A contribution to understanding the flotation behavior of lithium metal oxides and spheroidized graphite for lithium-ion battery recycling

Vanderbruggen, Anna; Sygusch, Johanna; Rudolph, Martin; Serna-Guerrero, Rodrigo

doi:10.1016/j.colsurfa.2021.127111

Cited by 61 publications

(62 citation statements)

References 47 publications

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“…For instance, when the model or spent black mass is added to water, non-wetted clusters were observed on top of the pulp, as shown in Supplementary Material (Figure S2), some of which were not broken even under a rotor agitation at 1000 min −1 . As shown in the study of Vanderbruggen et al [35], LMO particles were entrapped in such nonwetted clusters. By applying an attrition pre-treatment, such unselective agglomerates were broken [57] and the full wetting of LMOs in the pulp was promoted.…”

Section: Black Mass and Particle Entrainmentmentioning

confidence: 76%

“…This test resulted in a low mass pull of 12% and only 31% graphite recovery in the overflow product, leading to low separation efficiency. However, in a previous study from our group [35], pristine spheroidized graphite was floated with a 90% recovery under similar conditions in the absence of kerosene. These results point out that the hydrophobicity of spent graphite is lower than fresh spheroidized graphite, possibly due to residual binder or a solid electrolyte interphase (SEI) layer partially removed during pyrolysis [13].…”

Section: Flotation Trends Of Spent Black Massmentioning

confidence: 80%

“…While kerosene increase graphite recovery, it also promoted the flotation of metallic particles, highlighting a selective character of the oily collector. In a previous study [35], it was observed tha osene interacted with graphite particles as well as with lithium metal oxide particl creasing their agglomeration and their attachment to an air bubble. The improvement in the C grade between (I) and (II) is correlated with the dec in the metals reporting to the overflow product (Figure 4).…”

Section: Flotation Trends Of Spent Black Massmentioning

confidence: 92%

“…According to the literature on black mass flotation studies, a minimum of 10% and up to 50% of LMOs reported to the overflow, depending on the recycling process applied and the amount of binder removed [15,23,24,54]. In most of these studies, it was assumed that the LMO recovery in the overflow product was due to true flotation via the residual binder, although our group has recently demonstrated that other mechanisms may be responsible for their flotation [35]. The significant difference in LMO recovery between the spent and model black mass (i.e., 29.2 ± 3% and 7.5 ± 0.9%, respectively) hereby measured (Figure 7) highlights the contribution of the residual binder in the LMO recovery.…”

Section: Effect Of Residual Binder On Lmo Recoverymentioning

confidence: 99%

“…It is also worth noting that entrainment may not be the only mechanism of LMO recovery in black mass flotation. Vanderbruggen et al [35] recently reported that LMOs without a coated binder could attach to an air bubble and also interact with kerosene.…”

Section: Introductionmentioning

confidence: 99%

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Improving Separation Efficiency in End-of-Life Lithium-Ion Batteries Flotation Using Attrition Pre-Treatment

et al. 2022

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The comminution of spent lithium-ion batteries (LIBs) produces a powder containing the active cell components, commonly referred to as “black mass.” Recently, froth flotation has been proposed to treat the fine fraction of black mass (<100 µm) as a method to separate anodic graphite particles from cathodic lithium metal oxides (LMOs). So far, pyrolysis has been considered as an effective treatment to remove organic binders in the black mass in preparation for flotation separation. In this work, the flotation performance of a pyrolyzed black mass obtained from an industrial recycling plant was improved by adding a pre-treatment step consisting of mechanical attrition with and without kerosene addition. The LMO recovery in the underflow product increased from 70% to 85% and the graphite recovery remained similar, around 86% recovery in the overflow product. To understand the flotation behavior, the spent black mass from pyrolyzed LIBs was compared to a model black mass, comprising fully liberated LMOs and graphite particles. In addition, ultrafine hydrophilic particles were added to the flotation feed as an entrainment tracer, showing that the LMO recovery in overflow products is a combination of entrainment and true flotation mechanisms. This study highlights that adding kerosene during attrition enhances the emulsification of kerosene, simultaneously increasing its (partial) spread on the LMOs, graphite, and residual binder, with a subsequent reduction in selectivity.

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Section: Black Mass and Particle Entrainmentmentioning

confidence: 76%

Section: Flotation Trends Of Spent Black Massmentioning

confidence: 80%

Section: Flotation Trends Of Spent Black Massmentioning

confidence: 92%

Section: Effect Of Residual Binder On Lmo Recoverymentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Improving Separation Efficiency in End-of-Life Lithium-Ion Batteries Flotation Using Attrition Pre-Treatment

et al. 2022

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Development of Fine Particle Mechanical Separation Processes with Representative Catalyst Materials for Recycling PEM Water Electrolyzers Exploiting their Wetting Characteristics

Ahn,

Rudolph

2023

ChemCatChem

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Demand for technologies using water electrolysis to produce green hydrogen is increasing, although recycling research on membrane electrode assemblies, which contain various precious and highly critical metals, is still limited. This study therefore aims at exploiting the feasibility of fine particle separation processes based on the difference in hydrophobicity of the ultrafine materials used as catalysts in polymer electrolyte membrane electrolyzers and at providing a fundamental study with representative materials of carbon black and TiO2. Since the cathode materials including carbon black are hydrophobic and the anode materials as well as TiO2 are hydrophilic, the characterizations of their various surface properties such as zeta potentials, dispersion characteristics, and bubble coverage angle tests have been investigated. In addition, using liquid‐liquid particle extraction in a mixture model, 99 % of carbon black is recovered in the organic phase and 97 % of TiO2 is selectively separated in the aqueous phase with the help of the dispersant, sodium hexametaphosphate.

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Recycled graphite for more sustainable lithium‐ion batteries

Olutogun,

Vanderbruggen,

Frey

et al. 2024

Carbon Energy

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The demand for lithium‐ion batteries (LIBs) is driven largely by their use in electric vehicles, which is projected to increase dramatically in the future. This great success, however, urgently calls for the efficient recycling of LIBs at the end of their life. Herein, we describe a froth flotation‐based process to recycle graphite—the predominant active material for the negative electrode—from spent LIBs and investigate its reuse in newly assembled LIBs. It has been found that the structure and morphology of the recycled graphite are essentially unchanged compared to pristine commercial anode‐grade graphite, and despite some minor impurities from the recycling process, the recycled graphite provides a remarkable reversible specific capacity of more than 350 mAh g−1. Even more importantly, newly assembled graphite‖NMC532 cells show excellent cycling stability with a capacity retention of 80% after 1000 cycles, that is, comparable to the performance of reference full cells comprising pristine commercial graphite.

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A contribution to understanding the flotation behavior of lithium metal oxides and spheroidized graphite for lithium-ion battery recycling

Cited by 61 publications

References 47 publications

Improving Separation Efficiency in End-of-Life Lithium-Ion Batteries Flotation Using Attrition Pre-Treatment

Improving Separation Efficiency in End-of-Life Lithium-Ion Batteries Flotation Using Attrition Pre-Treatment

Development of Fine Particle Mechanical Separation Processes with Representative Catalyst Materials for Recycling PEM Water Electrolyzers Exploiting their Wetting Characteristics

Recycled graphite for more sustainable lithium‐ion batteries

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