The present invention provides a process for crosslinking of polyallylamine hydrochloride wherein an aqueous solution of polyallylamine hydrochloride is partly neutralized with alkali and epichlorohydrin is added. The aqueous solution is dispersed in an organic medium containing a surfactant. This leads to gelation in individual droplets. The crosslinking in individual gel beads is completed by raising the temperature. The resulting beads are then separated, washed with water, treated with an organic solvent and dried. The method maximizes the yield of crosslinked polyallylamine hydrochloride particles in the range 60-100 mesh.