Nanocomposites of polyaniline(PANI) and the macrocycle thiacalix[4]arene tetra sulfonate(TCAS) were successfully synthesized in feed ratios of 1:0.25, 1:0.50 and 1:0.75 by three prevail synthetic methods, i.e. in situ polymerization, emulsion polymerization and solution casting technique. The structures of the nanocomposites were confirmed by FTIR, UV-Vis, XRD, SEM, and TEM techniques. The conductivity was measured by a four probe method. The conductivity was recorded to be as high as 105 × 10 2S cm 1for the nanocomposite with a nanometer size structure and homogeneously distributed morphology. The electroactivity of the nanocomposites was approved by cyclic voltammetry(CV) and impedance spectroscopy technique(EIS). The antioxidant ability and thermal property of the composites were further studied. Preliminary studies have evidenced the production of conductive nanocomposites with good thermal property and relatively good solubility in N-methyl 2-pyrrolidone(NMP), with the antioxidant activity reaching up to 80%. Nanocomposites of polyaniline (PANI) and the macrocycle thiacalix [4] arene tetra sulfonate (TCAS) were successfully synthesized in feed ratios of 1: 0.25, 1: 0.50 and 1: 0.75 by three prevail synthetic methods, ie in situ polymerization, emulsion polymerization The structures of the nanocomposites were confirmed by FTIR, UV-Vis, XRD, SEM, and TEM techniques. The conductivity was measured by a four probe method. The conductivity was recorded as be as high as 105 x 10 2S cm 1 for the nanocomposite with a nanometer size structure and homogeneously distributed morphology. The electroactivity of the nanocomposites was approved by cyclic voltammetry (CV) and impedance spectroscopy technique (EIS). The antioxidant ability and thermal property of the composites were further studied. have evidenced the production of conductive nanocomposites with good thermal property and relatively good solubility in N-methyl 2-pyrrolidone (NMP), with the antioxidan t activity reaching up to 80%.