The Impacts of Various Acid and Reductant

Types on Lithium and Cobalt Leaching from

Spent Lithium Ion Batteries
Tugce Kukrer1, Emine Sayilgan2, Nevzat O. Yigit2, Ata U. Akcil3, Mehmet Kitis2
1
Il Bank Inc., Izmir, Turkey
2
Department of Environmental Engineering, Suleyman Demirel University, Isparta, Turkey
3
Department of Mining Engineering, Suleyman Demirel University, Isparta, Turkey

CONTACT DETAILS
Tugce Kukrer
Address: Il Bank Inc., 35170 Izmir, Turkey
Tel: +90-232-255-4115
E-mail: tugce.nakiboglu@gmail.com

EXECUTIVE SUMMARY

The economic values of especially lithium and cobalt in lithium ion batteries (LIBs), stringent
regulations and environmental issues all result in a driving force for the collection and recycling of
spent LIB components. In this work, various acids (H2SO4, HCl and HNO3) and carbohydrate-type
reducing agents (glucose, sucrose, fructose, lactose) were tested to leach lithium and cobalt from
spent LIBs. Also, hydrogen peroxide was also tested as a reducing agent. As pre-treatment steps
prior to leaching, both sieving and further treatment with NaOH were very effective in removing
aluminum from the cathode powders prior to acid leaching. For all the tested reductants, Li and Co
leach yields were always lower than 50% when the acid concentrations were 1 M and the
temperature was 30 or 75 oC. Increasing acid concentrations from 1 to 4 M significantly increased
both Li and Co leach yields above 80%. Both the type of reducing agent and temperature
simultaneously played role in the leaching of Li and Co from spent LIBs. For the Li leaching,
highest leach yields (about 47%) were found with sulfuric acid alone and with sucrose as the
reductant. Similarly, highest Co leach yields (about 50%) were obtained when sucrose was used as
a reducing agent. Different particle size fractions provided different leaching effectiveness. As the
Li and Co amounts in particle size fractions decreased the percent leaching yields also decreased.
For full-scale applications, it is suggested to use 500-700 µm powder size fractions in leach
reactors. When all the tested reductants and acids were compared at constant conditions, the
combined use of hydrogen peroxide and hydrochloric acid performed better in Li and Co leaching
from spent LIBs.

Keywords: cobalt; environmental; hydrometallurgy; leaching; lithium; recycling.

INTRODUCTION

Lithium ion batteries (LIBs) have become the major power source for most of the small portable
electrical equipment due to their various advantages including high volumetric and gravimetric
energy density, low self discharge rate, no memory effect, quick charge acceptance, excellent cycle
life, wide temperature range of operation, and light weight (Nishi 2001; Ra & Han 2006; Ritchie &
Howard 2006).

LIBs consist of a plastic casing and several cell units. Each cell unit has a cathode, an anode, an
organic separator, an organic electrolyte, and a steel casing. In the cathode, LiCoO2 active
materials, carbon-conducting additives and a binder are pasted on aluminum foil. The anode is
fabricated by the same process with graphite active materials, carbon-conducting additives and a
binder pasted on copper foil (Lee & Rhee 2002). The potentially hazardous components of batteries
include mercury, lead, copper, zinc, cadmium, manganese, nickel, and lithium (Bernardes et al.
2004). Recycling of the major components of spent LIBs appears to be a beneficial way to prevent
environmental pollution, raw material consumption, while meeting the new legal requirements and
providing alternative resources of cobalt and lithium (Castillo et al. 2002; Nan et al. 2005;
Mantuano et al. 2006; Nan et al. 2006; Xu et al. 2008). Therefore, the economic values of especially
lithium and cobalt in LIB wastes, stringent regulations and environmental issues all result in a
driving force for the collection and recycling of spent LIB components.

