Development of sustainable processes for recycling spent lithium-ion batteries

The increasing numbers of electric vehicles and electronic devices around the world are leading to a wider application of rechargeable batteries, and lithium-ion batteries (LIBs) are currently the most dominant kinds. Spent LIBs contain toxic organics, salts, and heavy metals that can cause severe pollution to the environment. On the other hand, the spent LIBs are rich in some critical and high value elements including lithium (Li), cobalt (Co), manganese (Mn) and nickel (Ni) that are worth to be recovered. Therefore, recycling spent LIBs has important significance from both environmental and economic aspects.

Current recycling processes are usually wasteful and can bring about severe environmental hazards. The thermal treatment or pyrometallurgy process for recycling is often energy-intensive and will release toxic off gas. The traditional hydrometallurgy process for metal recovery usually over consumes acids and redox agents, which results in large amount of waste water. Processes that save resources, reduce energy consumption and avoid secondary pollution are needed for environmental friendliness and sustainability. In this thesis, we focus on dealing with these current problems, and investigating efficient and environmentally friendly pathways for recycling of spent LIBs. The thesis aims to develop new processes that avoid the use of expensive and toxic additives, reduce chemical consumption and also reduce the generation of secondary wastes for recycling spent LIBs.

Ni-Co-Mn ternary (LiNi_xCo_yMn_zO₂, short as NCM) batteries and lithium iron phosphate (LiFePO₄, short as LFP) batteries are two major groups of LIBs, but they usually have different recycling processes because of their different chemical compositions. An electrochemical approach by analyzing electric potentials of the metal ions was developed to evaluate their redox abilities. Based on the results, a salt leaching method was proposed using water-soluble NH₄Fe(SO₄)₂ as redox intermediate for synergistic recovery of valuable metals from NCM and LFP cathode. Li, Mn, Co and Ni can be leached out under mild condition while PO₄^3- is completely retained in the solid residue. Thermodynamic analysis on leaching solutions is shown to be feasible for separating products for LFP and NCM battery systems, and the products obtained from the process all have high purities. Moreover, the process makes full use of the intrinsic redox ability of NCM and LFP, which reduces the consumption of redox additives to a large extent.

Deep eutectic solvent (DES) provides a green alternative route for metal extraction from spent battery cathode, and the organic acids with strong reducibility are expected for effective extraction of metals. A simple and universal approach was proposed by applying ionization energy (IE) calculation assisted with cyclic voltammetry test to select organic acid as efficient reductant in the DES for battery recycling. The reducibility of the organic acid was found to have a close relationship with the IE. The organic acids with lower IE are found to be preferred reductants. Based on this approach, the hydrous choline chloride-L-ascorbic acid DES was identified and verified to be efficient for metals leaching from LiNi_1/3Co_1/3Mn_1/3O₂ cathode under mild conditions. The DES designed from IE calculation is versatile for treating various kinds of spent battery cathodes and recyclable for multiple uses, decreasing the generation of secondary chemical waste and pollution.

The DES can be used not only for metal extraction, but also for other steps during recycling. Electrode material separation is an essential element for recycling spent LIBs, and the key is to decompose/remove the organic polymer binder that is usually polyvinylidene fluoride (PVDF). The Density Functional Theory calculation is used to predict suitable DES for degrading the PVDF binder as required for effective separation of the electrode active materials from current collector foils. The potassium carbonate-ethylene glycol DES was identified based on the calculation to be an efficient DES for the electrode material separation under a mild reaction condition. The molecular reaction mechanism study revealed that it was the carbonate ions that react with the PVDF polymer chains and cause the degradation of the polymer, leading to effective separation. The separated electrode materials all had high purities and their crystal structures remained unchanged. The strategy of using green DES provides a highly efficient and environmentally friendly pathway for the pretreatment of spent LIBs.

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