Aluminosilicate microspheres are a valuable fraction of coal fly ash with diverse applications due to their low density. Currently, there is no efficient and ecologically rational method of cenosphere recovery from fly ash. A combination of dry methods for the recovery of both fine ash particles and aluminosilicate microspheres from coal fly ash is presented. It is comprised of fluidised bed separation followed by screening and pneumatic separation in a free-fall air chamber. Fluidised bed separation was assisted by a mechanical activator to prevent agglomeration. This step reduced the portion of material that required further treatment by 52–55 wt.%, with the recovery of microspheres exceeding 97%. Then, the concentrates were individually subjected to pneumatic separation. The final separation product for the fly ash containing 0.64 wt.% cenospheres was a cenosphere concentrate that constituted about 17 wt.% of the initial fly ash. The recovery of cenospheres was around 81%. Usage of a combination of dry methods allowed for maintaining almost 83 wt.% of the raw material in its dry form. Furthermore, the produced fly ash grain fractions could be used for different industrial purposes.