Cellulose tri-stearate (CTs) was synthesized employing triﬂuoroacetic anhydride (TFAA), stearic acid (SA), with microcrystal cellulose (MCC) and characterized with FT-IR and 1
H-NMR. The degree of substitution of CTs was determined by the traditional saponiﬁcation method and 1
H-NMR. The thermal properties of CTs were investigated by the thermogravimetric analysis (TGA) under Ar flow in dynamic heating conditions. Thermal stability, activation energy, as well as the degradation mechanism of the decomposition process were revealed. The results showed that the thermal stability of CTs is superior to that of raw materials-MCC, and that the degradation of CTs in argon is a first-order weight loss; the initial decomposition temperature and the temperature corresponding to maximum degradation rate (Tp
) increase with an increase in heating rate. The activation energy values were calculated with the Ozawa method, Coats-Redfern method and Kinssinger method, respectively. Analyses of experimental results suggest that the degradation mechanism 0.10 < α
< 0.80 is F2 type, A3 for α
< 0.1, and R3 for α
> 0.80. The degradation mechanism of CTs in the whole conversion range is a complex mechanism, and is the combination of A3, F2 and R3.