Several studies have been carried out to recover valuable metals from the waste cathodic active
material (LiCoO2) by pyrometallurgical and hydrometallurgical processes. The methods reported
commonly include crushing, physical separation, acid leaching, and precipitation or solvent
extraction to recover the cobalt and lithium from the LIB wastes (Swain et al. 2007). Detailed
reviews of technologies for the recovery of Li and Co from spent LIBs were reported by Kukrer et
al. 2007 and Xu et al. 2008.

In this work, various acids (H2SO4, HCl and HNO3) and carbohydrate-type reducing agents
(glucose, sucrose, fructose, lactose) were tested to leach lithium and cobalt from spent LIBs.
Different carbohydrate-type reducing agents were tested and used for acidic leaching of various
ores (Trifoni et al. 2000; Veglio et al. 2001). Furthermore, hydrogen peroxide was also tested as a
reducing agent. In aqueous solutions depending on thermodynamics, hydrogen peroxide can oxidize
or reduce a variety of inorganic ions. The evolved oxygen from the decomposition of hydrogen
peroxide converts Co(III) to Co(II) to help the dissolution. The main objective was to determine the
impacts of the tested reducing agents on the effectiveness of acidic leaching. Furthermore, the
impacts of leach temperature and powder particle size on the leaching kinetics were also studied.
The following chemical reactions were considered for the dissolution of lithium and cobalt from
spent LIB powders.

8LiCoO2 + 12H2SO4 + C12H22O11 → 8CoSO4 + 4Li2SO4 + 12CO2 + 3H2O + 20H2 (1)

4LiCoO2 + 6H2SO4 + C6H12O6 → 4CoSO4 + 2Li2SO4 + 6CO2 + 2H2O + 10H2 (2)
2LiCoO2 + 3H2SO4 + H2O2 → 2CoSO4 + Li2SO4 + 4H2O + O2 (3)
8LiCoO2 + 24HCl + C12H22O11 → 8CoCl2 + 8LiCl + 12CO2 + 3H2O + 20H2 (4)
4LiCoO2 + 12HCl + C6H12O6 → 4CoCl2 + 4LiCl + 6CO2 + 2H2O +10H2 (5)
2LiCoO2 + 6HCl + H2O2 → 2CoCl2 + 2LiCl + 4H2O + O2 (6)
8LiCoO2 + 24HNO3 + C12H22O11→ 8Co(NO3)2 + 8LiNO3 + 12CO2 + 3H2O + 20H2 (7)
4LiCoO2 + 12HNO3 + C6H12O6 → 4Co(NO3)2 + 4LiNO3 + 6CO2 + 2H2O + 10H2 (8)
2LiCoO2 + 6HNO3 + H2O2 → 2Co(NO3)2 + 2LiNO3 + 4H2O + O2 (9)
MATERIALS AND METHODS

Powder Preparation and Characterization

Spent LIBs were collected from the Campus of Suleyman Demirel University and a volunteer
foundation in Turkey. Spent LIBs were first separated and then manually dismantled. Dismantling
products such as plastic films and ferrous scraps were discarded. After dismantling, all battery
components were separated and weighed. The cathode and anode folios were crushed using a
blender for 15 minutes for particle size reduction. The battery powders were characterized by X-ray
fluorescence (XRF) (Spectro Xepos) and elemental analysis (Leco, CHNS-932, Mikro). Table 1
shows the elemental composition of each powder sample. In order to remove aluminum from the
powders, the powder samples were mixed with 10% (by weight) NaOH solution with a 1/10
solid/liquid ratio and then left to settle in room temperature for 5 hours (Nan et al. 2006). After
settling, the solution containing the dissolved aluminum was filtered. The solid powder residues on
the filter paper were dried for 24 h at 105 ºC until constant weight was achieved. The dried solid
residues were then weighed to determine the mass losses during aluminum removal.

