Sodium azide is a key component in the automobile air bag. When dissolved in aqueous solution, it reacts rapidly with water to form hydrazoic acid which is a highly toxic chemical and is strongly regulated by government. In the present study, adsorption of hydrazoic acid from aqueous solution by macroreticular resin is investigated. This method can provides a convenient means for dealing with the toxic hydrazoic acid. Experimental tests of batch equilibrium adsorption and continuous column adsorption of hydrazoic acid were conducted and the test results were employed to establish adsorption isotherm and to evaluate the column adsorption efficiency. The test results revealed that the multilayer adsorption isotherms, like the modified Langmuir or Jossens model, are needed to adequately describe the hydrazoic acid adsorption equilibrium between the liquid and solid (resin) phases. In the column adsorption process, a theoretical model was adopted for representing the hydrazoic acid change in the aqueous solution exiting the column and the verified theoretical model significantly facilitates prediction of adsorption breakthroughs and column design. Regeneration of exhausted resin was investigated. Solution of 10% (w/w) NaCl was found to be a very efficient regenerant.