The invention relates to a highly reactive, high-purity, free-flowing and dust-free lithium sulfide powder having an average particle size between 250 and 1,500 μm and BET surface areas between 1 and 100 m.sup.2/g. The invention, furthermore, relates to a process for its preparation, wherein in a first step, lithium hydroxide monohydrate is heated in a temperature-controlled unit to a reaction temperature between 150° C. and 450° C. in the absence of air, and an inert gas is passed over or through it, until the residual water of crystallization content of the formed lithium hydroxide is less than 5 wt. % and in a second step, the anhydrous lithium hydroxide formed in the first step is mixed, overflowed or traversed by a gaseous sulfur source from the group consisting of hydrogen sulfide, elemental sulfur, carbon disulfide, mercaptans or sulfur nitrides.

The invention relates to a highly reactive, high-purity, free-flowing and dust-free lithium sulfide powder having an average particle size between 250 and 1,500 μm and BET surface areas between 1 and 100 m.sup.2/g. The invention, furthermore, relates to a process for its preparation, wherein in a first step, lithium hydroxide monohydrate is heated in a temperature-controlled unit to a reaction temperature between 150° C. and 450° C. in the absence of air, and an inert gas is passed over or through it, until the residual water of crystallization content of the formed lithium hydroxide is less than 5 wt. % and in a second step, the anhydrous lithium hydroxide formed in the first step is mixed, overflowed or traversed by a gaseous sulfur source from the group consisting of hydrogen sulfide, elemental sulfur, carbon disulfide, mercaptans or sulfur nitrides.

A method of production of a solid electrolyte, which comprises: a step of obtaining a mixture comprising a sulfide solid electrolyte and a tertiary alcohol including 9 or less carbon atoms, and a step of removing the tertiary alcohol from the mixture.

A method of production of a solid electrolyte, which comprises: a step of obtaining a mixture comprising a sulfide solid electrolyte and a tertiary alcohol including 9 or less carbon atoms, and a step of removing the tertiary alcohol from the mixture.

A process for producing a low-cost water-reactive sulfide material includes reacting a substantially anhydrous first alkali metal salt, a substantially anhydrous first sulfide compound, and a substantially anhydrous first alkali metal hydrosulfide compound in a substantially anhydrous polar solvent, providing differential solubility for a substantially high solubility second sulfide and a substantially low solubility second alkali metal salt, and forming a mixture of the high solubility second sulfide, a second alkali metal hydrosulfide, and the low solubility second alkali metal salt; removing the low solubility second alkali metal salt to isolate the supernatant including the second sulfide, and separating the polar solvent from the second sulfide and the second alkali metal hydrosulfide followed by heating to produce the second sulfide. The present disclosure provides a scalable process for production of a high purity alkali metal sulfide that is essentially free of undesired contaminants.

A method for preparing high-purity lithium sulfide by using industrial-grade butyllithium includes the following steps: step A: under an inert gas condition, thoroughly mixing 1.5-2.5 g of lithium chloride, 0.5 L of an industrial-grade n-butyllithium solution (2.5 mol/L) and 1.5-2.5 L of n-hexane to obtain a mixed solution, and charging the mixed solution into a sealed container; step B: under the sealed condition, firstly introducing H.sub.2S gas into a gas-washing bottle through a submerged pipe at a rate of 10.5 L/h, then introducing into the mixed solution through the submerged pipe, controlling the reaction temperature at 25-40° C., and continuously stirring for reaction for 4-6 h to obtain a reaction slurry; and step C: under an inert gas condition, filtering the reaction slurry with a G3 sand core funnel to obtain a crude lithium sulfide solid wet material.

A method for preparing high-purity lithium sulfide by using industrial-grade butyllithium includes the following steps: step A: under an inert gas condition, thoroughly mixing 1.5-2.5 g of lithium chloride, 0.5 L of an industrial-grade n-butyllithium solution (2.5 mol/L) and 1.5-2.5 L of n-hexane to obtain a mixed solution, and charging the mixed solution into a sealed container; step B: under the sealed condition, firstly introducing H.sub.2S gas into a gas-washing bottle through a submerged pipe at a rate of 10.5 L/h, then introducing into the mixed solution through the submerged pipe, controlling the reaction temperature at 25-40° C., and continuously stirring for reaction for 4-6 h to obtain a reaction slurry; and step C: under an inert gas condition, filtering the reaction slurry with a G3 sand core funnel to obtain a crude lithium sulfide solid wet material.

A process for producing a low-cost water-reactive sulfide material includes reacting a substantially anhydrous first alkali metal salt, a substantially anhydrous first sulfide compound, and a substantially anhydrous first alkali metal hydrosulfide compound in a substantially anhydrous polar solvent, providing differential solubility for a substantially high solubility second sulfide and a substantially low solubility second alkali metal salt, and forming a mixture of the high solubility second sulfide, a second alkali metal hydrosulfide, and the low solubility second alkali metal salt; removing the low solubility second alkali metal salt to isolate the supernatant including the second sulfide, and separating the polar solvent from the second sulfide and the second alkali metal hydrosulfide followed by heating to produce the second sulfide. The present disclosure provides a scalable process for production of a high purity alkali metal sulfide that is essentially free of undesired contaminants.

A process for producing a low-cost water-reactive sulfide material includes reacting a substantially anhydrous first alkali metal salt, a substantially anhydrous first sulfide compound, and a substantially anhydrous first alkali metal hydrosulfide compound in a substantially anhydrous polar solvent, providing differential solubility for a substantially high solubility second sulfide and a substantially low solubility second alkali metal salt, and forming a mixture of the high solubility second sulfide, a second alkali metal hydrosulfide, and the low solubility second alkali metal salt; removing the low solubility second alkali metal salt to isolate the supernatant including the second sulfide, and separating the polar solvent from the second sulfide and the second alkali metal hydrosulfide followed by heating to produce the second sulfide. The present disclosure provides a scalable process for production of a high purity alkali metal sulfide that is essentially free of undesired contaminants.

A process for producing a low-cost water-reactive sulfide material includes reacting a substantially anhydrous first alkali metal salt, a substantially anhydrous first sulfide compound, and a substantially anhydrous first alkali metal hydrosulfide compound in a substantially anhydrous polar solvent, providing differential solubility for a substantially high solubility second sulfide and a substantially low solubility second alkali metal salt, and forming a mixture of the high solubility second sulfide, a second alkali metal hydrosulfide, and the low solubility second alkali metal salt; removing the low solubility second alkali metal salt to isolate the supernatant including the second sulfide, and separating the polar solvent from the second sulfide and the second alkali metal hydrosulfide followed by heating to produce the second sulfide. The present disclosure provides a scalable process for production of a high purity alkali metal sulfide that is essentially free of undesired contaminants.