Method for preparing precursor of lithium composite transition metal oxide using a reactor
View Patent ↗Disclosed is a method for preparing a precursor of lithium composite transition metal oxide for lithium secondary batteries, using a reactor having a closed structure including an outer stationary cylinder; an inner rotary cylinder on the same axis; and a rotation reaction area disposed between them, wherein ring-shaped vortex pairs that are uniformly arranged in a rotation axis direction and rotate in opposite directions are formed in the rotation reaction area. According to the method of the invention, raw materials comprising an aqueous solution of two or more transition metal salts, an aqueous solution of a complex forming additive, and a basic aqueous solution for maintaining pH are fed through an inlet into the rotation reaction area where a coprecipitation reaction is performed under a non-nitrogen atmosphere to form lithium composite transition metal oxide particles which are then discharged through a reactor outlet.
1. A method for preparing composite transition metal hydroxide particles using a reactor having a closed structure, the method comprising:
injecting raw materials comprising an aqueous solution of two or more transition metal salts, an aqueous solution of a complex-forming additive, and a basic aqueous solution for maintaining pH of an aqueous solution of the raw materials within a range of 10 to 12, into a rotation reaction area of a reactor through an inlet; and
performing a coprecipitation reaction under a non-nitrogen atmosphere for 1 to 6 hours,
wherein the reactor comprises:
a stationary hollow cylinder;
a rotary cylinder having the same axis as the stationary hollow cylinder and an outer diameter smaller than an inner diameter of the stationary hollow cylinder;
an electric motor to generate power, enabling rotation of the rotary cylinder;
a rotation reaction area disposed between the stationary hollow cylinder and the rotary cylinder, wherein ring-shaped vortex pairs that are uniformly arranged in a rotation axis direction and rotate in opposite directions are formed in the rotation reaction area; and
an inlet through which a reactant fluid is fed into the rotation reaction area and an outlet through which the reactant fluid is discharged from the rotation reaction area, wherein there is a distance between the stationary hollow cylinder and the rotary cylinder, and the ratio of that distance to the outer radius of the rotary cylinder is between 0.05 and 0.4.
2. The method according to claim 1 , wherein a kinematic viscosity of reactant fluid is 0.4 to 400 cP and power consumed per unit weight thereof is 0.05 to 100 W/kg.
3. The method according to claim 1 , wherein a critical Reynolds number of the vortex pairs is 300 or more.
4. The method according to claim 1 , wherein the inlet comprises two or more inlets.
5. The method according to claim 4 , wherein the two or more inlets are arrayed in a line by a predetermined distance in a direction of the outlet.
6. The method according to claim 1 , wherein the aqueous solution of a complex-forming additive is present in an amount of 0.01 to 10% by weight, based on the total amount of the two or more transition metal salts.
7. The method according to claim 6 , wherein the aqueous solution of a complex-forming additive is an aqueous ammonia solution.
8. The method according to claim 1 , wherein the transition metal salt is a transition metal sulfate and/or a transition metal nitrate.
9. The method according to claim 8 , wherein the sulfate comprises one or two or more selected from the group consisting of nickel sulfate, cobalt sulfate and manganese sulfate, and the nitrate comprises one or two or more selected from the group consisting of nickel nitrate, cobalt nitrate and manganese nitrate.
10. The method according to claim 1 , wherein the transition metal composite hydroxide is a compound represented by Formula 1 below:
M(OH 1−x ) 2 (1)
wherein M comprises two or more selected from the group consisting of Ni, Co, Mn, Al, Cu, Fe, Mg, B, Cr and transition metals of the second period of the Periodic Table of the Elements; and 0≦x≦0.8.
11. The method according to claim 10 , wherein M comprises two or more transition metals selected from the group consisting of Ni, Co and Mn.