In the reported study, the polymerization of phenylacetylene to polyphenylacetylene was accomplished with the combined catalysts triethyl aluminum and titanium tetraethoxide. The progess of the reaction was monitored by gas chromatography. The parameters included temperature ( minus 80, 25, 140 degree C), solvent (benzene, chlorobenzene, toluene, cyclohexane, and nitrobenzene), mole ratio of catalysts (Al/Ti; 1. 5, 3. 0, 4. 5, 6. 0, and 9. 0), aging times of catalysts (2, 10, and 40 min), and order of addition of reagents. Derivatives of polyphenylacetylene were obtained by the acylation of polyphenylacetylene with p-nitrobenzoyl chloride, the sulfonation of polyphenylacetylene with benzenesulfonyl chloride, and the formation of polyphenylacetylene complexes with complexing agents such as bromine, iodine, iodine chloride, boron trifluoride, and ferric chloride. A new phenylacetylene-acetylene product mixture was produced by the polymerization of phenylacetylene and acetylene at 25 and minus 80 degree C. The electrical conductivity of polyphenylacetylene and its derivatives is in the range of 10** minus **1**0-10** minus **3 OMEGA ** minus **1 cm** minus **1.