Recycling of lithium-ion batteries

student Josephine Röhner

e-mail josephine.roehner@uni-jena.de

report date June 11, 2020

module BC 6.3.4 ”Umweltchemie II”

Chemisch-Geowissenschaftliche Fakultät
Josephine Röhner June 11, 2020

Contents
1 Introduction 1

2 Process steps for recycling of LIB 2

2.1 Disassembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
2.2 Stabilization and Passivation . . . . . . . . . . . . . . . . . . . . . . . . . 2
2.3 Physical materials separation . . . . . . . . . . . . . . . . . . . . . . . . 3
2.4 Pyrometallurgical recycling . . . . . . . . . . . . . . . . . . . . . . . . . . 3
2.5 Hydrometallurgical recycling . . . . . . . . . . . . . . . . . . . . . . . . . 3
2.5.1 Sulfate system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
2.5.2 Chloride system . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
2.5.3 Nitrate system . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
2.5.4 Other leaching systems . . . . . . . . . . . . . . . . . . . . . . . . 5
2.6 Bioleaching . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2.7 Direct recycling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

3 Commercial processes 6
3.1 Retriev . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
3.2 Umicore . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
3.3 Recupyl . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
3.4 Accurec . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

4 Outlook 11

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1 Introduction
Lithium-ion batteries (LIB) are rechargeable energy storage devices that show high
energy capacity and a longer life-span as well as a higher voltage output compared to
other highly used battery types (such as nickel metal-hydride or lead-acid batteries) [1].
Since LIB have been commercialized in 1991, they have greatly influenced the innovation
of new electrical applications [2] . Currently, the biggest field of application for LIB are
mobile phones and notebooks. For these kind of applications, LIB are preferred as they
are very lightweight. Another domain where the use of LIB has greatly risen over the
past few years, are electric vehicles (EV). While e-bikes and e-scooters are already seen
frequently on the streets these days, the demand for electric and hybrid cars has rapidly
increased due to the urgent will to reduce greenhouse gas emissions [3]. Now, questions
regarding the disposal and the long-term availability of LIB must be discussed [4].

LIB contain a variety of metals such as lithium, nickel or cobalt which are high-value
materials whose reserves on earth are finite. Especially the supply of cobalt is a great
concern because until 2025, battery production alone could potentially use up 10% of
the world reserves [5]. Also, the extraction of cobalt in third-world countries like the
Democratic Republic of Congo (the world’s leading producer of colbalt) is linked to huge
social and humanitarian problems. Dangerous working conditions, a high rate of child
labour and negative impacts for indigenous communities are only a few of the issues that
need to be addressed when thinking of the increased mining due to high demand of LIB
[6].
Meanwhile, the mining of lithium has a huge environmental impact as well. To produce
1 t of lithium, it takes 250 t of ore or 750 t of mineral-rich brine which has to be pumped
up from the salt flat through drilling holes. This process uses up a lot of water - 1900 t
of water are needed to extract 1 t of lithium [4].
Essentially, the big increase of the environmental footprint associated with the extraction
of metals stands in direct conflict with the environmental improvements by the usage of
LIB powered vehicles [1].

Recycling could solve a big portion of environmental and social problems which are caused
by the extraction of metals necessary for LIB production. For example - in comparison
to the usual production of lithium - 28 t of LIB from mobile devices or 256 batteries of
electric vehicles would be needed to produce 1 t of lithium through recycling [7]. The
first pilot plant for commercialized recycling of LIB was put into operation in Hofors
(Sweden) with a recycling rate of 2000 t of batteries per year. 2011, a semi-industrial
plant was openened in Hoboken (Belgium) based on the experiences from Hofors with an
annual capacity of 7000 t. Since then, different methods for the recycling of LIB have
been developed and implemented industrially [8].

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2 Process steps for recycling of LIB

In general, it has to be noticed, that the recycling of LIB is more difficult, than for
example the recycling of NiMH or Pb-acid batteries. This is due to the high variety
of different materials in LIB. Not only are a lot of different materials such as polymer
separators, different metals and graphite, contained in a cell but also, LIB are not as
highly standardized yet as other kinds of batteries. Therefore, the most common cathode
material may be LiCoO2 (LCO) but it is also possible to replace some of the cobalt with
combinations of Mn, Al or Ni. Another promising cathode material is LiFePO4 (LFP).
As anode material, graphite is mostly used but the use of silicon is also being investigated
[5].
In general, LIB contain around 5–20% cobalt, 5–10% nickel, 5–7% lithium, 15% organic
chemicals and 7% plastics, depending on the manufacturer [9].

