelerating rate calorimeter(ARC). The MTI synthesis reaction process has many reaction factors and complicated reaction mechanism of multiphase reaction. Through this study, we can use as a tool for assessment of thermal hazard of other reaction processes by applying experiment method provided.