A process for hydrofluoric acid digestion of silica/alumina matrix material for the production of silicon tetrafluoride which comprises:
- (a) reacting inorganic silica/alumina matrix material with hydrofluoric acid to produce silicon tetrafluoride gas;
- (b) purifying said silicon tetrafluoride gas by condensation removal of contaminants in one or more cold trap(s);
- and
- (c) reacting the purified silicon tetrafluoride gas of step (b) above with aqueous sodium fluoride to form a solution/slurry of fluorosilicate salt;
- (d) delivering said solution/slurry of step (c) above to a filter press to separate sodium fluorosilicate powder from said solution/slurry;
- (e) drying and then introducing said sodium fluorosilicate powder to a kiln at a temperature of about 600.degree. C. to 650.degree. C. to form silicon tetrafluoride gas and sodium fluoride powder;
- (f) collecting said silicon tetrafluoride gas and/or said sodium fluoride powder of step (e) above.