Abstract: Spent pot-lining(SPL)of aluminium electrolytic reduction cells is currently the largest hazardous solid waste with high fluoride content in aluminium industry， which pollutes the surrounding environment seriously. Fluoride and carbon from SPL were recovered by water wash， chemical leach and calcination process using Al₂(SO₄)₃·18H₂O solutions. The results show that the appropriate leaching conditions were time of 24h at 25℃， the recovery rate of carbon is 88% from SPL， and the carbon purity increases from 61.3% to 89.6%. The effects of time， temperature and pH value of solution on recovery rate of fluorine were investigated. Fluoride can be precipitated as Al₂((OH)_0.46F_0.54)₆H₂O and Na₅Al₃F₁₄. The appropriate conditions of fluoride recovery were temperature of 90℃， pH value of 5.5 and time of 180min. The maximum fluorine recovery rate is 99.7%. The main products were AlF₃ and Na₅Al₃F₁₄ after calcination.

Key words: spent pot-lining, aluminium electrolysis, recovery, aluminium sulfate, fluoride