Leach Experiments
Kinetic leaching tests were conducted using mixed (50% cathode, 50% anode) LIB powders. This is
because it is challenging to separately process cathode and anode powders in full-scale applications.
The tested acids were HCl, HNO3 and H2SO4, each at 1 M concentration. As reducing agents,
glucose, sucrose, fructose, lactose (20 g/L) and hydrogen peroxide (10% wt.) were used. For all the
leaching experiments, powder dosage was 50 g/L. Additional kinetic leach tests were also
conducted at higher acid concentrations (4 M). The tested leach temperatures were 30 and 75 ºC.
All acidic leaching tests were performed in 250-mL high-density polyethylene flasks (solution
volume 100 mL) which were mixed at 200 rpm by a stirrer in a temperature-controlled water bath
(ST402, Nuve). The flasks were loosely covered with caps to allow carbon dioxide release which is
formed during the chemical reactions. During the leach tests, 1 mL of leach liquor sample was
withdrawn from the flasks after 0.1, 0.25, 0.5, 1, 2, 4, and 6 h to analyze for Li and Co. These liquor
samples were centrifuged at 10,000 rpm for 5 min (MiniSpin Plus, Eppendorf) to remove solid
residues prior to Li and Co analysis. Each sample was diluted by 1:10 using nitric acid solution
(pH~2) to avoid the precipitation of metals, and then the samples were kept at 4 ºC in the fridge
until analysis. Additional experiments were conducted to determine the impacts of powder particle
size on the leaching kinetics of Li and Co. Such experiments were carried out at 75 ºC with 2 M
H2SO4 and 10% (wt.) H2O2.

Analytical Methods
Li and Co concentrations were determined by inductively coupled plasma (ICP-OES) (DV2100,
Perkin Elmer). pH was measured during all leaching experiments using a pH-meter (6250, Jenco).
A 98% sulfuric acid, 37% hydrochloric acid and 65% nitric acid solutions were used as the stock
solutions for all experiments. Hydrogen peroxide stock solution used was 30%. All chemicals used
were reagent grade and were obtained from Merck or Rie del-de Haen. Sodium hydroxide solution
(10% wt.) was used to remove aluminum from powders. Distilled and deionized water (DDW) was
used for stock solution preparations and dilutions.
RESULTS AND DISCUSSION

Characterization of Spent LIBs and Powders

Table 1 shows the elemental composition of each powder sample.

Table 1. The characterization of spent lithium ion battery powders (% mass).

Total Value
Sample Li Co Al Cu Mn Cd Ni Zn Fe Pb P C H
(%)
OC 4.9 47.5 9.5 0.2 1.20 <0.0006 0.03 0.02 0.03 0.02 0.32 6.6±0.7 0.4±0.1 70.7
OA 0.7 0.9 0.1 30.9 0.01 <0.0005 0.002 0.02 0.01 <0.0005 1.88 68.4±6.5 0.9±0.1 103.8
SC 5.5 50.2 0.8 0.1 0.21 <0.0006 0.05 0.02 0.007 0.003 0.25 6.5±1.0 0.4±0.1 64.2
SA 1.1 1.7 0.1 5.8 0.02 <0.0005 0.01 0.03 0.02 <0.0005 1.18 76.1±8.7 0.7±0.1 86.8
MCA 3.3 24.4 0.4 2.4 3.96 <0.0006 0.02 0.02 0.003 <0.0006 0.96 47.8±2.4 0.5±0.1 83.8
TC 4.7 45.0 3.6 0.08 0.81 <0.0006 0.05 0.01 0.008 0.02 0.07 7.1±0.2 0.6±0.1 62.0
STC 5.4 53.6 0.1 0.06 1.72 <0.0006 0.10 0.01 <0.0006 0.02 0.02 6.1±0.4 0.1±0.1 67.3
OC: original cathode powder.
OA: original anode powder.
SC: Sieved cathode. <425 µm cathode powder.
SA: Sieved anode. <425 µm anode powder.
MCA: Mixed cathode and anode. <425 µm mixed (50% cathode, 50% anode) powder.
TC: Treated (through NaOH treatment) cathode, no sieving.
STC: Sieved and treated cathode. Sieved through 425 µm and then treated with NaOH for further Al removal.

