Nickel and magnesium hydrotalcite-like compounds (NiAlHT, MgAlHT) were investigated to remove fluoride ions from aqueous solutions in batch system. F − ions were determined in the remaining solutions using a fluoride ion selective electrode. Kinetic of the fluoride sorption from aqueous solutions by nickel hydrotalcite-like compound with different grain size were determined as well as the effects of Cl − , SO 4 2− and As(V) on the sorption kinetic. It was found that the adsorption rate is the highest using grains samples of 25–50 mesh and in about 600min the equilibrium was reached in all systems; the results were best fitted to the Elovich rate model equation which indicates that the sorption mechanism is trough a chemisorption process. Other anions interfere on the F − adsorption from bicomponent aqueous solution by NiAlHT and MgAlHT. NiAlHT is more efficient than MgAlHT to remove fluoride from the aqueous solutions.