Fligh incilecular weight powdery polyacrylonitrile (PAN) polymers were prepared by aqueous suspension polymerization employing itaconic acid (IA) as comonomer and alpha,alpha'-azobisisobutyronitrile (AIBN) as initiator at 60 degrees C. PAN polymers obtained with different monomer ratios were characterized by EA, DSC, FFIR and XRD. It is investigated that the oxygen element content in PAN polymers increased with the increase of required IA amounts in the feed and heat-treatment temperatures. DSC curves of PAN copolymers exhibited the triplet character, owing to the exothermic cyclization and oxidative reactions during heat-treatment process. Introduction of IA in the feed relaxed exothermic reactions of PAN polymers under air atmosphere. Structure and crystallinity changes were affected by required IA amounts in the feed and enhancement of heat-treatment temperatures. The characteristic functional groups (including C N, C=O, CH2) presented in FTIR spectra of PAN polymers indicated copolymerization reaction of AN and IA. Existence of sonic organic groups (C-O, C=C and/or C=N) indicated formation of ladder like structure during heat-treatment process. PAN homopolymer had the better crystallinity (mainly peak intensity and peak area around 2 theta = 17 degrees) than most RT-PAN copolymers. When heat-treatment temperature is around 210 degrees C, peak intensity, peak area, L, and Cl of HT-PAN polymers corresponding to samples 1# and 2# got maxima, while crystallinity became weak at higher heat-treatment temperatures. (C) 2008 Elsevier Inc. All rights reserved.