The nanocomposites based on organic-inorganic hybrid have been attracting much attention due to their potential applications used as new type of functional materials, such as colloidal stabilizers, electro-optical devices, and nanocomposites materials. The organic-inorganic hybrid of poly(acrylic acid-acrylonitrile)/attapulgite. P(A-N)/AT nanocomposites, were prepared by using in situ polymerization and composition of acrylic acid (AA) and acrylonitrile (AN) onto modified attapulgite (AT) nanoparticles. The resulting P(A-N)/AT nanocomposites were transformed into novel nano-adsorbent of poly(acrylic acid-acryloamidoxime)/attapulgite by further functionalization, i.e. P(A-O)/AT nano-adsorbent. The adsorption properties of P(A-O)/AT toward metal ions were determined, and the results indicated that the adsorbents with nanocomposite structure held a good of selectivity to Pb2+ among numerous metal ions. The maximum removal capacity of Pb2+ was up to 109.9 mg/g and it is notable to see that the adsorption removal of P(A-O)/AT nano-adsorbent for Pb2+ could achieve more than 96.6% when the initial concentration of Pb2+ was 120.0 mg/l. The kinetics, isotherm models, and conductivity were introduced to study the adsorption mechanism of P(A-O)/AT for Pb2+ and it was concluded that it could be chemisorptions process and the best coordination form took place when AO:AA:Pb2+ = 1:1:1. In addition, after simply treated with CTAB, P(A-O)/AT nano-adsorbent showed better adsorption properties for phenol than the same kinds of materials. (C) 2010 Elsevier B.V. All rights reserved.