In the present research work Taguchi method was applied to investigate the effect of reductive leaching parameters and mechanical pretreatment of ilmenite on nano synthetic rutile synthesis. The parameters such as ilmenite to acid mass ratio, ilmenite to iron powder mass ratio, milling time and initial leaching temperature were selected for optimization of experimental conditions. Consequently, the milling time was the most effective parameter on synthetic rutile preparation compared to the rest of the selected parameters. The optimum conditions obtained were as follows: milling in Argon atmosphere 40min, initial reaction temperature 100°C, ilmenite to hydrochloric acid mass ratio 1:9.55 and ilmenite to iron powder mass ratio 1:0.075. The characterization of products indicated that the prepared powder with milling time 40min, temperature 100°C, ilmenite to hydrochloric acid mass ratio 1:12.8 and ilmenite to iron powder mass ratio 1:0.05 had particles size of less than 100nm. The analysis further confirmed that synthetic rutile nano powder had 91.1% TiO 2 . The nano powder obtained under the optimized condition had a BET surface area of 54.6m 2 /g.