2.1 Disassembly
The first step in every recycling process is the disassembly of battery packs, at least to
module level. However, there are hazards associated with battery pack disassembly that
require proper handling of the batteries. Electrocution as well as short-circuiting should
be avoided because the latter can lead to explosion of the battery packs [4].
As different manufacturers follow different design approaches for their LIB packs, it is
difficult to automate the disassembly process. Still, some options have been established,
such as the Optisort system which uses computer algorithms to recognize labels and is
then able to sort batteries according to their content [10].
However, it is still a challenge to automate the disassembly of LIB and therefor make
this process more efficient. Thus, the state-of-the art disassembly is still either done by
hand or half-automated.

2.2 Stabilization and Passivation

The following process steps are stabilization, opening and separation of the LIB compo-
nents. In industry, it is preferred to shred or crush the batteries in an inert gas (nitrogen
or carbon dioxide) to carry out opening and stabilization collectively. Opening the cells
in an atmosphere of carbon dioxide leads to the formation of a passivation layer LiCO3
around the exposed lithium.
It is also possible to discharge low-voltage cells by immersion in salt solution or brine.
However, it has to be considered that competing electrochemical reactions will take place
in this case which go together with gas evolution.
Another alternative is direct Ohmic discharge. The electricity from this method can
either be recovered or dissipated, but both options are not very cost-efficient.
State-of-the art recycling processes feed LIB directly into a shredder or a high-temperature
reactor and therefor avoid the stabilization step [4].

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2.3 Physical materials separation

After shredding processes, recovered materials can be separated by their physical proper-
ties for reclamation purposes. For example, density, particle size, ferromagnetism and
hydrophobicity can be used. First, a fine and a coarse fraction can be separated. The
fine fraction contains electrode coatings (metal oxides and graphite) whereas the coarse
fraction contains plastics, casings and metal foils. The latter can be further separated by
a magnet.
Metal oxides and carbon can undergo froth flotation to separate the graphite from the
more hydrophilic metal oxides. Moreover, the polymeric binder can be removed from the
fine fraction to detach the cathode material from the current collectors [4].

2.4 Pyrometallurgical recycling

In the pyrometallurgical recycling or smelting step, battery parts at module level are
fed into a high-temperature shaft-furnace. A slag-forming agent, containing limestone,
sand and slag is added. Energy for the process is provided by the burning of organic
components such as the electrolyte [11].
The pyrometallurgical process yields three major product mixtures: The smelting alloy,
the slag and fly ash [3]. The alloy contains copper, cobalt, nickel and iron. By hydromet-
allurgical processes, these metals can be recovered. Meanwhile, aluminium and lithium,
as well as silicon, calcium and manganese are left in the slag. It is not efficient to recover
lithium or aluminium from the slag and therefore can not be used for battery production
again [11]. However, the slag can still be used for other purposes, e.g. in the cement
industry [4]. The fly ash still contains small amounts of valuable metals and is either
returned to the furnace or treated in a hydrometallurgical process [3].

Summing up, pyrometallurgical recycling has the advantages of a flexible input, the
avoiding of size reduction, the recovery of cobalt, nickel and copper as well as the indus-
trial feasability of the process. Disadvantages are that aluminium and lithium are lost in
the slag, the organics are burned and additional process steps are needed to extract the
metals from the alloy. Also, the process requires high temperatures, an expensive gas
treatment and a high process volume and is not suited for LFP electrodes [5].

2.5 Hydrometallurgical recycling

In hydrometallurgical recycling processes, valuable metals are recovered using acid or
alkaline solutions. This method is presenting with low cost, little energy consumption
as well as a small environmental footprint [12]. Prominent leaching agents are H2 SO4 ,
HNO3 , HCl and organic acids.

