In this paper, sodium oleate, polyacrylamide, soluble starch and sodium carboxymethyl cellulose were used as flocculants to study the flocculation and sedimentation behavior of microfine ilmenite. Sedimentation test shows that sodium oleate and polyacrylamide have good flocculation effect on ultrafine ilmenite. The flocculation rate of ilmenite can be further improved by the combination of sodium oleate and polyacrylamide. It was found that both flocculants could generate chemical adsorption with ilmenite surface, and they all react with Fe3+ on ilmenite surface. However, sodium oleate reacts with Fe3+ to form a water-insoluble iron oleate precipitate which coats the surface of the ilmenite and hinders the action of polyacrylamide and the remaining Fe3+. This problem can be avoided by adding polyacrylamide followed by sodium oleate, and the flotation recovery can be increased significantly.