Cellulose triacetate (CTA) was prepared from cotton linter and pulps which contain various contents of α-cellulose. CTA which contains 2.8 of degree of substitution (DS) and 222 of degree of polymerization (DP) was obtained from V-81 pulp under the heterogeneous system. The DS was measured by the titration method, and the DP was obtained by measurement of viscosity. FT-IR spectometer (FT-IR 6300, JASCO) was used to analyze the chemical structure of raw materials and cellulose triacetate, and X-ray diffractometer (X-pert MPD PW3040, Philips) was used to confirm the crystal structure and to calculate the relative crystallinity index (RCI). As α-cellulose content in pulp increased, the acetylation yield increased. Besides with a kind of pulp, it contains insoluble residue which was mainly formed due to the formation of glucomannan triacetate and xylan diacetate during the esterification.