A sol-gel polymerization has been employed to prepare organic aerogels through the reaction of resorcinol and formaldehyde with multiple organic acid as catalyst and cetyltrimethylammonium bromide as surfactant. The gels were dried under ambient pressure and carbonized at high temperature. The samples were characterized by methylene blue adsorption test, scanning electron microscopy (SEM), and X-ray diffraction analysis (XRD). The results indicated that the carbon aerogels are uniform spheres, and the microspheres were abundant in connected pore for the electronic transfering. The X-ray diffraction pattern showed two broad peaks, indicating that the materials are amorphous . The methylene blue adsorption test shows that there are a lot of mesoporous in the materiales and the surface area is as high as 740 m?g. Cyclic voltammetry (CV) was used to study the electrochemical performance of the materials . The test results show that the samples have perfect conductivity , high specific capacitance and stable performance with a longer cycle life. They could be used as the effective electrode materials for supercapacitors.