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2.5.1 Sulfate system

The sulfate system is by far the most studied hydrometallurgical process. In this case,
cathode material is leached by 4 M sulfuric acid at 80◦ C. It can also involve a reducing
agent (mostly H2 O2 , glucose or sulfites) for accelerating the leaching kinetics. Then,
2 M H2 SO4 is used in combination with, for example, 15 vol% H2 O2 at 75◦ C [7]. The
following reaction takes place with metals M = Co, Ni, Mn [12]:

2 LiM O2 + 3 H2 SO4 + H2 O2 → 2 M SO4 + Li2 SO4 + 4 H2 O + O2 (1)

Alternatively, H2 SO4 can also be used for the leaching of LFP electrodes:

2 LiF eP O4 + H2 SO4 + H2 O2 → 2 F eP O4 + Li2 SO4 + 2 H2 O (2)

After dissolution of the cathode materials, the valuable products are extracted and
purified in different process steps. Metals can either be precipitated, extracted by solvent
extraction or deposited by electrowinning. For example, cobalt can be precipitated as
oxalate while lithium is usually recovered as carbonate [13].

2.5.2 Chloride system

Another efficient system for hydrometallurgical treatment is the chloride system. Either
a 4 M solution of HCl or a 3 M solution of HCl combined with H2 O2 can be used for the
leaching process [7]:

4 LiM (III)O2 + 12 HCl → 4 LiCl + 4 M (II)Cl2 + 6 H2 O + O2 (3)

After that, valuable elements can be precipitated as hydroxides or carbonates. The

chloride system can also be used for LFP electrodes. In this case, the LFP electrode is
completely dissolved. Titanium is then recovered as TiO2 and iron as FePO4 which can
be used as a precursor in LFP electrode production [12].

2.5.3 Nitrate system

Nitric acid can also be used as a leaching agent although compared to the former two
processes, the leaching with HNO3 shows slower kinetics and is inefficient for LFP
electrodes without the addition of H2 O2 .The leaching reaction is not completely clear as
HNO3 has an oxidizing character. Still, a proposed reaction is shown in the following
[12]:
3 1
LiM (III)O2 + 3 HN O3 → LiN O3 + M (II)(N O3 )2 + H2 O + O2 (4)
2 4
The valuable elements are then regained by precipitation.

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2.5.4 Other leaching systems

Other solutions are recently investigated to make leaching more environmentally friendly
and efficient. Organic acids often are very selective but in exchange can be more ex-
pensive than mineral acids. Citric acid is the most prominent organic acid investigated
for leaching. A further example for leaching with organic acids is a system proposed by
Nayaka et. al. [14]. It uses mild organic acids like nitrilotriacetic acid and adipic acid as
leaching agents and ascorbic acid as reducing agent.
Another interesting approach is the use of deep eutectic solvents as leaching agent that
allows a low solute to solvent ratio for complete Co dissolution compared to other leaching
agents and therefor could be a very economic option [15].

Concluding, hydrometallurgical processes allow lithium to be recovered in a process

with mild conditions (low temperature and low energy). The output from the process can
be used for either cathode precursors or mixed cathodes. However, the process requires
size reduction, the cathode structure is broken down by the acid and solvent extraction
or various precipitation steps are necessary to separate cobalt from nickel and other
valuable metals [5].

2.6 Bioleaching
Another approach to the recovery of metals from LIB is the use of bacteria such as
Acidithiobacillus ferrooxidans for leaching. These bacteria feed on sulfur and Fe(II) ions
and convert these into sulfuric acid and Fe(III) ions. These metabolites are delivered
into the leaching medium and help dissolve the metals from the spent cathode material
[16]. This process is similar to the standard hydrometallurgical process and has to be
further investigated for effectiveness although is has already been successful used in the
mining industry [4].

2.7 Direct recycling

Direct recycling describes the recovery of battery materials with little or no additional
processing. Afterwards, the battery materials will be reinserted in the supply chain.
Therefore, the electrolyte is extracted with supercritical CO2 . After the CO2 is removed
again from the cells, the electrolyte can also be recovered and reused. The cells then
undergo pulverization and afterwards, the different materials are separated by their
physical properties (see 2.3) [11]. The efficiency of the direct recycling process is
dependent on the status of battery health and very sensitive to contaminants [4].
On one hand, direct recovery retains the cathode structure and not only cathode material
but also anode, electrolyte and foils can be recovered. LFP electrodes can be recovered
as well. It can be used at low temperature, low energy and with a small input volume.
On the other hand, this process is not yet demonstrated at scale and requires the input
of single cathodes. Also, the process can not be repeated too often due to degradation.
Most likely, the materials will also not perform as well as virgin materials and therefor
be rather used in less demanding applications [5].

