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1 s2.0 S0304386X12000357 Main
1 s2.0 S0304386X12000357 Main
Hydrometallurgy
journal homepage: www.elsevier.com/locate/hydromet
a r t i c l e i n f o a b s t r a c t
Article history: A hydrometallurgical process was developed to recover lithium from a brine collected from Salar de Uyuni,
Received 27 December 2011 Bolivia, which contains saturated levels of Na, Cl and sulphate, low Li (0.7–0.9 g/L Li) and high Mg (15–
Received in revised form 4 February 2012 18 g/L Mg). Unlike other commercial salar brines currently being processed, the high levels of magnesium
Accepted 8 February 2012
and sulphate in Uyuni brine would create difficulties during processing if conventional techniques were
Available online 16 February 2012
used. A two-stage precipitation was therefore first adopted in the process using lime to remove Mg and sul-
Keywords:
phate as Mg(OH)2 and gypsum (CaSO4.2H2O). Boron (at 0.8 g/L in the raw brine), a valuable metal yet dele-
Uyuni salar brine terious impurity in lithium products, could also be mostly recovered from the brine by adsorption at a pH
High purity lithium carbonate lower than pH11.3 in this first stage. The residual Mg and Ca (including that added from lime) which were
Removal of magnesium and sulphate subsequently precipitated as Ca–Mg oxalate could be roasted to make dolime (CaO ∙MgO) for re-use in the
Calcium first stage of precipitation. Evaporation of the treated brine up to 30 folds would produce 20 g/L Li liquors.
Boron The salt produced during evaporation was a mixture of NaCl and KCl, containing acceptable levels of sulphate,
Mg, Ca, etc. The final precipitation of lithium at 80–90 °C produced a high purity (99.55%) and well crystalline
lithium carbonate.
© 2012 Elsevier B.V. All rights reserved.
0304-386X/$ – see front matter © 2012 Elsevier B.V. All rights reserved.
doi:10.1016/j.hydromet.2012.02.008
J.W. An et al. / Hydrometallurgy 117–118 (2012) 64–70 65
Table 1
Compositions of various brines of commercial value around the world (Boryta et al., 2011; Evans, 2008; Roskill, 2009).
Source Na K B Li Mg Ca Cl SO4
Clayton Valley, USA 4.69 0.4 0.005 0.0163 0.019 0.045 7.26 0.34
Salton Sea, USA 5.00–7.00 1.30–2.40 0.039 0.01–0.04 0.07–0.57 2.26–3.9 14.20–20.90 42–50
Salar de Atacama, Chile 9.1 2.36 0.04 0.157 0.965 0.045 18.95 1.59
HombreMuerto, Argentina 9.9–10.30 0.24–0.97 0.068–0.121 0.018–0.14 0.019–0.09 15.80–16.80 0.53–1.14
Salar de Uyuni, Bolivia 7.06 1.17 0.071 0.0321 0.65 0.0306 5
Searles Lake, USA 11.08 2.53 0.0054 0.0016 12.3 4.61
Great Salt Lake, USA 3.70–8.70 0.26–0.72 0.007 0.0018 0.5–0.97 0.026–0.036 7.00–15.60 0.94–2.00
Dead Sea, Israel 3.01 0.56 0.003 0.0012 3.09 1.29 16.1 0.061
Sua Pan, India 6 0.2 0.002 7.09 0.83
Bonneville, USA 8.3 0.5 0.007 0.0057 0.4 0.0057 14
Zabuye, China 7.29 1.66 0.0489 0.0026 0.0106 9.53
Taijinaier, China 5.63 0.44 0.031 2.02 0.02 13.42 3.41
content reaches 6% Li. Products of 99.5% to 99.99% lithium carbonate al. (2008) could precipitate Mg(OH)2 of a larger particle size range
can now be manufactured using brine evaporation, precipitation of (5–60 μm) within 60 min from a sea bittern containing 30 g/L Mg by
K and Mg, solvent extraction or ion exchange to remove other impu- adding seeds (5–40 μm) and adopting slow NaOH addition.
rities (Boryta et al., 2002, 2011). After Ca, Mg, B and sulphate are recovered, the concentrated brine
In salar brines containing Mg, carnallite (KCl.MgCl2.6H2O) or can then be purified to remove other residual impurities. The clean
bishoffite (MgCl2.6H2O) starts precipitating when the brine is con- brine is then subjected to carbonation to precipitate lithium carbon-
centrated to ~ 4.4% Li (Atashi et al., 2010; Boryta et al., 2011; ate using sodium carbonate. The conventional process used by most
Wilkomirsky, 1999). The solar evaporation reaches 5.5–6.5% Li before plant operations can produce lithium carbonate of >99.5% grade.
