Upcycling of Cathode Materials from Industrial Lithium Iron Phosphate Black Mass: Process Design and Optimization
Loading...
Authors
Traversy, Michael
Date
Type
thesis
Language
eng
Keyword
Lithium , Recycling , Circular Materials Economy , LiFePO4 , LFP , Process Optimization , Chemical Engineering , Mining , Lithium Carbonate , Lithium Phosphate , Upcycling , Clean Energy Minerals , Organic Lixiviant
Alternative Title
Abstract
Lithium is the principal active material for clean energy storage and transformation, and its stable supply is critical to achieving international climate objectives. Projected supply challenges and unprecedented demand for Li have revealed the necessity of developing spent Li-ion battery recycling as a secondary Li resource stream. Following the optimization of Li-selective leaching from industrial grade LiFePO4 black mass by formic acid and H2O2, this work explores the treatment of the derived liquor, with the objective of advancing the process to technology readiness level 5. Purification of the liquor was affected by multi-step precipitation of Al, Co, Ni, Mn, Fe, and Cu hydroxides. Processes for Li recovery by the addition of Na3PO4, H3PO4, and Na2CO3 were optimized. Interactions of reaction temperature, pH, and precipitant dosage were evaluated, and compared to synthetic solutions. The kinetics of Li2CO3 precipitation from the proprietary liquor were investigated. The conversion of Li3PO4 to LiOH by Ca(OH)2 causticization was explored. In 2-L validation experiments, the maximum recovery of Li3PO4 and Li2CO3 from the 6.5 g Li/L leachate were 98.92% and 74.73%, respectively. Li2CO3 recovery by antisolvent addition was investigated, increasing Li2CO3 recovery to 94.42% with the addition of 1:1 v/v isopropanol. The lithium content of Li2CO3 and Li3PO4 met 97.20% and 98.00%. Li2CO3 purity exceeded 99.50% after CO2 digestion and thermal decomposition recrystallization. Impurity concentrations met battery grade specifications in both products. This work provides a basis for the development of a continuous reactor, capable of upcycling Li-bearing black mass into different cathode precursors.
Description
Citation
Publisher
License
Queen's University's Thesis/Dissertation Non-Exclusive License for Deposit to QSpace and Library and Archives Canada
ProQuest PhD and Master's Theses International Dissemination Agreement
Intellectual Property Guidelines at Queen's University
Copying and Preserving Your Thesis
This publication is made available by the authority of the copyright owner solely for the purpose of private study and research and may not be copied or reproduced except as permitted by the copyright laws without written authority from the copyright owner.
ProQuest PhD and Master's Theses International Dissemination Agreement
Intellectual Property Guidelines at Queen's University
Copying and Preserving Your Thesis
This publication is made available by the authority of the copyright owner solely for the purpose of private study and research and may not be copied or reproduced except as permitted by the copyright laws without written authority from the copyright owner.