Article pubs.acs.org/jced
Solubility Data for the KOH−K2CO3−K3VO4−H2O System at (313.15 and 353.15) K Na Yang,†,‡ Hao Du,† Shaona Wang,*,† Shili Zheng,† and Yi Zhang† †
National Engineering Laboratory for Hydrometallurgical Cleaner Production Technology, Key Laboratory of Green Process and Engineering, Institute of Process Engineering, Chinese Academy of Sciences, Beijing, 100190, China ‡ Beijing Shenwu Environment & Energy Technology Co., Ltd., Beijing, 102200, China
ABSTRACT: The effective separation of K3VO4 and K2CO3 from KOH−K2CO3−K3VO4−H2O system plays an important role in a new vanadium production process developed by the Institute of Process Engineering, Chinese Academy of Sciences. In order to design an effective separation strategy, the dissolution behavior of K3VO4 and K2CO3 in KOH−K2CO3−K3VO4−H2O system at (313.15 and 353.15) K was investigated, and the solubility isotherms were plotted. In addition, the solubility of K3VO4 in KOH solutions was compared with that in K2CO3 saturated KOH solutions, and the solubility of K2CO3 in KOH solutions was also compared with that in K3VO4 saturated KOH solutions. From the solubility data analysis, a method of first separation K2CO3 via cooling crystallization followed by separation K3VO4 via cooling crystallization in the concentrated alkaline solution was proposed.
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INTRODUCTION Vanadium is an important nonferrous metal and due to its outstanding physical and chemical properties, such as high tensile strength, hardness, and resistance to oxidization in air, acid, and alkali solutions,1−6 has been widely used in steel making. Furthermore, vanadium is a promising functional material in making humidity sensors, electrochromic devices, chemical catalysts, and vanadium redox flow battery (VRB). Vanadium slag is one of the most important sources for vanadium extraction, accounting for 58 % of vanadium production globally.7 The chemical composition of typical vanadium slag is vanadium, chromium, iron, silicon, and titanium, etc. Roasting of vanadium slag with sodium salts is currently the most popular vanadium extraction process,8 and the main operating units include roasting, leaching, solution purification, and vanadium precipitation.9 This sodiumination roasting of vanadium slag technology is simple and easy to operate, but suffers from high reaction temperature (1023.15 K to 1073.15 K), low vanadium extraction efficiency (80 % after multiple roasting practice), release of toxic gases such as HCl and Cl2, and generation of a large amount of residue containing high toxic hexavalent chromium and pentavalent vanadium compounds.10,11 The roasting process of vanadium slag with calcium salts solves the problem of toxic gas release, but the high-energy consumption and low vanadium extraction efficiency limit its application in industry.12 Therefore, it is © XXXX American Chemical Society
highly beneficial to develop an efficient and eco-friendly vanadium extraction process that excels in both vanadium recovery and operational easiness. In this regard, a novel vanadium slag treatment process using high concentration KOH solution as reaction media has been proposed by the Institute of Process Engineering, Chinese Academy of Science,13 and the main reaction involved in the process is as follows: 1 FeO • V2O3 + 3KOH + 2 1 3 → Fe2O3 + H 2O + 4 2
5 O2 8 K3VO4
1 7 FeO • Cr2O3 + 2KOH + O2 2 8 1 → Fe2O3 + H 2O + K 2CrO4 4
(1)
(2)
By using high concentration KOH solution media, the reaction temperature for treating vanadium slag can be decreased to 453.15 K, and in comparison with the sodium salt roasting technology the recovery of V and Cr has been Received: November 6, 2012 Accepted: January 28, 2013
A
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increased from 80 % to 95 % and 0 % to 90 %, respectively.13 In this new process, due to the presence of CO2 in air and the carbonate impurities in the KOH reagent, a complex multicomponent solution containing KOH, K3VO4, K2CrO4, and K2CO3 is obtained after solid/liquid separation at 353.15 K. From the solubility data of KOH−K2CrO4−H2O system [(40, 80, and 95) °C] reported in the literatures,14,15 it is proposed that K2CrO4 can be separated via evaporation crystallization based on its dissolution behavior in alkaline solutions at different KOH concentrations. After the separation of K2CrO4, a solution of KOH−K3VO4−K2CO3−H2O at 353.15 K is obtained. The concentration of the solution is as follows: KOH 20 % (mass fraction), K3VO4 5 % (mass fraction), K2CO3 4 % (mass fraction). To design an effective K3VO4 and K2CO3 separation strategy, the solubility data of the KOH−K2CO3− K3VO4−H2O quaternary system is thus highly desirable. The solubility data of KOH−K2CO3−H2O at (313.15 and 353.15) K has been reported in the literature.16 However, the study of the quaternary system of KOH−K2CO3−K3VO4−H2O and the ternary subsystem of KOH−K3VO4−H2O has never been reported up to this time. In this study, systematic work has been carried out to determine the solubility data of the above-mentioned systems at (313.15 and 353.15) K, and further, a separation method based on the solubility data analysis has been proposed.
