Abstract:
A method for detoxification of spent catalyst from a fluorination process includes the step of hydrolyzing such spent catalyst in the presence of aqueous calcium chloride to produce insoluble compounds which are separable from the aqueous medium. The spent catalyst is one which includes at least one antimony halide, such as SbCl. sub. 5, SbF. sub. 5, SbCl. sub. 3 and/or SbF. sub. 3, usually with some halogenated hydrocarbons, such as partially chlorinated methane, partially chlorinated ethane and/or chlorofluorocarbons of 1 to 5 carbon atoms, often in the presence of arsenic compounds, such as AsCl. sub. 3, hydrofluoric acid, and antimony chlorofluoride, such as SbCl. sub. 4 F. The spent catalyst may be directly treated with the aqueous calcium chloride solution, very preferably with such solution containing small amounts of a transition metal ion, such as Fe. sup. ++ or Fe. sup. +++, or aluminum ion, e. g. , Al. sup. +++, after which volatile gases emitted are treated, an organic liquid phase is separated from an aqueous liquid phase containing dispersed precipitated insoluble compounds of antimony and arsenic (when arsenic is present), such as calcium salts of acids thereof, oxides, hydroxides and/or oxyhalides thereof resulting from the hydrolysis reaction, such insolubles are separated from the aqueous liquid medium, as by filtration, and the filtrate is neutralized with lime.