Thermodynamics Phase Equilibria for the System Containing Lithium

Aug 30, 2013 - The Zabuye salt lake brine is a typical carbonate–borate brine type. There is ..... Institute of Qinghai Salt-Lake of Chinese Academy...
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Thermodynamics Phase Equilibria for the System Containing Lithium, Sodium, Chloride, and Carbonate in Aqueous Solution at 273.15 K Xudong Yu,† Ying Zeng,*,†,‡ Pengtao Mu,† Qinghong Yin,† and Qi Tan† †

College of Materials and Chemistry & Chemical Engineering, Chengdu University of Technology, Chengdu, 610059, P. R. China Mineral Resources Chemistry Key Laboratory of Sichuan Higher Education Institutions, Chengdu 610059, P. R. China

‡

ABSTRACT: The mixed aqueous electrolyte system containing lithium, sodium, chloride, and carbonate has been investigated using the isothermal evaporation method at 273.15 K. The stereophase diagram and the planar projection diagram have been constructed based on the Jänecke method. The compositions of the equilibrated solid phases and liquid phase corresponding to equilibrium points were measured. The system contained only four single salts, sodium chloride (NaCl), lithium chloride monohydrate (LiCl·H2O), lithium carbonate (Li2CO3), and sodium carbonate decahydrate (Na2CO3· 10H2O). Salt LiCl has a strong salting-out effect on the other salts. The density coefficients Ai which were used for the calculation of density at 273.15 K were obtained by fitting. The calculated values of density using an empirical equation have a maximum relative error less than 0.020.

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INTRODUCTION Over the last years, the research of liquid lithium mineral resources is becoming more and more of interest because of the lack of solid deposits. Seawater, salt lake, and underground brine are the representative liquid lithium mineral resources. To exploit these resources, thermodynamics phase equilibria studies on different types of brine are necessary. Commonly, the seawater is of a sulfate type, and the main components of the seawater are sodium, magnesium, chloride, and sulfate, and the research temperature is around room temperature. Compared to seawater, the salt lake has a higher concentration and the temperature in the region of the salt lake is always lower than room temperature; accordingly, the phase equilibrium of the salt lake mostly concentrates on a lower temperature. The underground brine has a higher temperature and higher concentration than seawater; thus the phase equilibrium of underground brine mostly focuses on a higher temperature. The Zabuye salt lake brine is a typical carbonate−borate brine type. There is a natural mineral named zabuyelite that exists in the Zabuye salt lake. The zabuyelite is a high quality raw material used for lithium production.1 The climate conditions in the region of the Zabuye Lake are windy and arid, with little rainfall, and great evaporating capacity, with an average temperature of about 273.15 K.2 Therefore, metastable phase equilibria research at 273.15 K can objectively describe the interaction between the brine minerals and predict the crystallization path of various salts. The main component of the brine mostly belong to the salt − water system containing lithium, sodium, potassium, chloride, carbonate, sulfate, borate ions. Up to now, a number © 2013 American Chemical Society

of papers describing the phase equilibria focused on Zabuye salt lake brine system at different temperature have been reported, such as the investigations on quaternary system Na+ + K+ + CO32− + SO42− + H2O at 273.15 K, and quinary system Na+ + K+ + CO32− + SO42− + borate + H2O at 273.15 K, Na+ + K+ + Cl− + CO32− + borate + H2O at 298.15 K, Na+ + K+ + Li+ + CO32− + borate + H2O at 288.15 K.3−6 The reciprocal quaternary system (LiCl + NaCl + Li2CO3 + Na2CO3 + H2O) is one of the basic subsystems of the Zabuye salt lake brine system. To date, no literature data have been found on the phase equilibrium of this quaternary system at 273.15 K. Accordingly, studying the quaternary system is of both fundamental and practical importance. In the present work, the phase equilibria of this quaternary system at 273.15 K have been studied.