whether the equilibrium state was reached, and an equilibrium state was proved to be achieved when the composition of the liquid phase did not change with time. All of the solubility data are the average values of three measurements, with the relative standard deviation (RSD) values of less than 2 %. If the liquid phase of the samples prepared by the two methods had the same trend, we could affirm that our samples were in the equilibrium state. Once the system was in the equilibrium state, the shaking was stopped and the samples were kept in the baths for two more days to ensure that all the suspended crystals settled. After equilibrium, the liquid phase was treated as follows: it was removed out by a 1 mL pipet of which the temperature was about (313.15 or 353.15) K. The liquid phase was weighed before it was placed into a volumetric flask with a capacity of 100 mL and then diluted with high-purity water immediately. For the determination of potassium vanadate contents, 1 mL of the previously diluted solution was further diluted 100 times after the addition of 2 mL of concentrated hydrochloric acid. For the determination of potassium carbonate contents, 10 mL of the previously diluted solution was further diluted 10 times after the addition of a certain amount of concentrated hydrochloric acid for adjusting the pH value of solutions between 7 and 8. The solids obtained were washed by ethanol in advance for several times and then dried in a vacuum drying oven until the weight of the solid did not change any more before analysis. To avoid the decomposition of the solid phase, the drying temperature was set at 313.15 K. Analysis. The content of potassium vanadate in the liquid phase was determined by inductively coupled plasma/optical emission spectrometry (ICP-OES, PE Optima 5300DV, PerkinElmer). The content of potassium carbonate in all samples was determined by analyzing CO32− using total organic carbon analyzer (TOC-VCPH, Shimadzu) which also can determine the content of inorganic carbon. Potassium hydroxide was determined by titration using hydrochloric acid solution with phenolphthalein solution as the indicator. All titrations were performed in triplicate, and the amount of sample was chosen for a required titrate volume of more than 5 mL. The mean value of the triplicate titration results was employed. To guarantee the accuracy of the analysis, each equilibrium system was sampled and analyzed at least three times, and the results were the average of multiple measurements with a standard deviation of less than 3 %. The solid phases were identified through X-ray diffraction (XRD, Philips PW226/30 with Cu Kα radiation, 40 kV and 100 mA).
