Sodium Hydroxide → Ammonia

Participants

Reaction Steps

With the object of obtaining active material particles comprising a plurality of metal oxide layers by using 3 or more reaction-deposition vessels connected in series and changing the composition and/or kind of metal salts in respective reaction-deposition stages, and as a specific example, a process for producing a composite oxide of a plurality of metal elements of 3-layer structure wherein the inner layer comprises nickel hydroxide containing manganese as solid solution, the layer of the outside thereof comprises nickel hydroxide containing aluminum as solid solution and the outermost layer (surface layer) comprises nickel hydroxide containing calcium as solid solution is described below. The production apparatus used was of the same structure as that shown in FIG. 4 comprising three reaction-deposition vessels 28, 29 and 30 connected in series, each having a volume of 5 l. First, a 2.2 mol/l aqueous nickel nitrate solution, 0.2 mol/l aqueous manganese nitrate solution and 4.8 mol/l aqueous ammonia solution were prepared. These solutions were simultaneously fed each at a rate of 0.5 ml/min into the reaction vessel 28 and, while the inner temperature of the vessel being kept constant at 50° C. and with stirring to effect rapid and uniform mixing, a 4.8 mol/l aqueous sodium hydroxide solution was added at an average rate of 0.5 ml/min so as to keep the pH value in the reaction vessel within the range of 12.0±0.2. After the conditions in the reaction vessel had become stable, the suspension in the vessel containing particles of nickel hydroxide containing manganese as solid solution grown to an average particle diameter of 12 μm was fed at an average rate of 2.0 ml/min into the reaction vessel 29. Simultaneously with the suspension, a 2.2 mol/l aqueous nickel nitrate solution and 0.2 mol/l aqueous aluminum nitrate solution were fed each at an average rate of 0.5 ml/min into the reaction vessel 29 and, while the inner temperature of the vessel being kept constant at 50° C. and with stirring, a 4.8 mol/l aqueous sodium hydroxide solution was added at an average rate of 0.5 ml/min so as to keep the pH value in the reaction vessel within the range of 12.5±0.2. After the conditions in the reaction vessel had become stable, the suspension in the vessel containing particles having an inner layer comprising nickel hydroxide containing manganese as solid solution and a surface layer comprising nickel hydroxide containing aluminum as solid solution, grown to an average particle diameter of 12.5 μm, was fed at an average rate of 3.5 ml/min into the reaction vessel 30. Simultaneously with the suspension, a 2.2 mol/l aqueous nickel nitrate solution and 0.2 mol/l aqueous calcium nitrate solution were fed each at an average rate of 0.5 ml/min into the reaction vessel 30 and, while the inner temperature of the vessel being kept constant at 50° C. and with stirring, a 4.8 mol/l aqueous sodium hydroxide solution was added at an average rate of 0.5 ml/min so as to keep the pH value in the reaction vessel within the range of 12.0±0.2. After the conditions in the reaction vessel had become stable, the suspension in the reaction vessel was made to overflow from the upper part of the vessel to collect samples continually. The suspension thus obtained was centrifuged, the supernatant was replaced with deionized water, the resulting sediment was subjected to in-liquid classification to remove minute crystals of oxides comprising mainly Ni and containing Ca throughout the inside formed in the reaction vessel 30, and then washed with water and dried to obtain a powder with an average particle diameter of 12.7 μm.

Provenance & Evidence