Due to the presence of LiCoO2 in the cathode of LIBs, higher mass percentages of Li and Co were
found in samples SC (<425 µm cathode powder), STC (<425 µm de-aluminized cathode powder),
OC (original cathode powder), and TC (de-aluminized cathode powder, no sieving). Sieving the
cathode powder through a 425-µm sieve was very effective in removing Al; most of the Al folio
remained on the sieve. While the relative Al mass was 9.5% in the original cathode powder, it
decreased to 0.8% after sieving through 425-µm. In addition to the sieving, NaOH treatment was
also effective in removing Al from the powders. While the relative Al mass was 9.5% in the
original cathode powder, it was 3.6% after removal through NaOH treatment. These results
indicated that both sieving and further treatment with NaOH are very effective in removing Al from
the cathode powders of spent LIBs.

Due to the presence of copper folio and graphite in the anode of LIBs, higher mass percentages of
Cu and C were found in samples OA (original anode powder) and SA (<425 µm anode powder).
Relative Cu amount of about 31% was decreased to about 6% through sieving. On the other hand,
sieving was not effective in reducing carbon amounts; almost all of the carbon passed through the
425-µm sieve.

Sieve analysis was performed for the whole batch of cathode and anode powders of the spent LIBs
from various manufacturers (Fig. 1). Therefore, the results shown are not for a single brand but for a
combination of different LIB brands.
 35
Anode
Cathode
30

25
% (mass)

20

15

10

0 00 00
0
71
0
50
0
42
5
35
5
30
0
25
0
18
0 25 –7
5
<4
5
>1 0- 1 0- 5- 5– 0– 0- 0– 5– –1 45
71 50 42 35 30 25 18 12 75
Particle size (µm)

Figure 1. Sieve analysis for cathode and anode LIB powders.

As indicated in Fig. 1, the particle size fractions both in the cathode and anode powders exhibited a
wide range from <45 µm to >1000 µm. It is also obvious that such fractionation is also dependent
on the degree of crushing and blending. For the cathode powder, the majority of particles based on
mass were in the 180-425 µm size range. On the other hand, for the anode powder, the majority of
particles had a size of >425 µm. These results overall indicated that at the same degree of crushing
and blending the relative mass of large particles in the anode powder is more than those in the
cathode powder. In other words, crushing and blending was more effective in reducing particle sizes
in the cathode powder. This result may be considered important in full-scale applications since
leaching efficiency may be higher for smaller particles in powders.
Leach Tests
Figure 2 shows the impacts of the types of reducing agents on Li and Co leaching from spent LIBs
at 30 oC leach temperature.

100

90 A
80

70
Li leaching efficiency (%)

60 H2SO4
H2SO4+Glucose
50 H2SO4+Sucrose
H2SO4+Fructose
40 H2SO4+Lactose
H2SO4+H2O2
30

20

10

0
0 25 50 75 100 125 150 175 200 225 250 275 300 325 350 375 400
Reaction time (min)

100 B
90

80
Co leaching efficiency (%)

70 H2SO4
H2SO4+Glucose
60
H2SO4+Sucrose

50 H2SO4+Fructose
H2SO4+Lactose
40
H2SO4+H2O2

30

20

10

0
0 25 50 75 100 125 150 175 200 225 250 275 300 325 350 375 400
Reaction time (min)

Figure 2. The impacts of the types of reducing agents on Li (A) and Co (B) leaching from spent LIBs at 30 oC
leach temperature (1M H2SO4, 50 g/L battery powder). Error bars indicate 95% confidence intervals.

