US 12,172,891 B2
Method for preparing lithium iron phosphate using by-product ferrous sulfate from titanium dioxide
Yihong Tian, Shenzhen (CN)
Assigned to SHENZHEN WARRANT NEW ENERGY CO., LTD., Shenzhen (CN)
Filed by SHENZHEN WARRANT NEW ENERGY CO., LTD., Shenzhen (CN)
Filed on Mar. 29, 2024, as Appl. No. 18/621,122.
Application 18/621,122 is a continuation of application No. PCT/CN2022/107776, filed on Jul. 26, 2022.
Claims priority of application No. 202210251781.6 (CN), filed on Mar. 15, 2022.
Prior Publication US 2024/0239660 A1, Jul. 18, 2024
Int. Cl. C01B 25/45 (2006.01); H01M 4/36 (2006.01); H01M 4/58 (2010.01); H01M 4/587 (2010.01)
CPC C01B 25/45 (2013.01) [H01M 4/366 (2013.01); H01M 4/5825 (2013.01); H01M 4/587 (2013.01); C01P 2004/80 (2013.01); C01P 2006/40 (2013.01)] 7 Claims
 
1. A method for preparing lithium iron phosphate using by-product ferrous sulfate from titanium dioxide, characterized in comprising the following steps:
(1) adjusting pH of water to a range of 1.5-2.0 by adding sulfuric acid, then dissolving by-product ferrous sulfate from titanium dioxide in the water to prepare a saturated solution; adding iron powder into the saturated solution, and stirring the iron powder in the saturated solution for reacting at a temperature of 80-90° C. for 2-3 hours until the pH of the saturated solution is 2 to obtain a first mixture, precipitating and settling the first mixture to obtain a supernatant, wherein the supernatant is a ferrous sulfate solution;
(2) adding iron phosphate or lithium iron phosphate waste powder to the ferrous sulfate solution, stirring the phosphate or the lithium iron phosphate waste powder in the ferrous sulfate solution at a temperature of 80-90° C. for 30-60 minutes to obtain a second mixture, allowing the second mixture to settle and cool to below 40° C., and filtering the second mixture to obtain a purified ferrous sulfate solution;
(3) dissolving lithium hydroxide in water, adding phosphoric acid and a lithium hydroxide solution in a co-current manner in an autoclave for neutralization; subsequently, adding the purified ferrous sulfate solution to obtain a third mixture, heating the third mixture under stirring, then filtering, washing, and drying the third mixture to obtain lithium iron phosphate powder;
wherein in step (2), an amount of the iron phosphate or lithium iron phosphate waste added is 2-3 wt % of a mass of ferrous sulfate in the ferrous sulfate solution.