Pitch fluoride is a new fluorine-carbon compound which has an excellent water repellency with a contact angle of more than 145 degrees, thermal resistance and high solubility in some fluoro solvents. In this study, various types of coal tar pitch were directly fluorinated by fluorine gas in order to prepare pitch fluoride at temperatures ranging from 50 degrees C to 130 degrees C. Depending on the softening point of each raw pitch, an optimum reaction temperature exists, at which pitch fluoride was synthesized at 200% increase in weight without decomposition of -C-C- bonds, and it was found that pitch with a high softening point is suitable as a raw material for synthesis.