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EXPERIMENTAL SECTION

Analytical grade purity chemicals and doubly deionized water with an electrical conductivity less than 1·10−4 S·m−1 were used to prepare solutions. The isothermal evaporation method was employed in the experiment. A SHH-250 type thermostatic evaporator was used in the solubility experiment, with a device for controlling the temperature at 273.15 ± 0.1 K. The gravity bottle method with a precision of ± 0.0002 g·cm−3 was applied to measure the density of equilibrated solution. The composition of the liquid phase was determined by chemical or instrument analysis. The lithium and sodium ion Received: May 28, 2013 Accepted: August 21, 2013 Published: August 30, 2013 2799

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Table 1. Experimental Values of Solubility and Density of the Equilibrated Solution in the Reciprocal Quaternary System LiCl + NaCl + Li2CO3 + Na2CO3 + H2O at 273.15 Ka Jänecke index of dry salt composition of solution, w(B)·102

a

J(Li22+) + J(Na22+) = J(Cl22−) + J(CO32−) = 100

density/(g·cm−3)

no.

w(Li+)

w(Na+)

w(Cl−)

w(CO32−)

w(H2O)

J(Li22+)

J(Na22+)

J(Cl22−)

J(CO32−)

J(H2O)

expt

calcd

equilibrated solid phase

1,A 2 3 4 5 6 7 8 9,E1 10,B 11,E2 12,C 13 14 15 16 17 18 19 20 21 22 23 24 25,E1 26,D 27,E2 28 29 30

0.00 0.02 0.02 0.03 0.04 0.05 0.07 0.17 0.20 6.83 6.82 0.21 0.22 0.24 0.24 0.30 0.34 0.46 0.59 0.58 0.53 0.57 0.50 0.21 0.20 6.53 6.82 0.65 1.96 2.94

10.88 10.87 10.75 10.85 10.75 10.70 10.65 10.52 10.57 0.00 0.11 3.14 3.55 3.47 3.49 3.33 3.47 3.51 4.04 4.34 4.36 4.64 6.05 9.89 10.57 0.29 0.11 7.01 3.98 1.45

14.48 14.39 14.31 14.40 14.37 14.27 14.06 13.85 13.56 31.99 33.70 0.00 0.71 0.74 0.77 0.89 1.03 1.33 1.81 2.37 3.28 3.59 6.03 12.43 13.56 33.38 33.70 12.61 15.37 16.67

1.78 1.92 1.85 1.94 1.88 1.96 2.16 2.58 3.00 2.11 0.72 5.02 4.97 4.92 4.94 4.86 5.12 5.44 6.26 6.14 5.16 5.44 4.86 3.17 3.00 0.00 0.72 1.14 0.51 0.30

72.86 72.80 73.07 72.78 72.96 73.02 73.06 72.88 72.67 59.07 58.65 91.63 90.55 90.63 90.56 90.62 90.04 89.26 87.30 86.57 86.67 85.76 82.56 74.30 72.67 59.80 58.65 78.59 78.18 78.64

0.00 0.61 0.61 0.91 1.22 1.52 2.13 5.08 5.90 100.0 99.52 18.14 17.04 18.65 18.56 22.99 24.51 30.28 32.61 30.69 28.71 28.93 21.50 6.57 5.90 98.68 99.52 23.47 62.04 87.03

100.0 99.39 99.39 99.09 98.78 98.48 97.87 94.92 94.10 0.00 0.48 81.86 82.96 81.35 81.44 77.01 75.49 69.72 67.39 69.31 71.29 71.07 78.50 93.43 94.10 1.32 0.48 76.53 37.96 12.97

87.46 86.53 86.89 86.42 86.76 86.19 84.80 82.15 79.48 92.85 97.57 0.00 10.91 11.42 11.79 13.57 14.71 17.33 19.86 24.86 35.27 36.13 51.54 77.07 79.48 100.0 97.57 90.44 96.24 97.97

12.54 13.47 13.11 13.58 13.24 13.81 15.20 17.85 20.52 7.15 2.43 100.0 89.09 88.58 88.21 86.43 85.29 82.67 80.14 75.14 64.73 63.87 48.46 22.93 20.52 0.00 2.43 9.56 3.76 2.03

1712 1702 1726 1699 1713 1715 1713 1681 1657 666.8 660.5 6084 5411 5439 5390 5372 4999 4521 3726 3531 3624 3356 2744 1792 1657 696.7 660.5 2193 1904 1797

1.2291 1.2249 1.2265 1.2312 1.2266 1.2274 1.2313 1.2317 1.2352 1.2324 1.2441 1.0919 1.0960 1.0999 1.0973 1.1005 1.0987 1.1052 1.1262 1.1272 1.1245 1.1276 1.1422 1.2194 1.2352 1.2530 1.2441 1.1924 1.1621 1.1592

1.2291 1.2306 1.2277 1.2309 1.2290 1.2290 1.2300 1.2344 1.2392 1.2324 1.2380 1.0919 1.1001 1.0993 1.1000 1.0990 1.1054 1.1136 1.1346 1.1399 1.1330 1.1423 1.1655 1.2257 1.2392 1.2559 1.2380 1.1704 1.1512 1.1430

