PROCESS FOR PRECIPITATING A CARBONATE OR (OXY)HYDROXIDE

Abstract

Process for precipitating a carbonate or (oxy)hydroxide comprising nickel from an aqueous solution of a nickel salt wherein such process is carried out in a vessel comprising (A) a vessel body, (B) one or more elements that control the hydraulic flow of the slurry formed during the precipitation and that induce a loop-type circulation flow, and (C) a stirrer whose stirrer element is in the vessel but located separately from the element(s) (B).

Claims

1-10. (canceled)

11. A process for precipitating a carbonate or (oxy)hydroxide comprising nickel from an aqueous solution, the process comprising combining an aqueous solution of at least two different metal salts of which one is a nickel salt with an aqueous solution of an alkali metal hydroxide or (hydrogen)carbonate, wherein the process is carried out in a vessel comprising (A) a vessel body, (B) an element that controls a hydraulic flow of a slurry formed during the precipitating and that induces a loop-type circulation flow, and (C) a stirrer whose stirrer element is in the vessel and located below (B).

12. The process of claim 11, wherein (B) is selected from the group consisting of a draft tube and a guide vane.

13. The process of claim 11, wherein the carbonate or (oxy)hydroxide comprises a transition metal selected from the group consisting of manganese and cobalt.

14. The process of claim 11, wherein the stirrer element of (C) is selected from the group consisting of a stirrer disc, a blade, a paddle, and a bended cutout.

15. The process of claim 11, wherein (B) is mounted to an internal surface of the vessel.

16. The process of claim 11, wherein (B) is mounted between a vessel lid and side walls of the vessel.

17. The process of claim 11, wherein the vessel is a stirred tank reactor.

18. The process of claim 11, wherein the vessel does not comprise a separate compartment, an external loop or an additional pump in which precipitation of the carbonate or (oxy)hydroxide is carried out.

19. The process of claim 11, wherein the carbonate or (oxy)hydroxide has an average particle diameter (D50) in a range of from 2 to 7 m.

Description

BRIEF DESCRIPTION OF THE DRAWING

[0092] A: vessel body

[0093] B: a draft tube

[0094] C: stirrer element

[0095] D: baffles

[0096] E: engine for stirrer

[0097] The drawing is a conceptual one. In the drawing, feeds and the like have been omitted for simplification matters.

Working Example 1

[0098] A 50 L stirred vessel was charged with an aqueous solution of (NH.sub.4).sub.2SO.sub.4, 25 g of per kg of solution. The vessel body (A.1) of the vessel was equipped with baffles, a draft tube (B.1) and a Rushton turbine stirrer element (C.1) with a diameter of 0.165 m and placed below the draft tube (diameter 0.23 m).

[0099] The temperature of the vessel volume was set to 45 C. The stirrer element was activated and constantly operated at 500 rounds per minute (rpm, 2.7 Watt/I). An aqueous solution containing NiSO.sub.4, CoSO.sub.4 and MnSO.sub.4 (molar ratio 6:2:2, total metal concentration: 1.65 mol/kg), an aqueous solution containing sodium hydroxide (25 wt % NaOH) and aqueous ammonia solution (25 wt % ammonia) were simultaneously introduced through different feeds into the vessel. The molar ratio ammonia to transition metals was 0.2. The sum of volume flows was set to adjust the mean residence time to 8 hours. The flow rate of the NaOH was adjusted by a pH regulation circuit to keep the pH value at a constant value of 12.05. The apparatus was operated continuously keeping the liquid level in the reaction vessel constant. A mixed hydroxide of Ni, Co and Mn was collected via free overflow from the vessel. The resulting product slurry contained about 120 g/l hydroxide precursor with an average particle diameter (D50) of 6 m. The hydroxide was excellently suited as precursor for a lithium ion battery cathode active material.

Working Example 2

[0100] The protocol of Working Example 1 was repeated with the following modification: the rotation speed of the Rushton turbine stirrer was set to 300 rpm (0.6 Watt/I). The resulting slurry contained about 120 g/l hydroxide precursor with an average particle diameter (D50) of 7 m. The hydroxide precursor was excellently suited as precursor for a lithium ion battery cathode active material.

Working Example 3

[0101] The protocol of Working Example 1 was repeated with the following modification: the molar ratio between ammonia and metal was adjusted to 0.4. The resulting product slurry contained about 120 g/l hydroxide precursor with an average particle diameter (D50) of 13.3 m. The hydroxide precursor was excellently suited as precursor for a lithium ion battery cathode active material.

Working Example 4

[0102] The protocol of Working Example 1 was repeated with the following modifications: the molar ratio between ammonia and transition metal was adjusted to 0.4 and the sum of the volume flows was set to adjust the mean residence time to 4 hours. The resulting product slurry contained about 120 g/l hydroxide precursor with an average particle diameter (D50) of 10.6 m. The hydroxide precursor was excellently suited as precursor for a lithium ion battery cathode active material.

Working Example 5

[0103] The protocol of Working Example 4 was repeated with the following modification: the sum of the volume flows was set to adjust the mean residence time to 12 hours. The resulting product slurry contained about 120 g/l hydroxide precursor with an average particle diameter (D50) of 16.4 m. The hydroxide precursor was excellently suited as precursor for a lithium ion battery cathode active material.

Working Example 6

[0104] The protocol of Working Example 1 was repeated with the following modification: A dissolver blade with diameter of 0.2 m was used as stirrer instead of the Rushton turbine. Its rotation speed was set to 500 rpm (1.7 Watt/I). The sum of volume flows was set to adjust the mean residence time to 4 hours. The resulting slurry contained about 120 g/l hydroxide precursor with an average particle diameter (D50) of 6.6 m. The hydroxide precursor was excellently suited as precursor for a lithium ion battery cathode active material.

Working Example 7

[0105] The protocol of Working Example 6 was repeated with the following modification: The sum of volume flows was set to adjust the mean residence time to 8 hours. The resulting product slurry contained about 120 g/l hydroxide precursor with an average particle diameter (D50) of 8.3 m. The hydroxide precursor was excellently suited as precursor for a lithium ion battery cathode active material.

Working Example 8

[0106] The protocol of Working Example 6 was repeated with the following modification: The sum of volume flows was set to adjust the mean residence time to 12 hours. The resulting product slurry contained about 120 g/l hydroxide precursor with an average particle diameter (D50) of 9.5 m. The hydroxide precursor was excellently suited as precursor for a lithium ion battery cathode active material.