Catalytic properties of Zirconium phosphonates layered structure (ZPLS) catalysts with organic sulfonic acid pendant groups have been studied. The NaOH titration demonstrated the presence of sulfonic acid groups. The ZPLS contained acid sites per weight similar to or acetic acid with ethanol were studied as test reactions. Accessibility of the reactants to the acid sites present in the interlayer spacing of ZPLS was a determining factor for the activity. Thus the activity depended on the ease of swelling and particle size of the ZPLS.