Precursor with transformed crystal form and preparation method thereof

Patent metadata

Field	Value
Publication number	US-2023399238-A1
Application number	US-202318238525-A
Country	US
Kind code	A1
Filing date	Aug 28, 2023
Priority date	Aug 27, 2021
Publication date	Dec 14, 2023
Grant date	—

Abstract

The disclosure discloses a precursor with a transformed crystal form and a preparation method thereof. The preparation method includes: (1) heating a carbonate solution, a cobalt salt to allow a reaction, and spray adding a carbonate solution to allow a reaction to obtain a cobalt carbonate slurry; (2) allowing the slurry to stand, spray adding a cobalt salt and a carbonate solution, and spray adding a cobalt salt using a single spray head at a flow rate of 1 m3/h to 3 m3/h and a carbonate solution using no less than three spray heads each at a flow rate of 0.2 m3/h to 5 m3/h to obtain cobalt carbonate with a transformed crystal form; and (3) further spray adding a cobalt salt and a carbonate solution to the cobalt carbonate with a transformed crystal form, heating to allow a constant-temperature reaction, and washing and calcining a product.

First claim

1 . A preparation method of cobaltosic oxide, comprising the following steps:
(1) heating a 0.8 mol/L to 1.8 mol/L carbonate solution, spray adding a cobalt salt and reacting, and spray adding a 2.5 mol/L to 3.5 mol/L carbonate solution and reacting to obtain a cobalt carbonate slurry with a particle size of 3 μm to 5 μm; (2) allowing the cobalt carbonate slurry to stand, and spray adding a cobalt salt and a 2.5 mol/L to 3.5 mol/L carbonate solution separately to allow a reaction to obtain a cobalt carbonate slurry with a particle size of 9 μm to 13 μm; and spray adding a cobalt salt using a single spray head at a flow rate of 1 m 3 /h to 3 m 3 /h and spray adding a 2.5 mol/L to 3.5 mol/L carbonate solution using no less than three spray heads each at a flow rate of 0.2 m 3 /h to 5 m 3 /h to obtain cobalt carbonate with a transformed crystal form; and (3) further spray adding a cobalt salt and a 2.5 mol/L to 3.5 mol/L carbonate solution to the cobalt carbonate with a transformed crystal form, performing a constant-temperature reaction under heating, and washing and calcining a resulting product to obtain the cobaltosic oxide, wherein in steps (1) and (2), the cobalt salt is spray added at a flow rate of 1 m 3 /h to 3 m 3 /h, and the 2.5 mol/L to 3.5 mol/L carbonate solution is spray added at a flow rate of 0.2 m 3 /h to 5 m 3 /h.

2 . The preparation method according to claim 1 , wherein in step (1), the carbonate solution is at least one selected from the group consisting of an ammonium bicarbonate solution, a sodium carbonate solution, a sodium bicarbonate solution, and a potassium bicarbonate solution.

3 . The preparation method according to claim 1 , wherein in step (1), the cobalt salt is one selected from the group consisting of cobalt sulfate and cobalt chloride.

4 . The preparation method according to claim 1 , wherein in step (1), a pH is controlled at 7.45 to 7.65 during the reaction.

5 . The preparation method according to claim 1 , wherein step (2) further comprises: allowing the cobalt carbonate slurry obtained after the reaction to stand, removing a resulting supernatant, and spray adding the cobalt salt and the 2.5 mol/L to 3.5 mol/L carbonate solution to allow a reaction; and repeating the above process multiple times until the cobalt carbonate slurry with a particle size of 9 μm to 13 μm is obtained.

6 . The preparation method according to claim 1 , wherein step (3) further comprises: allowing a cobalt carbonate slurry obtained after the constant-temperature reaction to stand, removing a resulting supernatant, and spray adding the cobalt salt and the 2.5 mol/L to 3.5 mol/L carbonate solution; repeating the above process multiple times until a solid content in the cobalt carbonate slurry reaches 400 g/L to 580 g/L; and dispensing the cobalt carbonate slurry, and further spray adding the cobalt salt and the 2.5 mol/L to 3.5 mol/L carbonate solution to obtain spherical cobalt carbonate with a particle size of 14.5 μm to 22 μm.

7 . The preparation method according to claim 1 , wherein in step (3), the calcining is conducted at 700° C. to 770° C. for 5 h to 10 h.

8 . Cobaltosic oxide prepared by the preparation method according to claim 1 .

9 . Cobaltosic oxide prepared by the preparation method according to claim 2 .

10 . Cobaltosic oxide prepared by the preparation method according to claim 3 .

11 . Cobaltosic oxide prepared by the preparation method according to claim 4 .

12 . Cobaltosic oxide prepared by the preparation method according to claim 5 .

13 . Cobaltosic oxide prepared by the preparation method according to claim 6 .

14 . Cobaltosic oxide prepared by the preparation method according to claim 7 .

Assignees

• Guangdong Brunp Recycling Technology Co Ltd
• Hunan Brunp Recycling Tech Co Ltd
• Hunan Brunp Ev Recycling Co Ltd

Inventors

• Li Bin
• Li Changdong
• Lu Xinghua
• Liu Weijian
• Cai Yong
• Ruan Dingshan

Classifications

• Y02E60/10

  Energy storage using batteries · CPC title

• H01M4/525

  of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy · CPC title

• C01G51/04 Primary

  Oxides · CPC title

• C01G51/00 Primary

  Compounds of cobalt · CPC title

• C01P2004/32

  Spheres · CPC title