the concentrated brine is processed to lithium carbonate or chloride. This study therefore focuses on the development of a general process
By then lithium carnallite, LiCl.MgCl2.6H2O, also precipitates thus re- to treat the salar brine from Uyuni, Bolivia and the optimization of the
ducing the lithium recovery from the process. The brine by then will unit operations used to recover a high purity lithium carbonate. The
contain ~ 6% Li, 1–4% Mg, 0.5–1% boron (as borate). The separate re- process considered also has to recover Mg, B and K as by-products.
covery of Mg is therefore necessary for the production of high purity
lithium carbonate or lithium chloride. Boron (B) should also be recov- 2. Experimental
ered as apart from improving the process economics its removal from
the concentrated brine is essential for the production of low B feed- 2.1. Materials
stock required for advanced battery manufacturing or Li metal pro-
duction (Boryta et al., 2011). Approximately 15 m 3 of the salar brine from Salar de Uyuni was
A new process scheme therefore needs to be developed for high sampled for the experimental testwork conducted at our laboratories
Mg salar brines such as that found in Uyuni, Bolivia. A different ap- in Korea. The brine was analysed by ICP-AES and its composition is
proach has to be implemented to remove Mg and B as by-products shown in Table 2. Hot plates or temperature-controlled water baths
before lithium carbonate can be recovered. were used in experiments where heating was required. All chemicals
Mg can be removed from sea water, bittern or process liquors as used in the study were of analytical grade.
Mg(OH)2 using slaked dolomite (CaMgCO3) or lime (Ca(OH)2)
(Carson and Simandl, 1994; Karidakis et al., 2005). In the presence of 2.2. Equipment used
sulphate, however, gypsum (CaSO4.2H2O) is normally formed. The
Mg(OH)2–CaSO4∙2H2O mixture has all properties (BET area, oil ad- In this study the chemical compositions of the brines were deter-
sorption, particle size, whiteness, etc.) required to be used as fire mined by ICP-AES (Optima-5300DV, Perkin-Elmer) or IC (ICS-2000,
retarding fillers (Hull et al., 2011; Karidakis et al., 2005). However, fur- Dionex). The structure of lithium carbonate product was determined
ther refining of this mixture is required before Mg can be recovered as by X-ray diffraction analysis (Cu-tube60kv 50 Ma, Philips). The zeta
a chemical grade product or as feedstock for Mg metal production. The potential of the Mg(OH)2 precipitate was measured using an instru-
use of NaOH to precipitate Mg(OH)2 would no doubt produce a high ment from Otsuka Electronics (ELZ-Z2).
purity Mg product. However the process yields very fine and poorly
crystalline Mg(OH)2, creating difficulty during the solid/liquid separa- 2.3. Experimental techniques
tion stage required for its recovery from the highly viscous brine
(Baird et al., 1988; Henrist et al., 2003). Attempts have been made to The precipitation of Mg and Ca salts was conducted at ambient
promote the “ripening” of nano-sized primary crystals of Mg(OH)2 temperature (20–22 °C) using various reactors incorporating differ-
to improve its settling and filterability by aging the precipitate in ent modes of stirring. Different precipitants were added (to known
24 h in non-stirring conditions (Turek and Gnot, 1995). Alamdari et volumes of brine, either 2 L or 4 L) in solid form to avoid the dilution
Table 2
Compositions (in g/L) of the Uyuni salar brine before and after treatment.
Raw Brine 1 105.4 15.7 3.33 16.7 0.84 0.70 203.7 21.3
Raw Brine 2 95.01 16.9 0.34 17.4 0.76 0.68 187.5 22.6
After lime precipitation 92.77 16.3 13.96 0.30 0.82 0.36 189.5 0.67
After oxalate precipitation 115.2 15.9 b0.05 0.17 0.82 0.20 196.3 0.76
After evaporation to 20 g/L Li 56.44 52.5 b0.05 0.35 19.8 2.91 201.4 20.2
After evaporation to 30 g/L Li 37.61 41.3 b0.05 0.65 30.3 4.22 215.6 13.3
66 J.W. An et al. / Hydrometallurgy 117–118 (2012) 64–70
Ca(OH)2solid
Solar evaporation
99.55%
Li2CO3
Fig. 1. Flowsheet developed for the recovery of lithium as carbonate from Uyuni brine.
