In this paper,Calixarenes 5,11,17,23 tetrasulfonic acid, tetrasodium salt was synthesized by the reaction of calixarenes and H 2SO 4. The yield of the Calixarenes 5,11,17,23 tetrasulfonic sodiums was improved to 20%～30% using the method that the reactant (filitrated H 2SO 4) was dissolved in a little amount of NaCl saturated solution and then the water was volatilized at room temperature.
