Two kinds of dit diethylenetriamine (2E3A) intercalation compounds of alpha-zirconium phosphate with different interlayer distances could be obtained by regulating the reaction time and temperature. Phase I (d = 10.2 Angstrom) slowly transforms to Phase II (d = 15.8 Angstrom) with transformation enthalpy of 30 kJ.mol(-1) in 2E3A aqueous solution. The conformation of 2E3A in Phase I and Phase II were confirmed to be bent and all trans (straight) forms by P-31 MAS NMR and XRD measurements. Two phases have different adsorption behavior for gaseous carboxylic acids. Phase II can adsorb considerable amount of carboxylic acids whereas Phase I adsorb a little.