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EXPERIMENTAL SECTION Apparatus and Reagents. A specially designed thermostatic air vibrator (HZ-9612K, Taicang science and education equipment Co., Ltd.) with a precision of ±0.2 K was used to keep samples in an equilibrium state at (313.15 and 353.15) K . A magnetic agitator with water bath (XMTD-701, Taicang science and education equipment Co., Ltd.) with a precision of ± 0.1 K was used for preparing samples at 368.15 K. Polyethylene bottles, each 200 cm3 capacity, containing planned excess solid phase and potassium hydroxide solution, was used for mixing and placed in the thermostat. Some chemicals used in this work, including KOH and K2CO3, were of analytical grade and manufactured by Beijing Reagents Company. Fresh and pure potassium vanadate hydrate crystal [K3VO4·3H2O ≥ 99 % (mass fraction)] was employed in this work, which was provided by Chengde Iron and Steel Group Co. Ltd. High-purity Milli-Q water, with a resistivity of above 18.2 MΩ·cm at 298.15 K was used. Experimental Method. The solubilities were determined by the method of isothermal solution saturation.17 The supersaturated solutions were prepared by two methods. The first method was the dissolution of K3VO4·3H2O and K2CO3 in KOH solutions at 368.15 K. In this method an alkaline solution was prepared by dissolving a certain amount of KOH in highpurity water in a flask positioned in the water bath of magnetic agitator maintained at 368.15 K. Then the salts were added to the alkaline solutions while stirring, and the stirring was stopped when the salts did not dissolve any more. These supersaturated solutions were then transferred into sealed polyethylene bottles, which were placed in thermostatic vibrator at constant temperature (313.15 and 353.15) K. Besides, the verifying experiments employed in the second method were conducted in order to ensure the accuracy of the solubility data. The second method was the addition of different solid phases at constant temperature (313.15 and 353.15) K until they could not be further dissolved. A sampling of the liquid phase was performed every week to determine
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RESULTS AND DISCUSSION Solubility Data of KOH−K3VO4−H 2O System at (313.15 and 353.15) K. The solubility data for the KOH− K3VO4−H2O ternary system at (313.15 and 353.15) K are precisely measured and presented in Table 1. All the solubility data in Table 1 are the average values of three measurements, with the relative standard deviation (RSD) values of less than 2 %. It can be seen from Table 1 that the solubility of K3VO4 decreases monotonically with an increase of KOH concentration at both 313.15 K and 353.15 K, and the solubility of K3VO4 at 313.15 K is significantly lower in comparison with the solubility at 353.15 K. So it is possible to separate K3VO4 from KOH solution using evaporation and/or cooling crystallization. Further observation from Table 1 shows that when the KOH concentration is above 40 % (mass fraction), the solubility of K3VO4 at (313.15 and 353.15) K does not show significant change with KOH concentration anymore, therefore, evapoB
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Table 1. Solubility Data of K3VO4 in KOH Solution at (313.15 and 353.15) K T = 313.15 K
T = 353.15 K
composition of liquid phase (100 w)
composition of liquid phase (100 w)
KOH
K3VO4
equilibrium crystalline phases
3.41 6.60 8.80 11.86 13.35 15.84 18.13 22.37 28.00 33.93 39.45 42.87 47.55 50.72 53.30
56.87 51.64 47.34 41.85 38.39 34.68 30.31 24.56 18.28 14.75 12.13 10.73 9.73 8.89 8.88
K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O
KOH
K3VO4
equilibrium crystalline phases
10.94 13.00 17.62 22.25 25.42 29.78 32.52 37.39 40.29 43.34 47.25
58.43 53.23 44.61 36.54 31.49 25.99 23.79 20.03 19.06 18.15 18.15
K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O
Figure 1. Solubility diagram of the KOH−K3VO4−K2CO3−H2O system.
respectively as KOH concentration increases at (313.15 and 353.15) K, but the decrease trend gets smaller with an increase of alkali concentration. To be more specific, the solubility of K 3VO 4 and K 2CO 3 decreases sharply until the KOH concentration reaches about 37 % (mass fraction). However, when the KOH concentration is above 37 % (mass fraction), the concentration of K3VO4 and K2CO3 at (313.15 and 353.15) K shows a small change with an increase of KOH concentration, and then almost reaches plateau. According to the similar solubility trend of K3VO4 and K2CO3 in KOH solution, it is possible to separate K3VO4 and K2CO3 using the same crystallization separation method. Therefore, it was necessary to study the salting-out effect between two kinds of salt for finally obtaining the effective separation method. The equilibrium solid phases were examined and determined to be K3VO4·3H2O and K2CO3·1.5H2O, and the solubility data is tabulated in Table 2 at both 313.15 and 353.15 K.
