Method for preparing reduced metal catalyst having metal surface area

Claim 1

A process of stabilizing, with respect to atmospheric air, a bed containing pyrophoric reduced metal catalyst with high active metal surface area formed by reduction of a compound of said metal at an elevated temperature ranging from 200° C. to 500° C. which comprises; (a) continuously circulating through said bed a stream of an inert gas while maintaining a catalyst temperature of at least 300° F. (149° C.); (b) cooling the catalyst throughout the bed with said inert gas until the catalyst in said bed attains a temperature ranging from about 50° to about 100° F.; (c) decreasing the inert gas flow and progressively adding CO 2 until the CO 2 concentration in the gas stream is at least about 80%; (d) adding O 2 to the gas stream to obtain about 0.05 vol. % O 2 in the gas stream and continuing this flow until a sufficient amount of O 2 has passed through the catalyst bed to attain about 25% of a monolayer coverage of oxygen on the active metal surface; (e) increasing the O 2 concentration in the gas stream at a rate that will have passed enough O 2 through the catalyst bed to form about a monolayer on the active metal surface by the time the concentration reaches about 1 vol. % O 2 ; and (f) increasing the O 2 concentration and decreasing the CO 2 concentration until said catalyst in the bed is stabilized with respect to atmospheric air, said stabilization treatments being characterized as providing a stabilized catalyst without loss of the initial metal surface area.