US 12,344,532 B2
Methods for preparing two-dimensional sheet-like Li4SiO4 adsorbents using attapulgite and waste lithium batteries
Xiazhang Li, Changzhou (CN); Taoli Huhe, Changzhou (CN); Shixiang Zuo, Changzhou (CN); Xiaofei Yin, Changzhou (CN); Xiaoshan Meng, Changzhou (CN); Chao Yao, Changzhou (CN); and Bingying Gao, Changzhou (CN)
Assigned to CHANGZHOU UNIVERSITY, Changzhou (CN)
Filed by CHANGZHOU UNIVERSITY, Jiangsu (CN)
Filed on Nov. 19, 2024, as Appl. No. 18/952,072.
Application 18/952,072 is a continuation of application No. PCT/CN2024/090547, filed on Apr. 29, 2024.
Claims priority of application No. 202310681390.2 (CN), filed on Jun. 9, 2023.
Prior Publication US 2025/0074777 A1, Mar. 6, 2025
Int. Cl. C01B 33/32 (2006.01); C22B 1/02 (2006.01); H01M 10/54 (2006.01)
CPC C01B 33/32 (2013.01) [C22B 1/02 (2013.01); H01M 10/54 (2013.01); C01P 2002/01 (2013.01); C01P 2002/72 (2013.01); C01P 2002/82 (2013.01); C01P 2004/04 (2013.01)] 9 Claims
OG exemplary drawing
 
1. A method for preparing a two-dimensional sheet-like Li4SiO4 sorbent using attapulgite and a waste lithium battery, comprising:
(1) obtaining LiCoO2 by performing discharging, aluminum foil stripping, and sieving on waste lithium battery cathode material containing LiCoO2, and drying; obtaining biomass by freeze-drying waste biomass, and grinding and sieving the freeze-dried waste biomass;
(2) taking the LiCoO2 and the biomass obtained in step (1), mixing uniformly to obtain a mixture, and putting the mixture into a tube furnace for nitrogen purging, heating and calcination, and carbothermal reduction to obtain a solid sample, hydrothermal stirring the solid sample, followed by filtering, and evaporating to obtain Li2CO3 powder;
(3) ultrasonically dispersing the attapulgite in a first solution that is acidic, and stirring in a water bath at 80° C. to obtain a first product, washing the first product until neutrality, filtering, and drying overnight to obtain SiO2; and
(4) weighing the SiO2 obtained in step (3) and ultrasonically dispersing the weighed SiO2 in deionized water, adding NaOH for hydrothermal stirring, adding the Li2CO3 obtained in step (2) for stirring reaction, followed by adding NH4F to obtain a second solution, and dropwise adding ammonia water to adjust pH of the second solution, transferring the second solution to a microwave hydrothermal reaction kettle for microwave hydrothermal reaction to obtain a second product, and centrifuging, washing, drying, and calcining the second product to obtain the two-dimensional sheet-like Li4SiO4.