As for certain high ash and difficult floatable fine coal, the coal quality characteristic is the frangible and easyly-clayed main gangue mineral kaolinite, and the high content of fine-grade and intermediate density grade materials. In order to reduce tiny slimes pollution and to increase quality and recovery rate of concentrate, we used cyclonic-static micro-bubble flotation column and XFD-3 flotation machine to experiment on separation process. It probed into re-concentration after grinding rough refined coal, classified flotation process and selective agglomeration-flotation process these three technical processes. The comparison of flotation machine test result showed that, using the flotation column as separation equipment, process of re-concentration after grinding rough refined coal could obtain the best refined coal accumulation index. When medicaments dosage is kerosene 800 g/t, GF 300 g/t, and sodium hexametaphosphate 1500g/t, refined coal production rate of flotation column is 59.47% and ash content is 10.63%.