ration crystallization of K3VO4 could not be operated at this concentration (CKOH > 40 %). The equilibrium solid phase were examined and determined to be K3VO4·3H2O and the solubility data is tabulated in Table 1 at both 313.15 and 353.15 K. Solubility data of KOH−K3VO4−K2CO3−H2O Quaternary System at (313.15 and 353.15) K. The solubility data for the KOH−K3VO4−K2CO3−H2O quaternary system at (313.15 and 353.15) K are presented in Table 2, and the solubility isotherm at (313.15 and 353.15) K is plotted in Figure 1. All of the solubility data in Table 2 are the average values of three measurements, with the relative standard deviation (RSD) values of less than 2 %. It can be seen from Figure 1 that the solubility of K3VO4 and K2CO3 decreases
Table 2. Solubility Data for the KOH−K3VO4−K2CO3−H2O System T = 313.15 K
T = 353.15 K
composition of liquid phase (100 w) KOH
K2CO3
K3VO4
11.92 13.29 16.07 18.24 21.67 23.52 25.09 27.93 30.36 34.13 38.30 40.61 41.46 42.29 45.84 47.64 49.27
22.64 20.52 16.49 13.98 11.19 9.62 8.08 6.51 5.18 2.97 1.27 0.90 0.78 0.74 0.54 0.50 0.46
39.15 35.75 31.09 27.65 23.12 21.48 19.86 17.29 15.45 13.52 11.43 10.57 10.53 10.07 9.29 9.34 9.30
composition of liquid phase (100 w) equilibrium crystalline phases K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O
+ + + + + + + + + + + + + + + + +
K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O C
KOH
K2CO3
K3VO4
9.33 12.34 13.52 16.15 18.49 22.09 24.05 25.31 28.14 30.08 34.09 38.66 41.64 44.31
36.93 30.75 28.62 24.14 21.35 17.61 15.86 14.37 12.07 10.81 8.52 6.52 5.46 5.09
57.19 51.55 49.48 45.21 41.07 34.89 32.24 30.47 26.94 24.87 21.62 18.85 18.16 18.07
equilibrium crystalline phases K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O K3VO4·3H2O
+ + + + + + + + + + + + + +
K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O K2CO3·1.5H2O
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Comparison of K2CO3 Solubility in KOH Solution with that in K3VO4 Saturated KOH Solution at (313.15 and 353.15) K. The solubility data of K2CO3 in KOH solution at (313.15 and 353.15) K have already been determined by Mr. Qu.16 The solubility data of K2CO3 in K3VO4 saturated KOH solution at (313.15 and 353.15) K are presented in Table 2. The solubility isotherms of K2CO3 in KOH solution with that in K3VO4 saturated KOH solution at (313.15 and 353.15) K are plotted in Figure 4 and Figure 5. It is concluded from Figure 4
Comparison of K3VO4 Solubility in KOH Solution with that in K2CO3 Saturated KOH Solution at (313.15 and 353.15) K. The solubility isotherms of K3VO4 in KOH solution with that in K2CO3 saturated KOH solution at (313.15 and 353.15) K are plotted in Figure 2 and Figure 3, respectively. As
Figure 2. Solubility isotherms of K3VO4 at 313.15 K: ■, in KOH solution; ●, in K2CO3 saturated KOH solution. Figure 4. Solubility isotherms of K2CO3 at 313.15 K: ■, in KOH solution; ●, in K3VO4 saturated KOH solution.