NaI + NaC NaI + NaC NaI + NaC NaI + NaC NaI + NaC NaI + NaC NaI + NaC NaI + NaC NaI + NaC + LiC LiC + LiI LiC + LiI + NI LiC + NaC LiC + NaC LiC + NaC LiC + NaC LiC + NaC LiC + NaC LiC + NaC LiC + NaC LiC + NaC LiC + NaC LiC + NaC LiC + NaC LiC + NaC LiC + NaC + NaI LiI + NaI LiI + NaI +LiC NaI + LiC NaI + LiC NaI + LiC

Note: NaI−NaCl, NaC−Na2CO3·10H2O, LiI−LiCl·H2O, LiC−Li2CO3.

Table 2. Experimental Solubility Values Corresponding to the Invariant Points of the Binary and Ternary Subsystems in the Quaternary System LiCl + NaCl + Li2CO3 + Na2CO3 + H2O at 273.15 Ka Jänecke index of dry salt composition of solution, w(B)·102 +

+

−

no.

system

w(Li )

w(Na )

w(Cl )

w(CO32−)

a b c d A B C D E1 E2

LiCl-H2O Li2CO3−H2O Na2CO3−H2O NaCl-H2O NaIC LiIC LiNaC LiNaI LiNaIC

6.70 0.29 0.00 0.00 0.00 6.83 0.21 6.53 0.20 6.82

0.00 0.00 2.84 10.34 10.88 0.00 3.14 0.29 10.57 0.11

34.30 0.00 0.00 15.97 14.48 31.99 0.00 33.38 13.56 33.70

0.00 1.23 3.70 0.00 1.78 2.11 5.02 0.00 3.00 0.72

J(Li22+) + J(Na22+) = J(Cl22−) + J(CO32−) = 100 w(H2O)

J(Li22+)

J(Na22+)

J(Cl22−)

2−

J(CO3 )

J(H2O)

59.10 98.48 93.46 73.69 72.87 59.07 91.62 59.80 72.68 58.66

100.0 100.0 0.00 0.00 0.00 100.0 18.14 98.68 5.90 99.52

0.00 0.00 100.0 100.0 100.0 0.00 81.86 1.32 94.10 0.48

100.0 0.00 0.00 100.0 87.46 92.85 0.00 100.0 79.48 97.57

0.00 100.0 100.0 0.00 12.54 7.15 100.0 0.00 20.52 2.43

679.6 26688 8419 1821 1712 666.8 6084 696.7 1657 660.5

equilibrium solid phase LiI LiC NaC NaI NaI+ NaC LiC + LiI LiC + NaC NaI+ LiI NaI + NaC+LiC NaI + LiI + LiC

Note: NaIC−Na+//Cl−, CO32−−H2O; LiIC−Li+//Cl−, CO32−−H2O; LiNaC−Li+, Na+//CO32−−H2O; LiNaI−Li+, Na+//Cl− - H2O; LiNaIC- Li+, Na+//Cl−, CO32−−H2O.

a

acid−base titration with a precision of 0.5 %.7 The composition of the solid phase was determined by X-ray diffractometer with Cu Kα radiation under the operating conditions of 40 kV and 30 mA.

concentration was determined by ICP-OES, with a precision less than 0.06 %. The composition of chloride ion was measured by AgNO3 titration with a precision of 0.3 %.7 The carbonate ion concentration was determined by a method of 2800

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RESULTS AND DISCUSSION The values of solubilities, densities, and composition of equilibrated solid phases in the quaternary system are presented in Table 1. The solubility data of invariant points in the binary and ternary subsystems of this quaternary system were listed in Table 2. In Tables 1 and 2, the ion concentration values were expressed in mass fraction w(B). J(B) is the Jänecke index values of B, with J(Li22+) + J(Na22+) = J(Cl22−) + J(CO32−) = 100. The Jänecke index, that is the Mole percentage, can be calculated according to the following correlations, w(Na +) =

⎡ w(Cl−) w(CO 2 −) 22.99⎢⎣ 35.45 + 2 60.013 −

w(Li+) ⎤ 6.94 ⎥ ⎦g

100 g (solution)

w(H 2O) = 1 − w(Cl−) − w(CO32 −) − w(Li+) − w(Na +)

