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A novel soluble π-conjugated polymer, poly [(3-acetylpyrrole-2, 5-diyl) p-(N, N-dimethylamino) azobenzylidene] (PAPDMAABE), was synthesized by condensation of 3-acetylpyrrole with 4-aldehyde-4-dimethylaminoazobenzene (ADMAA). The chemical structure of PAPDMAABE was characterized by Fourier transform infrared spectroscopy (FTIR),1H-NMR, and UV-Vis-NIR spectra. Transmission electron microscope (TEM) analysis for PAPDMAABE indicates that part of PAPDMAABE is in crystal state, due to the short-range order of the polymer. Thermogravimetric analysis (TGA) curve shows that the polymer has good thermal stability and its decomposition temperature is 248℃. The optical band gap of PAPDMAABE obtained from the optical absorption spectrum is about 1.73 eV. The resonant third-order nonlinear optical property of PAPDMAABE at 532 nm was studied using degenerate four-wave mixing (DFWM) technique.The resonant third-order nonlinear optical susceptibility of the polymer is about 7.48× 10-8 esu.