Influences of precipitating condition of gibbsite from sodium aluminate solution on particle size, specific gravity, specific surface area and formation ratio of boehmite after calcination of gibbsite were studied. Gibbsite obtained from a solution of Na
2O/Al
2O
3 molar ratio 1.4 has the maximum specific gravity and minimum specific surface area and indicated maximum particle size of 6.33 μm. In this case, the formation ratio of boehmite was 33%. Gibbsite particles are coarsened with rising the stirring temperature and lowering the keeping temperature. The reaction rate of gibbsite decomposition to boehmite, χ-Al
2O
3 and γ-Al
2O
3 was investigated by D. S. C. technique. The decomposition at an early stage from a part of gibbsite to boehmite at 220°C is controlled by chemical reaction, and that at a later stage is controlled by nucleation of boehmite. The remaining gibbsite changes into χ-Al
2O
3 at 300°C being controlled by chemical reaction. The change from boehmite to γ-Al
2O
3 at 500°C is controlled by nucleating reaction.
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