This paper is a critical overview on the experimental results on development of activation techniques to improve the catalytic activity of coal fly ash, in relation to its use as solid acid catalyst and catalytic support materials. Mechanical activation results in slight increase in silica percentage, amorphous nature, specific surface area and surface roughness, as evident by analytical measurements using XRF, XRD, FT-IR, BET surface area, TGA-DTA and SEM techniques. The mechano-chemical activation cangenerate sufficient activity on fly ash surface rendering its potential application in heterogeneous acid catalysis.