Abstract: Poly-N-［5-(8-quiniolinol)ylmethyl］aniline was synthesized by the chemical oxidative polymerization of 5-(anilinomethyl)-8-hydroxyquinoline, which was synthesized from aniline, 8-quinolinol and methanal, using ammonium peroxydisulfate as an oxidant. Then, poly-N-［5-(8-quinolinol)ylmethyl］aniline/silica hybrid with fluorescence property was prepared via the surface modification of poly-N-［5-(8-quinolinol)ylmethyl］aniline using tetraethyl orthosilicate. This hybrid not only shows a strong visible emission centered at 480 nm, but also has good redox reversibility in both strong acid and weak acid electrolytes.