Abstract: Two-dimensional IR spectrum was applied to the analysis of cellulose. One-dimensional IR spectrum,second derivative IR spectrum and deconvolution IR spectrum of absorbent cotton fiber were obtained in the temperature range of 293-393 K. It was found that the band resulting from α-cellulose appeared near 559 cm-1 and the bands resulting from β-cellulose appeared near 893,1 206,1 235 cm-1. With increasing temperature,infrared absorption intensity of 559 cm-1 decreased,while those of 893,1 206,1 235 cm-1 increased. Effect of temperature on structure of absorbent cotton fiber was further studied using two-dimensional IR spectrum. It was found that the sequence of intensity increases of IR characteristic absorption peaks was 893 cm-1>1 235 cm-1>1 206 cm-1>559 cm-1 with increasing temperature.