PVA films were crosslinked with dimethylol dihydroxy ethylene urea (DMDHEU) and three polycarboxylic acids of butanetetracarboxylic acid (BTCA), citric acid and malic acid Different factors influencing the crosslinking treatment with BTCA were investigated including BTCA and sodium hypophosphite (SHP) concentration, curing temperature and time. The cured films was extracted with boiling water and gel fraction was calculated based on weight change of the PVA films. The gel fraction of PVA films increased with increasing curing temperature and time. And the resistance to water and thermal stability of the crosslinked PVA films improved with the BTCA crosslinking treatment. While crosslinking with citric acid gave the highest gel fraction among the crosslinkers, crosslinking with malic acid showed the highest absorbancy in 0.9% saline solution, which was attributed to lower crosslink density and high number-average molecular weight between crosslinks. The superabsorbent PVA films could be prepared by adjusting the crosslinking condition of PVA with polycarboxilic acids.