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3 Commercial processes
In the following, different commercialized processes will be introduced and evaluated. An
overview of processes which are currently in operation around the world can be found
in table 1. Exemplary, Retriev, Umicore, Recupyl and Accurec have been chosen to be
elaborated on in the next sections.

Table 1: Overview of industrial LIB recycling processes in 2020 [12]

Company (country) Process type Recovered elements
Retriev (Canada) Cryo-hydrometallurgy Li
Umicore (Belgium) Pyro-hydrometallurgy Co, Ni, Mn
Sumimoto (Japan) Pyro-hydrometallurgy Cu, Ni
Recupyl (France) Hydrometallurgy Li, Co, Ni, Mn, Cu, Al
Snam (France) Pyrometallurgy Cd, Ni, Co, Fe
Accurec (Germany) Pyrometallurgy Al, Cu, Co, Ni, Fe
Glencore (Canada) Pyro-hydrometallurgy Ni, Co
Batrec (Switzerland) Pyro-hydrometallurgy Zn, Co, Ni, Mn, Hg
AkkuSer Oy (Finland) Mechanical LIB active materials
OnTo Technology (USA) Direct recycling LIB active materials
Dowa (Japan) Pyrometallurgy Co, Ni, Mn
Nickelhütte Aue (Germany) Pyrometallurgy Co, Ni, Mn
Brunp (China) Pyro- and Hydrometallurgy Li, Co, Ni, Mn, Cu, Al

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3.1 Retriev
In the Retriev process - formerly called Toxco process - primary and secondary lithium
batteries can be recycled. To reduce the batterie’s reactiveness, they are cryogenically
cooled with liquid nitrogen before the process. First, the batteries are shredded and
separated into different fractions by screening. A fraction rich in copper and cobalt and
another fraction containing steel, aluminium and plastics can be yielded on a shaking
table. In the next step, an alkaline solution is added and the slurry containing lithium,
metal oxide (MeO) and graphite particles is filtered. The result are a fraction of MeO
and graphite and a liquid fraction containing mostly lithium. The lithium is reacted with
CO2 and Na2 CO3 to obtain Li2 CO3 .
However, the filtered metal oxides and the resulting lithium carbonate are usually not
used again in the battery production but instead in the metal industry and are therefor
considered to be downcycled [1], [17].
A modified version of the Retriev process, which is currently under investigation, allows
to recover electrode materials. After the pyrolysis of the binder, anode materials like
graphite are separated from cathode materials like lithium and other metal compounds
by froth flotation [1], [18].

Figure 1: Process scheme of Retriev LIB battery recycling. [1]

The Retriev process uses a mechanical pretreatment followed by a purely hydrometal-

lurgical treatment. The special thing about this process is the use of cryogenic cooling
which makes the process especially safe but also energy intensive [19]. This process allows
lithium to be recycled - thanks to the modified version also in battery-grade quality. To
regain cobalt and other metals in pure quality, further refining methods would be needed.

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3.2 Umicore
The Umicore process is a combination of a pyrometallurgical, followed by a hydrometal-
lurgical process. Aluminium and lithium are lost in the slag after the pyrometallurgical
step and the alloy is treated in two leaching steps. 5000 MJ of heat are needed for the
smelter and gas clean-up of 1 ton of batteries [20] . The slag containing Al and Li can still
be used in the construction industry but is not available anymore for the production of
batteries. However, the recovered Ni(OH)2 and CoCl2 are reintroduced in the production
of battery precursors [3] .

Figure 2: Process scheme of Umicore LIB battery recycling. [1]

In the Umicore process, no pretreatment is needed. Instead, the process starts directly
with the pyrometallurgical treatment. The capacity of the pilot plant are about 7000 t of
LIB per year which equals 250.000.000 mobile phone batteries or 35.000 EV batteries [21].
A disadvantage of this process is that the lithium can not be used in the battery industry
again and a lot of battery components are lost in the process. The pyrometallurgical
process is also very energy intensive. Still, the more valuable metals like cobalt can be
recovered efficiently.

