Preparation of lithium amide

In a method of preparing finely divided solid lithium amide, the steps which comprise:

• (a) incorporating into a reaction vessel lithium metal in bulk or relatively large aggregate form, toluene, and finely divided active metallic cobalt as a catalyst,
• (b) admixing therewith anhydrous liquid ammonia under conditions of agitation and maintaining said mixture within a low temperature range under agitation conditions until at least most of the lithium metal dissolves to form a bronze lithium-ammonia solution,
• (c) gradually adding a substantial additional amount of toluene to said solution under conditions of agitation whereby a heterogeneous system is created in which a lithium-ammonia solution in liquid ammonia floats on the surface of the toluene,
• (d) and effecting formation of solid lithium amide by gradually raising the temperature of the contents of the reaction flask, under conditions of agitation, while liberating hydrogen and excess ammonia, the solid lithium amide, as it forms, falling into the lower toluene layer to produce a slurry of said solid lithium amide in said toluene.

In a method of preparing finely divided solid lithium amide, the steps which comprise:

• (a) admixing pulverulent metallic cobalt in a dispersion in toluene prepared by heating a mineral oil dispersion of lithium metal and cobalt chloride hexahydrate to melt said lithium metal and to effect reduction of said cobalt chloride to a finely divided active metallic cobalt, removing said mineral oil and washing said remaining dispersion with toluene and slurrying said dispersion with toluene,
• (b) adding said dispersion formed in step (a) and lithium metal in bulk form or in the form of relatively large aggregates,
• (c) cooling to a temperature in the range of about 0.degree. to about -60.degree. C. or lower,
• (d) gradually adding anhydrous liquid ammonia under conditions of agitation and while maintaining said mixture within said temperature range under agitation conditions until at least most of the lithium metal dissolves to form a bronze solution;
• (e) gradually adding a substantial additional amount of toluene under conditions of agitation whereby a heterogeneous system is created in which the lithium-ammonia solution in liquid ammonia floats on the surface of the toluene,
• (f) effecting formation of solid lithium amide by gradually raising the temperature of the mixture, under conditions of agitation, while liberating hydrogen and excess ammonia, the solid lithium amide, as it forms, falling into the lower toluene layer to form a slurry of said solid lithium amide in said toluene,
• (g) removing ammonia, and
• (h) recovering the solid lithium amide in finely divided form from the toluene.