of the original brine, which hindered the mass balance calculation including sulphate which causes gypsum formation during proces-
and the brine concentration afterwards. The precipitate suspension sing and (c) concentrating the brine by evaporation to achieve
was based on either (a) magnetic bar stirrer, (b) impeller-type stirrer 20–60 g/L Li for the precipitation of lithium carbonate. Fig. 1 outlines
set at 200 rpm and (c) impeller plus ceramic balls for grinding the the major steps involved in the recovery of lithium and other by-
precipitant added as solid. The use of ceramic balls (5 mm diameter) products. Each unit operation of this flowsheet was tested and the re-
added to the reactor at 5 g/L would help the reaction to reach equilib- sults are presented and discussed as follows.
rium quickly within 1 h. Samples were taken during the precipitation
to confirm the reaction has reached completion. Brine evaporation 3.1. Recovery of magnesium and boron
tests were also conducted by continuous boiling and the concentrated
liquors were separated from the precipitates by vacuum filtration or Different alternatives were evaluated to recover Mg, B and to re-
centrifuging. duce the levels of Ca and sulphate from the raw brine. Stabcal soft-
ware (Huang, 2008) was first used to predict the conditions for
3. Results and discussion selectively precipitating Mg and Ca using different precipitants. A typ-
ical example of the results obtained from Stabcal modelling is shown
This study investigates conditions for, (a) recovery of Mg, B and Ca in Fig. 2 for the addition of lime to the raw brine at the Lime/Mg molar
as by-products, (b) purification to remove deleterious impurities ratio of 1:1 and 0.1:1. Using lime, Mg could be removed as Mg(OH)2
Concentration (g/L)
Ca Mg Na (1:1)
B Li Na (0.1:1)
pH
Fig. 2. Stabcal modelling showing the stability of different Ca, Mg, Li and B species at different pHs and lime additions of 1:1 lime/Mg molar ratio. For Na, the precipitation of Na2-
SO4∙10H2O was predicted at 0.1:1 lime/Mg addition at a low pH range, whereas at 1:1 lime/Mg molar ratio the precipitation takes place at pH > 12.
J.W. An et al. / Hydrometallurgy 117–118 (2012) 64–70 67
Fig. 3. Measured concentration profiles of Brine 2 after precipitation of Mg at different lime/Mg molar ratios. Continuous or dotted lines are those predicted by stoichiometric cal-
culations (for Mg) or from Stabcal, except pH which was measured throughout the test.
at a pH > 8.6, whereas the precipitation of gypsum (CaSO4.2H2O) and pH > 8.6) is a mixture of gypsum and Mg(OH)2 which needs to be fur-
Na2SO4 takes place over a range of pH from pH2 to 12. The equilibri- ther processed to separate Mg from the gypsum waste. As shown
um concentrations of Ca, Mg, Na, and SO4 ions are therefore con- later, this precipitate also contained boron which was recovered by
trolled by these precipitates during lime addition. Lithium is stable adsorption during the first-stage precipitation. Further processing of
as soluble Li + ions over a wide range of pHs whereas solid this mixed product is required to recover high purity Mg and B by-
(CaO)2∙ B2O3 and (CaO)3∙B2O3 could be formed at a pH > 12. products from the mixed precipitate. The results of this study will
Several other precipitants (containing Na or Ca to avoid contaminat- be reported later. Residual Mg after lime precipitation and almost
ing the brine) were also tested, including sodium carbonate, sodium all soluble Ca can then be subsequently removed by adding sodium
phosphate, caustic (sodium hydroxide) and sodium oxalate. The precip- oxalate. This second-stage precipitate can be converted to MgO ∙CaO
itation of Ca/Mg carbonate, phosphate, hydroxide and oxalate took (dolime) by roasting for re-use in the lime precipitation stage.
