The 0.1 mol•L −1 MgSO 4 liquor and 5 mol•L −1 NaOH liquor were prepared by MgSO 4 ·5H 2 O and NaOH as raw materials, and then different diameter nano-Mg(OH) 2 powders were prepared by chemical precipitation. The DTA-TG curves data obtained was by SDT 2960 simultaneous DSC-TGA analysis apparatus. The mensuration conditions were that rise temperature velocity was 15 • C·min −1 , gas was air. The kinetics was calculated by DTA-TG curves data and dα dt = k(1−α) n kinetics model. The results shown that nano-Mg(OH) 2 powders shape were stick or spherical, their diameter were 7, 12, 20, 40, 70 nm. Their thermal decomposition reaction apparent activation energies were 188. 065, 195.935,202.493, 210.178, 297.527KJ·mol −1 , the apparent activation energy increase with Mg(OH) 2 diameter. Their frequency factors were 2.721 × 10 15 , 9.246 × 10 15 , 4.251 × 10 16 , 6.067 × 10 16 , 3.866 × 10 23 , the frequency factors increase with diameter Mg(OH) 2 . Their reaction progression were 0.8296, 0.9321, 0.8743, 1.0275, 0.8903, the reaction progressions were fluctuated in 0.9108 (average) about.