Novel ethylene diamine tetraacetic acid (EDTA)-modified zwitterionic hybrid materials were prepared via a sol-gel process. Their adsorption performances for Pb 21 ions were examined. Fourier transform infrared spectroscopy confirmed the reaction products. Thermogravimetric analysis revealed that the thermal stability of these hybrid materials could reach 200 C. Differential scanning calorimetry measurement showed that the addition of titanium butoxide could impact the crystallization transformation of these materials. Field emission scanning electron microscopy images showed that EDTA modification induced a decrease in the particle size. Adsorption experiments demonstrated that the optimal initial pH was 5. Moreover, we observed that the adsorptions for Pb 21 ions followed the Lagergren pseudo-second-order kinetic model, intraparticle diffusion, and Langmuir isotherm model. In addition, we found that the maximal Langmuir constant was 0.86 mmol/g. The negative Gibbs free energy values suggested that Pb 21 adsorption onto these samples was spontaneous in nature. The desorption experiment indicated that these samples could be recovered with aqueous HCl solution as a desorbent. These results suggest that the synthesized EDTA-modified zwitterionic hybrid materials are promising adsorbents that could be used to separate and recover heavy-metal ions from polluted wastewater. V C 2013Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014, 131, 39801.