The influence of reaction conditions on the preparation of poly(ether ketone) by Friedel—Crafts acylation of diphenyl ether and isophthaloyl chloride in 1,2-dichloroethane with aluminium trichloride as a catalyst was examined. The following factors were considered: catalyst quantity, reaction temperature, monomer ratio and polymer concentration. One of the characteristics of this reaction was precipitation of polymer/catalyst complexes. Polymerization proceeded even in the precipitate by the reaction between the chain-ends. At low polymer concentrations, crystalline grains appeared, and the reaction between the chain-ends was accelerated. As the polymerization of the precipitate proceeded, the precipitate could contact more effectively with fresh solvent because the hydrogen chloride formed by the acylation was easily removed from the reaction site.