Synthesis of microcrystalline cellulose (MCC) from jute sticks has been studied and reported in this work. The successful removal of lignin and hemi-cellulose has been confirmed through Fourier Transform Infrared (FTIR) spectroscopic technique. X-ray Diffraction (XRD) technique has been used to measure the crystal size and crystallinity index. The FTIR analysis revealed that the acid hydrolysis had an effect on the crystalline of the fibre; however it did not influence the chemical components of the fibres. Pharmaceutical standard tests were done. Higher concentration of sodium chlorite produces minimum particle size and the effective thermal degradation occurs at 340 °C.