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206 P. Meshram et al. / Hydrometallurgy 150 (2014) 192–208 52.32 and 47.72 kJ/mol for Co and Li, respectively (Lee and Rhee, 2003). The leaching reaction with HNO3 solution can be represented as: LiCoO2 was separated from aluminium foil with dimethyl acetamide (DMAC). Polyvinylidene fluoride and carbon powders in the active material were then eliminated by roasting at 450 °C for 2 h and 600 °C for 5 h, respectively. Finally LiCoO2 was obtained by adding a certain amount of Li2CO3 in the recycled LiCoO2 and calcining it at 850 °C for 12 h. 4. Conclusions Lithium is one of the rare metals with a variety of applications and demand for lithium is expected to increase with the ever increasing use of electrical and electronic devices/hybrid electric vehicles. A few established technologies are in vogue to produce lithium in the desired form from its primary resources like its minerals and brine, whereas limited exploitation of lithium resources from seawater and bitterns calls for their intensified tapping. Extraction of lithium from its minerals and clays is fraught with high mining costs and involves high energy, while extraction from brine and bitterns/seawater needs a long time for evaporation. Hence these processes need to be adequately modified to yield efficiency and better economic returns. Extraction processes from secondary resources like batteries depend on the chemistry of the battery material. Most processes involve dis- mantling of LIBs, separation of cathode and anode materials, leaching of valuable metals like Co, Li, Ni, Mn etc. from the cathode material in different mineral acids, and separation and recovery of metals from the solutions by solvent extraction/IX/precipitation. At present no lithi- um extraction is industrially practiced from LIBs. Therefore, a sufficient scope exists not only to reduce the process steps followed currently but also to improve the efficiency of metal extraction and separation, in- cluding lithium recovery. Points that may be considered include process intensification to save energy and improve the kinetics of leaching, while addressing the problem of selectivity and examining the use of unexplored/synergistic solvents with an ultra high metal loading capac- ity to cut down the process steps. There is a need to develop appropriate technology which can address the limitation of current processes for extraction of all valuable metals from its primary as well as secondary resources. Acknowledgements The authors are thankful to the Director, CSIR-National Metallurgical Laboratory (NML), Jamshedpur, India for giving permission to publish the paper. References Abe, Y., 2010. Rare metal series — current status of lithium resources. JOGMEC Mineral Resources Report. Abe, M., Hayashi, K., 1984. Synthetic inorganic ion-exchange materials. XXXIV. Selective separation of lithium from seawater by tin(IV) antimonate cation exchanger. Hydrometallurgy 12, 83–93. Aktas, S., Fray, D.J., Burheim, O., Fenstad, J., Acma, E., 2006. Recovery of metallic values from spent Li ion secondary batteries. Miner. Process. Ext. Metall. (Trans. Inst. Min. Metall. C) 115 (2), 95–100. Alberti, G.M., Massucci, M.A., 1970. Crystalline insoluble salts of tetravalent metals. IX. Thorium arsenate, a new inorganic ion-exchanger, specific for lithium. J. Inorg. Nucl. Chem. 32, 1719–1727. Amer, A.M., 2008. The hydrometallurgical extraction of lithium from Egyptian montmorillonite-type clay. J. Met. 60 (10), 55–57. An, J.W., Kang, D.J., Tran, K.T., Kim, M.J., Lim, T., Tran, T., 2012. Recovery of lithium from Uyuni salar brine. Hydrometallurgy 117–118, 64–70. Australia's Mineral Resource Assessment (AMRA), 2013. http://www.ga.gov.au/corporate_ data/77481/77481_AMRA_v2.pdf. Averill, W.A., Olson, D.L., 1978. A review of extractive processes for lithium from ores and brines. Energy 3, 305–313. Bach, R.O., Wasson, J.R., 1981. Lithium and lithium compounds, 3rd edition Ch. in Kirk- Othmer: Encyclopedia of Chemical Technology vol. 14. Wiley, pp. 448–476. Banerjee, D.C., Krishna, K.V.G., Murthy, G.V.G.K., Srivastava, S.K., Sinha, R.P., 1994. Occurrence of spodumene in the rare metal bearing pegmatites of Marlagalla– Allapatna area, Mandya District, Karnataka, India. J. Geol. Soc. India 44, 127–139. 