Letting [B] =

w(CO32 ‐) w(Na +) ⎤ 1 w(Cl−) 1 ⎡ w(Li+) + = ⎢ + ⎥ 2 35.45 60 2 ⎣ 6.94 22.99 ⎦

J(Li 2 2 +) =

1 w(Li+) 100 2 6.94[B]

J(Cl 2 2 −) =

1 w(Cl−) 100 2 35.45[B]

J(H 2O) =

Figure 1. The stereo phase diagram of the quaternary system LiCl + NaCl + Li2CO3 + Na2CO3 + H2O at 273.15 K.

w(H 2O) 100 18.02[B]

With the J(B) in Table 1 and Table 2, the stereo phase diagram of the quaternary system at 273.15 K was plotted, as shown in Figure 1. The shapes of crystallization regions of the system were constructed in Figure 2. The planar projection diagram (Figure 3) are presented as square coordinate, each vertex corresponds to pure components, the points on the sides correspond to the components of ternary systems, the points inside the square characterize the compositions of quaternary mixtures. Figure 4 is the partial enlargement diagram of Figure 3. The planar projection diagram consists of two invariant points, five isothermal evaporation curves, and four crystallization fields. The four crystallization fields correspond to single salts sodium carbonate decahydrate (Na2CO3·10H2O), sodium chloride (NaCl), lithium chloride monohydrate (LiCl· H2O), and lithium carbonate (Li2CO3). The five isothermal evaporation curves, namely curves AE1, BE2, CE1, DE2, and E1E2, are cosaturated with two salts and an equilibrated solution. The cosaturated salts for each univariant curve are listed below. AE1: saturated with NaCl + Na2CO3·10H2O BE2: saturated with Li2CO3 + LiCl·H2O CE1: saturated with Li2CO3 + Na2CO3·10H2O DE2: saturated with LiCl·H2O + NaCl E1E2: saturated with NaCl + Li2CO3 Invariant point of the quaternary system cosaturated with three salts and an equilibrated solution. Figure 5 is the X-ray diffraction pattern of the salts corresponding to the invariant point E1. Figure 5 shows that point E1 is cosaturated with salts NaCl, Na2CO3·10H2O and Li2CO3. The mass fraction composition of the equilibrated solution at the invariant point E1 is w (Li+) = 0.20 %, w (Na+) = 10.57 %, w (Cl−) =

13.56 %, w (CO32−) = 3.00 % and w (H2O) = 72.67 %. Invariant point E2 is cosaturated with salts LiCl·H2O, NaCl, and Li2CO3. The mass fraction composition of the corresponding liquid phase is w(Li+) = 6.82 %, w(Na+) = 0.11 %, w(Cl−) = 33.70 %, w(CO32−) = 0.72 % and w (H2O) = 58.65 %. There are two types of the invariant points, one is incommensurate and the other one is commensurate. In the planar projection diagram, the method to divide the types of invariant point relies on whether a point lies in a triangle formed by corresponding cosaturated salts or not. The commensurate invariant point locates in the triangle, whereas the incommensurate invariant point lies out the triangle.8 In Figure 3, point E1 lies in the triangle formed by its cosaturated salts NaCl, Na2CO3·10H2O, and Li2CO3, point E2 lies in the triangle formed by its cosaturated salts NaCl, LiCl·H2O, and Li2CO3, thus E1 and E2 are both the commensurate invariant point. In the planar projection diagram, the crystallization field of salt Li2CO3 is the largest, which indicates that lithium carbonate is easier to saturate and crystallize than the other three salts from solution at 273.15 K. Whereas the crystallization area of LiCl·H2O is the smallest because of its high solubility. Salt LiCl has a strong salting out effect on the salt NaCl. The effect is caused by the larger polarization of lithium ion, common-ion effect of chloride, and the similarity structure of LiCl and H2O.9 Sodium carbonate can be formed by various hydrated salts, such as Na2CO3·H2O, Na2CO3·7H2O, and Na2CO3·10H2O. Previous research shows that the crystallization forms of Na2CO3 are Na2CO3·10H2O between 273.15 and 298.15 K, Na2CO3·7H2O at 308.15 K, and Na2CO3·H2O at 318.15 K.3,10,11 The results in this system show that Na2CO3·10H2O is the one and only crystallization form of sodium carbonate at 2801

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Figure 2. The shapes of crystallization regions of the quaternary system LiCl + NaCl + Li2CO3 + Na2CO3 + H2O at 273.15 K.