Sulfuric acid alone (1 M concentration) without any reductant was not effective in Li and Co
leaching. The most effective Li and Co leaching efficiencies (leach yields) at 30 oC leach
temperature were obtained when hydrogen peroxide was used as the reducing agent in sulfuric acid
leaching. In these conditions, Li and Co leach yields were about 45 and 38%, respectively. Due to
the strong chemical bonds between cobalt and oxygen, acid leaching of lithium cobalt oxide is
difficult. When hydrogen peroxide is added as a reducing agent, the evolved oxygen from the
decomposition of hydrogen peroxide converts Co(III) to Co(II) to help the dissolution. Other
reducing agents exhibited much lower leach yields, around 27-34% for Li and 14-17% for Co. The
tested carbohydrates (glucose, sucrose, fructose, lactose) were not effective as reductants in
leaching of Li and Co at lower leach temperature (30 oC).
Also, leaching tests were conducted at 75 oC leach temperature (data not shown). For the Li
leaching, highest leach yields (about 47%) were found with sulfuric acid alone and with sucrose as
the reductant. Similarly, highest Co leach yields (about 50%) were obtained when sucrose was used
as a reducing agent. Apparently, at higher leach temperatures, sucrose performed well compared to
hydrogen peroxide which provided highest leach yields at lower temperatures. Overall, the results
indicated that at both leach temperatures of 30 and 75 oC Li and Co leach yields were always low
(i.e., ≤50%) with all the tested reducing agents in sulfuric acid solution of 1 M. At both of the tested
temperatures, Li leaching yields increased with reaction time of up to about 2 h after which the
leaching process achieved equilibrium. Contradicting results were found for the Co leaching
kinetics. While equilibrium was obtained at about 2 h for Co leaching at 30 oC, leaching continued
up to about 4 h at 75 oC.

Leach experiments were also conducted in the absence of reducing agents using H2SO4, HCl or
HNO3 at 75 oC leach temperature (Fig. 3).

100

90
A
80

70
Li leaching efficiency (%)

60 HNO3

50
HCl

40
H2SO4
30

20

10

0
0 25 50 75 100 125 150 175 200 225 250 275 300 325 350 375 400
Reaction time (min)

100

90 B
80

70
Co leaching efficiency (%)

60 HNO3

50 HCl

40
H2SO4

30

20

10

0
0 25 50 75 100 125 150 175 200 225 250 275 300 325 350 375 400
Reaction time (min)

Figure 3. The impacts of acid types in the absence of reducing agents on Li (A) and Co (B) leaching from spent
LIBs at 75 oC leach temperature (4M acid, 50 g/L battery powder). Error bars indicate 95% confidence
intervals.

It was found that increasing acid concentrations from 1 to 4 M significantly increased both Li and
Co leach yields for all the tested three acids. For example, Li leach yields higher than 80% were
obtained after about 2 h of reaction time (Fig. 3A). Similarly, Co leach yields higher than 70% were
obtained after the same reaction time for all the three acids (Fig. 3B). Increasing acid concentrations
also increased the leach kinetics. When considered for the overall leaching process, HCl appears to
be the most effective one. Based on the obtained data, the following leach conditions can be
suggested to achieve higher than 80% Li and Co leach yields from spent LIB powders even without
using any type of reductant: 4 M HCl, 75 oC leach temperature, 50 g/L battery powder, 2 h leach
period.

In order to determine the impacts of powder particle size on leaching yields, leaching tests were
conducted with various particle size fractions. The results are presented in Fig. 4.

110

100 A
90

80 500-710 micron
Li leaching efficiency (%)

425-500 micron
70
355-425 micron

60 300-355 micron
250-300 micron
50 180-250 micron
125-180 micron
40 75-125 micron
45-75 micron
30
< 45 micron

20

10

0
0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160
Reaction time (min)

100

90
B
80

70 500-710 micron
Co leaching efficiency (%)

425-500 micron
60 355-425 micron
300-355 micron
50 250-300 micron
180-250 micron
40 125-180 micron
75-125 micron
30 45-75 micron
< 45 micron
20

10

0
0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160
Reaction time (min)

Figure 4. The impacts of powder particle size on Li (A) and Co (B) leaching from spent LIBs (2 M H2SO4, 10%
(wt.) H2O2, T: 75 oC).

