The physicochemical properties and mineral separation of a phosphate rock with siliceous and carbonates gangues were investigated. The results showed that this ore mainly contains flour-apatite, calcite and quartz. The partial substitution of (CO3)2- for (PO4)3-exists. There are Ca,P,O,Si and C elements on the rock surface,and their amounts are different from those in the bulk, especially the Si and C elements. The P2O5 content tends to firstly increase and then decrease with the reduction of ore particle size. However the contents of A.I and L.O.I show a trend of first decrease and then increase. This indicated that the phosphate and gangue minerals are upgraded in different size particles. For fine ore particles with low P2O5 content, a reverse flotation with cationic collector was employed to separate quartz. The P2O5 grade is increased by 4% and high P2O5 recovery with 80% are obtained. Owing to the existence of carbonates gangues, the acid or weak acid conditions are suitable for flotation.