News
Focusing on mechanochemical (MC) processing, the chemical transformation of the black masses (BMs) supplied by partners ACCUREC and TES, is planned to be carried out within Work package 4.
Before MC processing, the black masses were analysed using a combination of different analytical techniques. Both quantitative and qualitative analysis were undertaken to determine the Lithium and transition metals yield of the developing recycling process.
Using different reducing agents such as Al, Ca, and their mixtures, researchers carried out preliminary investigations of the MC processing of BMs. Within this task, different aspects, such as the role of the ball milling conditions, the ball milling time, presence of other nonreactive components, and nature of the reducing material were investigated. The analysis led to the conclusion that the kinetics of the MC-induced reduction reaction is sensitive to multiple processing parameters, as shown in the featured image:
XRD patterns of the as-received BMs and products of their reduction after MC processing with Al and Ca as reducing agents: left-TES material; right-ACC material
The upcoming research will focus on improving the reduction reaction kinetics and eliminating the possible safety hazards of fine powder materials. Once finalised, this work will determine the optimal ball milling conditions to be scaled up.
Recovery of Lithium as battery grade materials
The process described in Task 4.4 leads to the chemical transformation of the black masses (BMs) into ferromagnetic Co-, Ni- and Mn-containing products, which will be separated from other by-products. Lithium will be extracted from the rest of the solid products in the subsequent aqueous leaching process to be further transformed into battery-grade lithium carbonate (Li2CO3) salt.
Within the M1-M6 period, aqueous leaching of the ball-milled samples using Al and Ca as reducing agents (RA) was carried out. At a preliminary stage of investigations, researchers noticed the resulted Li2CO3 materials presented small amount of impurities.
To increase the yield of lithium recycling, in the upcoming period, the research work will target the improvement of the leaching conditions and the purification process.
X-ray diffraction patterns of the as-milled BM obtained from TES, products of their reduction reactions after MC processing with Al (left) and Ca (right) as RA, and obtained Li salts after aqueous leaching
TECNALIA [TEC] has actively undertaken both the coordination tasks and the experimental activities that correspond to the solvometallurgical treatment of the received black masses. Firstly, the coordination of the project started with the preparation of the kick-off meeting, in which the entire Consortium assembled in San Sebastián (Basque Country – Spain) and comprises administration and management to ensure an efficient development of RHINOCEROS project.
Also, the experimental section concerning the critical materials extraction from the received black masses from spent batteries started out after receiving the samples from partners ACCUREC [ACC] and KIT.
After characterisation, TEC performed a first round of tests to these samples using a solvometallurgical route and assessing pre-treatment effect on the process. In parallel, State of Art is analysed for different relevant solvometallurgical systems aiming lithium recovery. New batches of experiments will be performed for process optimization and new tests will also be performed when further black mass samples are received.
