Sodium hydroxide (lye) and silica can be recovered in pure form from the alkaline sodium silicate waste of Nuclear Fuel Complex, Hyderabad. Electrolytic method was used to amalgamate the sodium present in an electrolyser with flowing mercury as cathode and nickel as anode. The amalgam is then denuded with water in a graphite packed tower to recover mercury for recycling to the electrolyser and sodium hydroxide lye. Sodium hydroxide lye can be recycled in the zirconium oxide plant. Silica is recovered from the spent electrolyte by ion exchange method using cation exchange resin. Both the process details are described in this paper, with experimental data useful for the scale up. The process converts waste to value products. (author). 3 figs., 2 tabs.