Figure 3. Solubility isotherms of K3VO4 at 353.15 K: ■, in KOH solution; ●, in K2CO3 saturated KOH solution.
shown in Figure 2 and Figure 3, the solubility trend of K3VO4 in KOH solution and K2CO3 saturated KOH solution is the same. To be more specific, the solubility of K3VO4 declines sharply until the KOH concentration reaches 40 % (mass fraction). However, when the KOH concentration is above 40 % (mass fraction), the concentration of K3VO4 at (313.15 and 353.15) K shows a gradual change with an increase of KOH concentration, and then finally remains stable. Compared with the KOH solution without K2CO3, the concentration of K3VO4 in K2CO3 saturated KOH solution decreases only slightly at (313.15 and 353.15) K. The presence of K2CO3 has a small influence on the solubility of K3VO4 in the KOH solution. So the first separation of K2CO3 from K3VO4 saturated KOH solution will not influence the solubility of K3VO4 in KOH solution.
Figure 5. Solubility isotherms of K2CO3 at 353.15 K: ■, in KOH solution; ●, in K3VO4 saturated KOH solution.
and Figure 5 that the solubility of K2CO3 in KOH solution almost declines linearly with an increase of alkali concentration. The concentration of K2CO3 decreases significantly when the alkali solution is saturated with K3VO4 at (313.15 and 353.15) K compared with KOH solution without K3VO4, which suggests that the salting-out effect of K3VO4 to K2CO3 is strong. The presence of K3VO4 has great influence on the solubility of K2CO3 in KOH solution. If K3VO4 was first separated from K2CO3 saturated KOH solution, the solubility of K2CO3 will increase. The separation of K2CO3 from KOH solution for the subsequent crystallization becomes more difficult as the increase of K2CO3 solubility. By studying the D
dx.doi.org/10.1021/je301157h | J. Chem. Eng. Data XXXX, XXX, XXX−XXX
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salting-out effect between two kinds of salt, one finds that the presence of K2CO3 has a small influence on the solubility of K3VO4 in KOH solution. So it is proposed to separate K2CO3 first from KOH solution via evaporative crystallization (CKOH < 40 %) or cooling crystallization (all alkali region). However, the solubility of K3VO4 in KOH solution has a small change after separation of K2CO3. Separation Method of K2CO3 and K3VO4 from KOH Solution. The specific graphical description of the separation process is shown in Figure 6. Points A and B represent the
Funding
The authors gratefully acknowledge the financial support from the National High Technology Research and Development Program of China (863 program) under Grant No. 2011AA060704, No. 2011AA060701, and the National Natural Science Foundation of China under Grant No. 51090382. Notes
The authors declare no competing financial interest.
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Figure 6. Separation process of K2CO3 and K3VO4 in KOH solution.
concentration of K3VO4 and K2CO3 in the original solution [KOH 20 % (mass fraction), K2CO3 4 % (mass fraction) and K3VO4 5 % (mass fraction)] achieved from the new process developed by Institute of Process and Engineering, Chinese Academy of Sciences.13 With the continuous vacuum evaporation of the KOH solution at 353.15 K, the concentration of K3VO4 and K2CO3 increases as shown along the line OA and OB, respectively. K3VO4 will not be salting-out only if the concentration of solution approaches point E. Pure K2CO3 crystal will be got at region S. The concentration of K2CO3 will move from C to D after cooling crystallization. According to better separation property of KOH solution CKOH < 45 % (mass fraction), the cooling crystallization of K3VO4 will operate at region L. So we will get K3VO4 crystal product from this system. However, the K3VO4 crystal acquired as shown at region L has some impurities of K2CO3, but the amount is very small and can be removed in subsequent process.
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CONCLUSIONS Solubility data for the KOH−K3VO4−K2CO3−H2O system and its subsystem KOH−K3VO4−H2O at (313.15 and 353.15) K were studied. From the data obtained from the experiment, a method of separation K2CO3 first via evaporative crystallization (CKOH < 40 %) or cooling crystallization, and then separation K3VO4 via cooling crystallization in the new process was proposed.
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