The effects of mechano-chemical treatment on the surface characteristics and sorption properties of hydrotalcite were studied. Non-milled (crushed) and milled samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), particle size analysis and specific area. A milling time of 2 h decreased the particle size of the hydrotalcite samples from 21 to 8.0 nm, the specific area from 97 to 5.7 m2 g–1 and the total pore volume from 0.41 to 0.01 cm3. After the crushed and milled samples had been separately calcined at 500°C, they were agitated with 10–2m Na2MoO4 aqueous solutions for 48 h. The molybdate ion content in the regenerated non-milled hydrotalcite samples (HTc-MoO4) was found to be 6.0 meq g–1 while in the milled hydrotalcite (HTm-MoO4) samples this content was 2.5 meq g–1. The lower molybdate content was thought to be a result of compaction and, hence, reduced reactivity of the milled HT samples.