isothermal evaporation curve BE2, with an increase of J(Na22+), the Jänecke index of water reaches the smallest value at the invariant point E2. While on the univariant curve DE2, with an decrease of J(Na22+), the Jänecke index of water reaches the smallest value at the invariant point E2. On the isothermal evaporation curve CE1, the concentration of NaCl increases and the concentration of Na2CO3 decreases in the evaporation process. Salt NaCl has greater solubility in the water than Na2CO3 at 273.15 K, thus with an increase of J(Na22+), the Jänecke index of water decreases gradually until it reaches the invariant point E1. Figure 7 is the density versus composition diagram of the equilibrated solution. The ordinate is the density of equilibrated solution, and the abscissa is the Jänecke index of sodium. The density changes regularly with the Jänecke index of sodium in the solution. On the isothermal evaporation curve AE1, the density value increases with the decreasing value of J(Na22+). On the isothermal evaporation curve DE2, the density value decreases to the invariant point E2 with the decreasing value of J(Na22+). While on the univariant curve BE2, the density value increases to the invariant point E2 with the increasing value of J(Na22+).

Figure 3. The planar projection diagram of the quaternary system LiCl + NaCl + Li2CO3 + Na2CO3 + H2O at 273.15 K.

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CALCULATION OF THE DENSITIES The empirical equation for the density of solutions developed in the previous study was employed in this study.12 ln

d = d0

∑ Ai × wi

where, d and d0 refer the density of the solution and the pure water at 273.15 K, respectively. The d0 value of the pure water at 273.15 K is 0.99987 g·cm−3.13 Ai is the density coefficient of the ith component of the solution, which can be obtained from the saturated solubility of the binary system; wi is the mass fraction of the ith component of the solution. Values of the Ai of NaCl, LiCl, Na2CO3, and Li2CO3 at 273.15 K were obtained by fitting. They are ANaCl = 0.007184, ALiCl = 0.004605, ANa2CO3 = 0.01031 and ALi2CO3 = 0.01180, respectively. On the basis of the empirical equation for the density of solutions, the densities of the equilibrated solutions were calculated. The calculated results are presented in Table 1. The maximum relative error is less than 0.020 for the calculated values relating the experimental ones.

Figure 4. The partial enlargement diagram of Figure 3.

273.15 K, which is in excellent agreement with the earlier reported results. The water content diagram of the system at 273.15 K is constructed in Figure 6. Figure 6 shows that the Jänecke index of water changes regularly with the index of sodium. On the 2802

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Figure 5. X-ray diffraction pattern of the invariant point E1 (Na2CO3·10H2O + Li2CO3 + NaCl).

Figure 6. Water-content diagram of the quaternary system LiCl + NaCl + Li2CO3 + Na2CO3 + H2O at 273.15 K.

Figure 7. Density versus composition diagram of the quaternary system LiCl + NaCl + Li2CO3 + Na2CO3 + H2O at 273.15 K.

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CONCLUSION Thermodynamics phase equilibria in the mixed aqueous electrolyte system containing lithium, sodium, chloride, and carbonate was investigated at 273.15 K. The stereo phase diagram, planar projection diagram, the water content diagram, and the density vs composition diagram were constructed. There are two invariant points, five univariant curves, and four crystallization fields in the planar projection diagram. The crystallized region of Li2CO3 is the largest, and the areas of the crystallization fields decrease in the sequence of Na2CO3· 10H2O, NaCl, LiCl·H2O. Salt LiCl has a strong salting out effect on the salt NaCl. The effect is caused by the larger polarization of lithium ion, common-ion effect of chloride, and

the similarity structure of LiCl and H2O. The densities of the equilibrated aqueous solution change regularly with the composition of sodium in the solution. The calculated densities using an empirical equation have the maximum relative error 0.020 relating the experimental ones.

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AUTHOR INFORMATION

Corresponding Author

*E-mail: [email protected]. Funding

Financial support for this work was provided by the National Nature Science Foundation of China (40673050, 41173071), National High Technology Research and Development 2803

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Program of China (2012AA061704), the Research Fund from the Sichuan Provincial Education Department (11ZZ009), China Geological Survey (12120113087700), and the Research Fund for the Doctoral Program of Higher Education from the Ministry of Education of China (20115122110001). Notes

The authors declare no competing financial interest.

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ACKNOWLEDGMENTS The authors thank the editor and the anonymous reviewers for their critical comments and kind help on the manuscript. REFERENCES

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