Abstract:In this paper,the polyphenylacetylene(PPA) is synthesised by the polymerization of phenylacetylene with two kinds of catalysts,anhydsous AlCl3and (Ph3P)2PdCl2. Using anhydrous AlCl3 as catalyst,the cis-trans PPA is obtained. And using (Ph3P)2PdCl2,the trans-cis PPA is found. Therefore,the polymerization of phenylacetylene may follow complex catalysis mechanism when anhydrous AlCl3 is used as a catalyst and it may follow metathesis catalysis mechanism when (Ph3P)2PdCl2 is used.