Abstract: Fine-grained minerals have large specific surface area and high surface energy, which makes it difficult for flotation reagents to adsorb selectively and flotation separation. This work used fine-grained (−10 μm) hematite and quartz as the research objects, polyethylene oxide (PEO) and starch as the selective flocculants and depressants, respectively, combined with flocculation flotation testing, sedimentation testing, and SEM scanning analysis, to determine the viability of the microfine-grained hematite/quartz asynchronous flocculation process. The flotation results demonstrated that starch and PEO can be utilized as selective flocculants to separate quartz and hematite using dodecylamine as the collector. The best separation result was obtained with grade 60.4% and recovery 81.8% of the concentrate when the dosage and molecular weight of PEO were 50 g/t and 800w, respectively. According to the results of sedimentation test and SEM analysis, PEO and starch have strong flocculation effects on quartz and hematite, respectively. Moreover, PEO has a stronger impact on quartz than that of starch on hematite. Asynchronous flocculation, which was achieved in the flotation process by the successive addition of PEO and starch, accentuates the differences in surface characteristics of the two minerals and creates the right circumstances for effective separation of fine-grained quartz and hematite.