Different particle size fractions provided different leaching effectiveness at the constant leaching
conditions. The lowest leaching yields both for Li and Co were found in the 250-300 µm fraction
(Fig. 4). This may be explained by the fact that this fraction had the least amount of Li and Co
contents among all particle size fractions. It appears that as the Li and Co amounts in particle size
fractions decrease the percent leaching yields also decrease. For the other size fractions except 250-
300 µm, Li leach yields more than 90% were consistently achieved. The impacts of particle size
fractions on the leach yields were more pronounced for Co. For example, at a leach period of 150
min, Co yields ranged between about 50 to 95%. Such range was much narrower for the Li yields.
Highest Co leach yields (>90%) were obtained by the 500-710 µm fraction which also contained the
highest Co content. Based on these lab-scale tests, it may be suggested to use about 500-700 µm
powder size fractions for effective Li and Co leaching from spent LIBs. However, other factors
related to the powder particle size should also be considered and optimized in full-scale designs
including the mechanical means for powder size reduction, reactor mixing, energy demands, and
powder dosages.

CONCLUSIONS

As pre-treatment steps prior to leaching, both sieving and further treatment with NaOH were very
effective in removing Al from the cathode powders of spent LIBs. Although sieving was also very
effective in reducing the Cu amounts in anode powders it could not retain carbon; almost all of the
carbon passed through the 425-µm sieve. The particle size fractions both in the cathode and anode
powders exhibited a wide range from <45 µm to >1000 µm. Crushing and blending was more
effective in reducing particle sizes in the cathode powder compared to anode powder. The most
effective Li and Co leach yields at 30 oC leach temperature were obtained when hydrogen peroxide
was used as the reducing agent in all the tested three acid solutions at 1 M concentrations. The
tested carbohydrates (glucose, sucrose, fructose, lactose) were not effective as reductants in
leaching of Li and Co at lower leach temperature (30 oC). Li and Co leach yields were always lower
than 50% when the acid concentrations were 1 M and the temperature was 30 or 75 oC. Such
finding was valid for all the reductants tested. Increasing acid concentrations from 1 to 4 M
significantly increased both Li and Co leach yields for all the tested three acids. Higher than 80% Li
and Co leach yields from spent LIB powders even without using any type of reductant can be
obtained at the following leach conditions: 4 M HCl, 75 oC leach temperature, 50 g/L battery
powder, 2 h leach period. It was found that both the type of reducing agent and temperature
simultaneously play role in the leaching of Li and Co from spent LIBs. At both of the tested
temperatures, Li leaching yields increased with reaction time of up to about 2 h after which the
leaching process achieved equilibrium. Increasing leach temperature from 30 to 75 oC also
increased the leaching kinetics of both Li and Co. Different particle size fractions provided different
leaching effectiveness at the constant leaching conditions. It was found that as the Li and Co
amounts in particle size fractions decrease the percent leaching yields also decrease. For full-scale
applications, it may be suggested to use about 500-700 µm powder size fractions for effective Li
and Co leaching from spent LIBs. When all the tested reductants and acids were compared at
constant conditions, the combined use of hydrogen peroxide and hydrochloric acid performed better
in Li and Co leaching from spent LIBs.

ACKNOWLEDGEMENTS

This work was supported by the Research Projects Funding Unit of the Suleyman Demirel
University, Isparta, Turkey (project no. BAP 1490-D-07). The authors would like to thank Prof.Dr.
Francesco Vegliò and his research group at University of L’Aquila, Italy for providing valuable
technical assistance and XRF analysis.
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