5,11,17,23tetrasulphonated25,26,27,28tetrahydroxycalix\[4\]arene was synthesized from calix\[4\] arene and concentrated sulfuric acid as raw materials, and characterized with a UVvisible spectrophotometer, thermal gravimetric (TG) and differential thermal analysis (DTA)；finally its electrochemical behavior was studied in the potassium dihydrogen phosphatesodium hydrogen phosphate buffer solution, and the results show that there is an irreversible reduction peak at about 0.93 V in the scan potential between -1.2 ~ 0.8 V, and the reduction peak potential changed with scanning speed.