Abstract: Aluminum and fluorine are recovered from fluorine containing waste materials from the production of aluminum metal (FCWM) as ALF.sub.2 OH hydrate by a process comprising: leaching FCWM with dilute sulphuric acid at a pH value within the range of 0-3; if needed adding aluminum in an acid soluble form; adjusting the pH value of the aqueous phase to a value within the range 3.7-4.1 at the end of the leaching period by addition of a caustic aqueous solution; precipitating silica at a temperature not exceeding 60.degree. C.; separating the reaction mixture into a solid phase containing precipitated silica and non-soluble residues of the FCWM and a purified solution; and precipitating AlF.sub.2 OH hydrate from the purified solution at a temperature within the range 90.degree.-100.degree. C. and at a pH value not exceeding about 4.1 by controlled continuous addition of an aqueous caustic solution. Reducing and/or non-oxidizing operating conditions are maintained during all these process steps. The precipitated AlF.