IP Library Granted Patent US 11,932,549
Granted Patent B2
US 11,932,549 · App. 17/265,371 · Granted Mar 19, 2024

Manufacturing apparatus for lithium sulfate and manufacturing method therefor

Inventors: Juyoung Kim (Pohang-si, KR); Ki Young Kim (Pohang-si, KR); Woonkyoung Park (Pohang-si, KR); Jung Kwan Park (Pohang-si, KR); Woo Chul Jung (Pohang-si, KR); Kwang Seok Park (Pohang-si, KR); Hyun Woo Lee (Pohang-si, KR); Sang Won Kim (Pohang-si, KR); Heok Yang (Pohang-si, KR); Seung Taek Kuk (Pohang-si, KR)
Assignees: POSCO CO., LTD; RESEARCH INSTITUTE OF INDUSTRIAL SCIENCE & TECHNOLOGY
C01D15/06B01J8/006B01J19/0066B01J2208/00867B01J2208/00902C01P2006/80
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Quick Facts
Patent No.
US 11,932,549
App. No.
17/265,371
Granted
Mar 19, 2024
Kind
B2
Abstract

It is introduced that a device of manufacturing lithium sulfate comprising: a reaction body in which a reaction of lithium phosphate and sulfuric acid is performed, the reaction body being divided into an upper space and a lower space; a pressurizer for applying pressure to the inside of the reaction body; a stirrer disposed in the upper space for stirring the lithium phosphate and sulfuric acid to produce a mixture containing lithium sulfate and phosphoric acid; and a filter disposed inside the reaction body and separating the filtrate containing the phosphoric acid into the lower space by filtering the mixture.

Claims (70)

1. A device of manufacturing lithium sulfate comprising:

a reaction body in which a reaction of lithium phosphate and sulfuric acid is performed, the reaction body being divided into an upper space and a lower space;

a pressurizer for applying pressure to the inside of the reaction body;

a stirrer disposed in the upper space for stirring the lithium phosphate and sulfuric acid to produce a mixture containing lithium sulfate and phosphoric acid; and

a filter disposed inside the reaction body and separating the filtrate containing the phosphoric acid into the lower space by filtering the mixture.

2. The device of claim 1 ,

the device further comprises a recovery unit connected to the lower space and collecting the filtrate.

3. The device of claim 1 ,

the device further comprises:

a cleaning liquid supply unit connected to the upper space and supplying a cleaning liquid into the reaction body; and

a circulation unit for circulating the cleaning liquid passed through the filter from the lower space to the upper space.

4. The device of claim 3 ,

the device further comprises:

a dissolution liquid supply unit connected to the upper space and supplying a dissolution liquid into the reaction body; and

a obtaining unit for obtaining lithium sulfate dissolved in the dissolution liquid through a resultant pipe connected to the lower space.

5. The device of claim 4 ,

wherein, the cleaning liquid supply unit comprises:

a first reservoir in which the cleaning liquid is stored;

a first supply pipe communicating the first reservoir and the upper space; and

a spray nozzle formed at the end of the first supply pipe.

6. The device of claim 5 ,

wherein, the cleaning liquid supply unit further comprises:

a connection pipe connecting the resultant pipe and the first supply pipe; and

a connection pump installed on the connection pipe.

7. The device of claim 4 ,

wherein the dissolution liquid supply unit comprises:

a second reservoir for storing the dissolution liquid; and

a second supply pipe communicating the second reservoir and the upper space.

8. The device of claim 3 ,

The circulation unit comprises:

a circulation pipe communicating the lower space and the upper space; and

a circulation pump installed on the circulation pipe.

9. The device of claim 8 ,

The circulation unit further comprises:

a density measuring device installed in the circulation pipe and measuring a density of the cleaning liquid passing through the filter.

10. A method of manufacturing lithium sulfate comprising:

introducing solid phase lithium phosphate and sulfuric acid into a reaction vessel;

producing a mixture comprising solid lithium sulfate and phosphoric acid by stirring the solid lithium phosphate and sulfuric acid;

recovering a filtrate comprising the phosphoric acid by pressurizing and filtering the mixture; and

cleaning and filtering the mixture by spraying the cleaning liquid with the mixture being pressurized.

11. The method of claim 10 ,

wherein, in the step of spraying the cleaning liquid,

the mixture is cleaned and filtered at the same time.

12. The method of claim 10 ,

wherein, in the step of filtering the mixture,

when a liquid content which is the ratio of the liquid in the mixture is 45 to 53% by weight, the spray of the cleaning liquid is started.

13. The method of claim 12 ,

wherein, in the step of spraying the cleaning liquid,

the cleaning liquid is sprayed so that the liquid content of the mixture is maintained at 45 to 53% by weight.

14. The method of claim 10 ,

in the step of filtering the mixture, the mixture is pressurized to 2 to 4 bar, and

in the step of spraying the cleaning liquid, the mixture is pressurized to 2 to 4 bar.

15. The method of claim 10 , further comprises:

determining that the mixture has been washed by measuring the density of the filtrate filtered from the mixture, if the density of the filtrate becomes 1.51 g/cc or less, after the step of spraying the cleaning liquid.

16. The method of claim 15 , further comprises:

terminating the spraying of the cleaning liquid when the density of the filtrate becomes 1.25 g/cc or less, after the step of measuring the density of the filtrate.

17. The method of claim 10 , further comprises:

supplying a dissolution liquid to the remained solid lithium sulfate filtered the filtrate from the mixture; and

obtaining lithium sulfate dissolved in the dissolution liquid, after the step of spraying the cleaning liquid.

18. The method of claim 10 ,

in the step of filtering the mixture,

the total concentration of phosphorus (P) and sulfur (S) in the filtrate is 5 mol/L or more.

19. The method of claim 10 ,

in the step of producing the mixture,

the mixture is produced through direct reaction of the solid lithium phosphate and sulfuric acid,

the mixture comprises a phosphoric acid solution in which sulfuric acid ions are present, and

the solid lithium sulfate is precipitated in the phosphoric acid solution.

20. The method of claim 10 ,

in the step of spraying the cleaning liquid,

wherein the total weight of the cleaning liquid to be sprayed is 0.9 to 1.2 times the weight of the solid phase particles contained in the mixture before spraying the cleaning liquid.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 4, 2023
From: POSCO HOLDINGS INC.; RESEARCH INSTITUTE OF INDUSTRIAL SCIENCE & TECHNOLOGY
To: POSCO CO., LTD; RESEARCH INSTITUTE OF INDUSTRIAL SCIENCE & TECHNOLOGY
Reel/Frame 063212/0009 →
CHANGE OF NAME Recorded Sep 28, 2022
From: POSCO
To: POSCO HOLDINGS INC.
Reel/Frame 061561/0756 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 1, 2021
From: KIM, JUYOUNG; KIM, KI YOUNG; PARK, WOONKYOUNG; PARK, JUNG KWAN; JUNG, WOO CHUL; PARK, KWANG SEOK; LEE, HYUN WOO; KIM, SANG WON; YANG, HEOK; KUK, SEUNG TAEK
To: POSCO; RESEARCH INSTITUTE OF INDUSTRIAL SCIENCE & TECHNOLOGY
Reel/Frame 056738/0481 →
Priority Claims (2)
KR 10-2018-0116489 · Sep 28, 2018 · national
KR 10-2018-0090311 · Aug 2, 2019 · national
Continuity (1)
Related Publication 20210300774A1 · Sep 30, 2021