The present invention relates to a method of preparing a precursor material of a positive electrode active material from a waste lithium secondary battery, to a method of preparing a lithium secondary battery positive electrode active material including a precursor material prepared by the same precursor preparation method, and to a lithium secondary battery positive electrode active material prepared by the same positive electrode active material preparation method.

In a method for recovering an active metal of a lithium secondary battery, a cathode active material mixture is prepared from a cathode of a lithium secondary battery. A first reductive process using a first reductive reaction gas and a second reductive process using a second reductive reaction gas that has a higher reaction source concentration than that of the first reductive reaction gas are performed sequentially and continuously to convert the cathode active material mixture into a preliminary precursor mixture. A lithium precursor is recovered from the preliminary precursor mixture. A lithium recovery ratio may be increased by a stepwise reduction while preventing an increase of heating value.

Integrated recycling method and processes including recycling spent catalyst to produce one or more water-soluble metal salts and one or more water-insoluble tail byproducts, and recycling rechargeable batteries to produce one or more battery-grade metals and one or more pure metallic byproducts, wherein the water insoluble tail byproduct is a feedstock in recycling the rechargeable batteries, the impure metallic byproduct is a feedstock in recycling the spent catalyst, or both.

Integrated recycling method and processes including recycling spent catalyst to produce one or more water-soluble metal salts and one or more water-insoluble tail byproducts, and recycling rechargeable batteries to produce one or more battery-grade metals and one or more pure metallic byproducts, wherein the water insoluble tail byproduct is a feedstock in recycling the rechargeable batteries, the impure metallic byproduct is a feedstock in recycling the spent catalyst, or both.

A green chemistry hydrometallurgical process for recovering one or more metals from a metal-containing material includes leaching the metal-containing material with formic acid, obtaining a leachate comprising the one or more metals as one or more metal formates, and precipitating at least one of the one or more metal formates. The metal-containing material may be a lithium-ion battery cathode material, resulting in Li formate remaining in solution and precipitation of salts including one or more of Ni, Co, and Mn formates. Steps may include filtration of the leachate, sulphurization of retained metal formate salts to produce metal sulphate salts, purification of filtered leachate by adding lithium carbonate and filtering, dewatering of the purified leachate, and thermal decomposition of resulting lithium salts to produce battery grade lithium carbonate. Carbon dioxide, water, and formic acid may be recovered and reused, without liquid or solid waste produced.

Provided is a production method and a production apparatus that increase a throughput of nickel sulfate per equipment. A first dissolution step I of introducing a nickel briquette, sulfuric acid, and water to a leaching tank (1) and dissolving the nickel briquette to obtain a primary nickel sulfate solution, and a second dissolution step II of introducing the primary nickel sulfate solution and additionally introducing a nickel briquette to a leaching adjustment tank (2) and dissolving the additionally introduced nickel briquette with free sulfuric acid in the primary nickel sulfate solution to obtain a nickel sulfate solution are executed in this order. With the leaching adjustment tank (2) having a role as a concentration adjustment tank that increases a nickel concentration and decreases a free sulfuric acid concentration, and the leaching tank (1) supplied with the sulfuric acid and the water in addition to the nickel briquette, a continuous dissolution is achievable without increasing a retention time and without unnecessarily enlarging the equipment.

Provided is a production method and a production apparatus that increase a throughput of nickel sulfate per equipment. A first dissolution step I of introducing a nickel briquette, sulfuric acid, and water to a leaching tank (1) and dissolving the nickel briquette to obtain a primary nickel sulfate solution, and a second dissolution step II of introducing the primary nickel sulfate solution and additionally introducing a nickel briquette to a leaching adjustment tank (2) and dissolving the additionally introduced nickel briquette with free sulfuric acid in the primary nickel sulfate solution to obtain a nickel sulfate solution are executed in this order. With the leaching adjustment tank (2) having a role as a concentration adjustment tank that increases a nickel concentration and decreases a free sulfuric acid concentration, and the leaching tank (1) supplied with the sulfuric acid and the water in addition to the nickel briquette, a continuous dissolution is achievable without increasing a retention time and without unnecessarily enlarging the equipment.

Provided is a method for preparing a positive electrode active material for a lithium secondary battery, the method comprising: mixing and reacting a nickel source, a cobalt source, and an aluminum source, ammonia water, sucrose, and a pH adjusting agent to prepare a mixed solution; drying and oxidizing the mixed solution to prepare a positive electrode active material precursor; and adding a lithium source to the positive electrode active material precursor and firing them to prepare a positive electrode active material for a lithium secondary battery.

Provided is a method for preparing a positive electrode active material for a lithium secondary battery, the method comprising: mixing and reacting a nickel source, a cobalt source, and an aluminum source, ammonia water, sucrose, and a pH adjusting agent to prepare a mixed solution; drying and oxidizing the mixed solution to prepare a positive electrode active material precursor; and adding a lithium source to the positive electrode active material precursor and firing them to prepare a positive electrode active material for a lithium secondary battery.

A novel process for treating pickling acid residue and recovering sulfates and nickel therefrom has been developed. By lowering the pH of a magnesium compound slurry to 4-5.5 with sulfuric acid containing pickling acid residue in the presence of ammonium sulfate, both magnesium sulfate and nickel sulfate are solubilized. Magnesium sulfate and nickel sulfate solution is separated from the solids by filtration and an iron hydroxide and chromium hydroxide residue is obtained as a precipitate. Magnesium sulfate and nickel sulfate are then separated from the solution.