A series of fine copolymer particles from 8-aminoquinoline (AQ) and o-phenetidine (PD) were simply synthesized by a chemical oxidative polymerization in three aqueous media. The potential and temperature of polymerization solution were effectively employed to pursue the polymerization progress. The molecular and morphological structures of the resulted AQ/PD copolymer particles were thoroughly characterized by IR, UV-vis, NMR, gel permeation chromatography, laser particle size analysis, and atomic force microscopy. An important dependency of polymerization yield, structure, and properties of the particles on AQ/PD ratio, temperature, and medium of polymerization has been found. The size of the AQ/PD copolymer base particles exhibits a monotonic decrease with increasing AQ content from 5 to 100 mol %. A facile technique of preparing semiconducting pure nanoparticles by introducing the AQ units with positively charged quaternary ammonium groups but without adscititious stabilizer or sulfonic groups is created for the first time. Both the molecular weight and bulk electrical conductivity of the copolymers display an utmost at AQ content of 5 mol %, while polymerization yield and bulk electrical conductivity seem to be the highest at the lowest polymerization temperature of 5 ° C. The solubility and film formability of the copolymers are superior in highly polar solvents and achieve the best at an AQ content of 5-10 mol %.