place rapidly and residual Ca/Mg concentration could reach steady Stabcal modelling (Fig. 2) was also used to predict accurately the
state within 1 h. All carbonate, phosphate and oxalate precipitates equilibrium concentrations of Na, K, Li and Cl and other minor ele-
could be recovered easily by filtration. However the Mg(OH)2 precipi- ments in the brine as shown in Fig. 3. At a lime addition of 0.1:1
tate formed from NaOH addition was fine and non-crystalline (particle Ca(OH)2/Mg molar ratio, the pH rises from pH7.1 to pH8.6, effecting
sizes b10 μm) and could not be easily separated from the viscous brine. the precipitation of Mg(OH)2. Stabcal however could not predict the
Our preliminary studies based on precipitation tests and Stabcal Mg equilibrium conditions accurately as there was large variation of
modelling showed Ca could be removed selectively in the first stage Mg concentration with respect to pH along the steep precipitation
using phosphate. Mg could also be removed as pure Mg3(PO4)2 salts line of Mg(OH)2, as seen in Fig. 2. The predicted Mg equilibrium con-
in the subsequent stage. These phosphates are valuable fertilizer centration therefore was stoichiometrically calculated from the lime
products. However even at additions of phosphate at PO4/Mg stoi- additions. Sodium sulphate started precipitating also (Fig. 2) within
chiometric ratios >2:1 the residual Mg concentration in the treated this range of pH, causing slight dips in both Na and SO4 concentra-
brine was still very high (at ~4 g/L Mg). This excessive use of phos- tions as measured by chemical analysis. As more lime is added,
phate would contaminate the liquor and cause further complications Na2SO4 re-dissolves, releasing SO4 ions for the formation of the less
in the following stages. When sodium carbonate was used as precip- soluble gypsum. The steady state concentrations measured after one
itant, the double salt of CaCO3.MgCO3 was formed in the neutral pH hour however showed lower precipitated Mg compared to stoichio-
range, negating the complete recovery of pure Mg products. metric predictions (i.e. higher Mg concentration remaining in the
Lime is the best precipitant that can be used for removing Mg from brine) indicating incomplete reaction of lime and Mg ions. This is
the brine, although it has to be added in slight excess for complete Mg expected with lime neutralization as the formation of gypsum coating
removal. The precipitation of gypsum (CaSO4.2H2O) also reduces the
sulphate to b1 g/L in the treated brine. The precipitate formed (at
0.7
60
0.6
Boron Concentration (g/L)
0.5
40
Zeta Potential (mV)
0.4
0.3
20
PZC 0.2
0 0.1
0
0 0.2 0.4 0.6 0.8 1
-20
7 8 9 10 11 12 13 Ca(OH)2/Mg2+ Ratio
pH
Fig. 5. Removal of boron from Brine 1, at different consecutive additions of Ca(OH)2
Fig. 4. Zeta potential measurements at different pHs showing the point-of-zero-charge (diamonds: addition at 0.1× stoichiometry each time, circles: at 0.2 × mole ratio, trian-
(PZC) at pH11.3. gles: 0.3 × mole ratio).
68 J.W. An et al. / Hydrometallurgy 117–118 (2012) 64–70
120 220
Na 20
80 210
15
Cl 10 SO4
Concentration (g/L)
40 200
K 5
0 190 0
0 10 20 30 40 50 60 0 10 20 30 40 50 60 0 10 20 30 40 50 60
0.7 32 4.5
0.6
0.5 24
3
0.4
16
0.3
Mg Li 1.5 B
0.2
8
0.1
0 0 0
0 10 20 30 40 50 60 0 10 20 30 40 50 60 0 10 20 30 40 50 60
Concentration Factor
would prevent complete dissolution of lime particles for the reaction. removal of Mg and Ca by lime and oxalate precipitation is minimal
The pH rose steadily from pH8.6 to pH9.2 at further additions of lime (within 3% of the analytical analysis error) as indicated in Table 2.
until the 1:1 Ca(OH)2/Mg molar ratio was reached. After this, the pH Following conventional techniques, lithium could be concentrated
would rise to pH > 11.5 at a further addition of lime. Above pH12, to 6% Li by solar evaporation. The operation was simulated in the lab-
Stabcal predicts that sodium sulphate would re-precipitate at 1:1 oratory in several trials to concentrate the brine several folds from the
lime/Mg molar ratio (as shown Fig. 2). initial volume of 4 L. In this context the degree of evaporation was
The recovery of boron during lime addition corresponding to the measured as the ratio between the initial volume and the volume of
lime/Mg molar ratio of 0.1:1 to 1:1 is mainly due to adsorption by brine recovered after evaporation and pressure filtration or centrifug-
the Mg(OH)2-gypsum mixed precipitate. This was confirmed by the ing, defined as Concentration Factor, representing the number of folds
measurement of zeta potential of the Mg(OH)2 precipitate. Fig. 4 the brine was concentrated by. Heavy losses of Li due to evaporated
shows the zeta potential Ezeta measured as 0–60 mV for the pH brine caught in NaCl, KCl and other complex salts precipitated during
range of pH8–11.3, with the zero-point-of-charge at pH11.3. Above evaporation were observed. As shown in Fig. 7, to achieve 20 g/L and
this pH, the surface of Mg(OH)2 is only lightly negatively charged. As 30 g/L Li, the maximum recovery of Li from evaporation and pressure
shown in the Stabcal stability diagrams (Fig. 2) boron exists as filtration is ~ 80% and 60%, respectively. In practice, using pond solar
HB4O7− or B(OH)4− cation within the range pH8–12, and therefore is evaporation the recovery is expected to be lower as the solid/liquid
easily adsorbed onto Mg(OH)2 below the point-of-zero-charge. The separation operation would not be as effective as in laboratory
Stabcal modelling however could not predict the adsorption process studies.
