Oil palm empty fruit bunch (OPEFB) cellulose fibre has been widely used as a reinforcing filler in polymer composites. Surface modification of OPEFB fibre was aimed enhancing inter-phase adhesion with a poly(lactic acid) matrix. In this study, the OPEFB fibres were pre-treated in a sodium hydroxide solution. Surface compositions and thermal stability of the fibres were studied using ATR-FTIR and TGA techniques, respectively. The pre-treatment resulted in the removal of non-cellulosic components leaving purer fibres. In addition, an acetylation of OPEFB cellulose fibres by acetic anhydride was conducted under solvent free condition at room temperature (30 °C). The acetylation reaction was catalyzed by iodine. The degree of substitution monitored by solid state 13C NMR depended upon reaction time and molar ratio of OPEFB cellulose and acetic anhydride. Crystalline structure and morphology of the partial acetylated fibres were investigated using WAXD and SEM, respectively.