2LiCoO2ðsÞ þ 3HNO3ðaqÞ→Li2NO3ðaqÞ þ 2CoðNO3Þ2ðaqÞ þ 3H2O 1 Recycling of Li-ion and polymer batteries while producing LiCoxNi(1− x)O2 as a cathode material was investigated by Lupi and Pasquali (2003). The process consists of cathodic paste leaching, Co–Ni separation by SX and recovery of Ni by electrowinning. The separation of Ni/Co was performed by solvent extraction using saponified 0.5 M Cyanex 272. Nickel was electrowon at a current density of 250 A/m2, 50 °C and pH 3–3.2 with an electrolyte of 50 g/L Ni and 20 g/L H3BO3. Elaborating further, Lupi et al. (2005) reported the current efficiency and energy consumption of 87% and 2.96 kWh/kg for nickel under the above conditions as compared to the figures of 96% and 2.8 kWh/kg, respectively for cobalt at the same current density and temperature, but at pH 4–4.2 from a solution containing manganese and (NH4)2SO4. 3.3.2.4. Metal extraction using organic acids/reagents. For the sustainable management of the secondary resource such as LIBs, organic acids such as DL-malic acid, citric acid etc. which have mild acidity, are sug- gested for the leaching of metals (Table 11). Li et al. (2010a) reported that DL-malic acid can dissolve lithium and cobalt of LIBs fairly rapidly under aerobic and anaerobic conditions as compared to the mineral acids like HCl, HNO3 and H2SO4, and the waste solutions can be treated easily. Almost 100% Li and N 90% Co were leached out with 1.5 M malic acid and 2.0% H2O2 at 90 °C in 40 min. Leaching of lithium and cobalt in citric acid was also reported after separating the anode and cathode material by the treatment of NMP (Li et al., 2010b). Nearly 100% Li and N 90% Co were extracted in 1.25 M citric acid and 1.0% H2O2 at 90 °C. Recently ultrasonic assisted leaching of cobalt and lithium from spent LIBs in the presence of ascorbic acid was investigated (Li et al., 2012). Leaching efficiencies of as high as 94.8% for Co and 98.5% for Li were achieved with 1.25 M ascorbic acid solution at 70 °C (Table 11). Sun and Qiu (2012) used oxalic acid as both leachant and precipitant to separate and recover cobalt and lithium from the spent LIBs. Cathode material consisting of LiCoO2 and CoO from the dismantled batteries, was peeled off from the aluminium foils after vacuum pyrolysis at 600 °C. Leaching was performed using 1 M oxalate at 80 °C with the reaction efficiency of N 98% of LiCoO2 while separating cobalt and lithium. The reaction with oxalate for leaching and precipitation proceeds as: 3H2C2O4 þ LiCoO2ðsÞ→LiHC2O4 þ CoðHC2O4Þ2 þ 2H2O þ 2CO2ðgÞ ð26Þ 4H2C2O4 þ 2LiCoO2ðsÞ→Li2C2O4 þ 2CoC2O4ðsÞ þ 4H2O þ 2CO2ðgÞ: ð27Þ During the oxalate leaching Co3 + was reduced to Co2 + which was dissolved and precipitated as cobalt(II) oxalate (Sun and Qiu, 2012). The reduction of Co3 + to Co2 + is also believed to proceed by the reaction of CO2 radicals generated from oxalic acid (Hoffman and Simic, 1973). The electrochemical performance of nano-Co3O4 anode material prepared from the spent LIBs was evaluated by Hu et al. (2013). From the leach liquor obtained from the alkali and acid process, Al(OH)3, MnOOH, Cu(OH)2 and Ni(OH)2 were removed at a pH N5 which was followed by the precipitation of CoC2O4 at pH 2 by adding a saturated solution of (NH4)2C2O4. The product CoC2O4 was used to synthesize nano-Co3O4 by the sol–gel method. þ 2 O2ðgÞ : ð25Þ The roasting of batteries under reduced pressure at 650 °C was reported by Kondás et al. (2006), which was followed by the leaching of Li2CO3 at ambient temperature and crystallization of pure Li2CO3. A process for the recycling and synthesis of LiCoO from the incisors 2 bound of Li-ion batteries was developed by Liu et al. (2006). Firstly,PDF Image | Extraction of lithium from primary and secondary sources
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