Solid state synthesis of some new Mx-CuSb2O6-CuSb2O4 (Mx=None, Fe, Ni, Ce and Yb) nanocomposites was introduced in the present research study. The physicoelectrochemical properties of synthesized nanocomposites were investigated by different techniques, such as XRPDT, Rietveld, FTIR, FESEM, UV-Vis, VSM, CV and EIS. Rietveld analysis data revealed that all of the synthesized samples display the monoclinic crystal phase with the space group of P21/n. The estimated direct band gap energy of the obtained nanocomposites was in the range of 2.0 to 2.7 eV, which confirms that are active in ultraviolet-visible region. The VSM data indicated that the maximum magnetic behavior was found for Ni doped - Cu-Sb-O nanocomposite. Also, the catalytic performance of nanocomposites to synthesis 2-amino-4H-benzochromenes under ultrasonic and microwave was investigated. The considered parameters, such as solvent type, catalyst amount and reaction time, influencing the yield of the 4H-benzochromene reaction were studied. The maximum yield for the synthesizing of the 4H-benzochromene compounds was obtained when EtOH was used as the reaction solvent. The catalyst amount and reaction time were 15 mol% and 8min, respectively, under ultrasonic conditions, while benzaldehyde was used as an aldehyde derivative.