3.3 Recupyl
The Recupyl process begins with shredding the LIB in an inert atmosphere. The shredding
is executed by a rotary shearing machine and an impact mill which finally reduces the
particle size to less than 3 mm. The CO2 passivates the lithium by forming a Li2 CO3
surface layer. Afterwards, different fractions are separated: A fine fraction containing
metal oxides (MeO) and carbon, a magnetic fraction containing the casings, a dense
non-magnetic fraction containing Al and Cu current collectors and a low-density non-
magnetic fraction containing paper and plastics. Water is added to the fines fraction and
the pH is adjusted to 12. A reaction with the lithium occurs which results in production
of lithium hydroxide and hydrogen gas. The lithium can be recovered by addition of
sodium carbonate. The remaining fraction undergoes another leaching step. First, it is
treated with H2 SO4 at 80◦ C. Remaining carbon and copper are removed from the system
and remaining lithium is precipitated as Li3 PO4 by adding H3 PO4 . In a final step, Co

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can either be recovered as hydroxide in the presence of NaClO or in elemental form by

electrolysis [20], [1].

Figure 3: Process scheme of Recupyl LIB battery recycling. [1]

The Recupyl process allows many different materials to be recycled from LIB. A com-
bination of different mechanical separation steps makes it possible to even yield the
plastics and different metals separately. Lithium and cobalt can be recovered as well.
The process seems complex yet energy efficient. However, only 110 t of LIB are recycled
annually in the Recupyl process [5].

3.4 Accurec
In the Accurec process, mechanical, pyrometallurgical and hydrometallurgical methods
are combined to yield a Co-Ni-Mn-Fe alloy and lithium cathode precursor material.
The sorting and dismantling step in the beginning provides the possibility of directly
separating reusable fractions like electronics. The electrolyte can be recovered as well
during a vacuum thermal treatment at 250◦ C. Afterwards, the battery components are
broken up and ferromagnetic metals and plastics are separated. The remaining electrode
material is agglomerated to pellets for better handling and afterwards molten down.
The slag as well as the fly ash undergo a leaching process which is how lithium cathode
precursors can be recovered as well [22]. As an alternative for the use of recovered lithium
of lower purity, Accurec names the glass and ceramics industry [1].

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Figure 4: Process scheme of Accurec LIB battery recycling. [1]

One advantage of the Accurec process is the recycling of electrolytes. However, they
might not be usable for battery production again. For the recovered metals, different
applications are possible but only cobalt and lithium can be used in the battery industry
again. The economical feasibility of the process is highly dependent on the market value
of cobalt [23]. About 1500-2000 t of LIB are recycled by the Accurec process per year
[19].

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4 Outlook
It seems clear that there is already a lot of effort put into the efficient recycling of
lithium ion batteries. Different processes have been established on an industrial scale and
various methods for environmentally friendly recycling are being investigated. Especially
hydrometallurgical treatment steps have proven to be advantageous as they allow lithium
to be recovered and are low in energy. Mechanical pretreatment steps also make it
possible for various materials like plastics and metal casings to be recycled [19].

In the European Union, it is now mandatory for LIB producers to provide for fu-
ture collection and recycling. The recycling efficiency should not go below 50%. This goal
was given by the EU Battery Directive in 2006 [24]. Still, there are no goals mandated
regarding the recovery of different materials. Therefor, various processes can be used
in the EU, although those which recover cobalt and nickel are preferred because they
have the highest market value. The recycling of LIB that do not contain cobalt (for
example, if they use LFP electrodes) is not economically profitable yet. Encouraging the
recycling of cobalt-reduced LIB would still be desirable, given the environmental factors
and thoughts about the future availability of various metals.

Hence, for the improvement of LIB recycling, not only the process efficiency but also the
collection rate has to be raised. Right now, 95& of LIB end up in landfills instead of
being recycled [25]. This can be a grave danger as the electrolyte can diffuse into the
ground or the untreated batteries could catch fire. That is why the public has to be
informed about the necessity of dispose of LIB correctly and new federal policies may
have to be established around the world. A deposit system could also help to increase
the recycling rate as it is done with plastic bottles in Germany.

Another effort which has to be made to facilitate LIB recycling is to make extensive
battery sorting easier. For example, a labeling system has been developed by the Battery
Association of Japan to provide information about the kind of battery, its composition
and the manufacturer [5]. Standardization of modules would also make the automation
of presorting and dismantling batteries easier but due to the big variety of manufacturers
on the market, this seems not yet realistic. Nevertheless, manufacturers should be
responsible to design batteries in a way that allows simple recycling. How components
can be easily disassembled and which materials are suitable for a closed-loop economy
should be considered already in early stages of battery invention.

In conclusion, the various approaches of commercialized processes show that there

are many options to construct a profitable recycling process for LIB. However, it is
still a challenge to balance economical feasibility and sustainable closed-loop recycling
management.

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