as shown in Fig. 3, where large discrepancies exist between the The cumulative losses of major ions are shown in Fig. 8. In the first
model prediction and boron concentration measured. The solution period when the concentration factor is b5, the precipitation of NaCl
pH increased steadily to pH ~ 11.5 at further additions of lime until is more predominant. After that (concentration factor: 5–20) KCl
1:1 stoichiometry. After this, the adsorbed boron was released from co-precipitates with some loss of Mg measured, possibly as Mg-
the Mg(OH)2 back to the brine. However with lime addition past 1:1 chloride salt or by adsorption on NaCl and/or KCl. By mass balancing
stoichiometry, (CaO)2B2O3 and (CaO)3B2O3 started precipitating as in- the cumulative number of moles losses, i.e. Δ(mol), from the liquor
dicated by Stabcal, causing incomplete recovery of boron at high pHs. obtained after evaporation, it was confirmed that most of the salt
The adsorption process was reproducible at different modes of lime
addition as shown in Fig. 5 (at 0.1×, 0.2× or 0.3× lime/Mg stoichio- 100
metric ratio). Typical compositions of the brine after lime treatment,
added at 1:1 Ca(OH)2/Mg molar ratio are listed in Table 2.
80
60
The residual Mg and Ca, including added amounts from lime,
could be removed using sodium oxalate (added at 1:1 sodium oxa-
40
late/[Ca + Mg] molar ratio to b50 ppm Ca and 170 ppm Mg). The con-
centrations of other ions after sodium oxalate treatment are also
shown in Table 2. The precipitate obtained is a mixed Ca–Mg oxalate 20
which can be converted to dolime (CaO∙MgO) by roasting for re-use
in the first stage of lime precipitation.
0
0 10 20 30 40 50
3.3. Concentration of lithium by evaporation
Achieved Li concentration (g/L)
After Mg, B and Ca were removed the brine contained Li, Na and K Fig. 7. Li recovery after consecutive evaporation of Brine 1 to achieve 10, 20, 30, 40 and
in a chloride brine of low sulphate. The loss of lithium throughout the 50 g/L Li targets.
J.W. An et al. / Hydrometallurgy 117–118 (2012) 64–70 69
25 2 25
20 20
1.5
15 Run 1 Run 1
15 Run 1
Run 2 1 Run 2 Run 2
10 Run 3 10 Run 3
Run 3
Na Run 4 0.5 K Run 4 Cl Run 4
5 5
Run 5 Run 5 Run 5
Δ(Mol)
0 0 0
0 10 20 30 40 50 60 0 10 20 30 40 50 60 0 10 20 30 40 50 60
0.03 0.2 0.05
0.025 0.04
0.15
0.02
Run 1 Run 1 0.03 Run 1
0.015 Run 2 0.1 Run 2 Run 2
Run 3 Run 3 0.02 Run 3
0.01 Mg Run 4 Li B Run 4
0.05 Run 4
0.005 Run 5 Run 5 0.01 Run 5
0 0 0
0 10 20 30 40 50 60 0 10 20 30 40 50 60 0 10 20 30 40 50 60
Concentration Factor
Fig. 8. Cumulative losses (as number of moles) of various ions after evaporation of Brine 1.
precipitated during the early stage of evaporation (at b20 folds) was a Table 3
mixture of NaCl and KCl (i.e. Δ(mol) (Cl −) = Δ(mol)(Na +) + Δ(mol) Composition of lithium carbonate (99.55%) product.
10
Acknowledgement
8 This work was supported by a grant from the Energy Efficiency &
Resources of the Korea Institute of Energy Technology Evaluation
and Planning (KETEP), Ministry of Knowledge Economy, Korea (no.
6
0 20 40 60 80 100
2010 T100100408).
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