In previous studies, we focused on a mechanochemical process for recycling fl y ash for use in cement; this process was expected to immobilize heavy metals in the fl y ash, a desirable outcome in light of the fact that recycled fl y ash is commonly used in the synthesis of inorganic materials. Here, we investigated the leaching of lead (Pb) from fl y ash treated by a mechanochemical process and from cement prepared from the treated fl y ash. We used lead oxide (PbO), a typical Pb compound in fl y ash, as a model substance. Mechanochemical treatment of the fl y ash inhibited Pb leaching by 93%, and further inhibition (more than 99.9%) was observed in cement produced from the treated fl y ash. During the mechanochemical treatment, PbO was reduced to Pb by iron from the stainless-steel mill used for processing, and the lower solubility of Pb in water resulted in immobilization of the Pb.