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Membranes 2020, 10, 198 16 of 21 On the other hand, as can be observed in Figure 11, a high initial concentration in the catholyte adversely affects purity of the LiOH solution and therefore less product purity is obtained. This could be attributed to the fact that, for a high LiOH concentration of 5.7 wt%, counterion condensation on the membrane can occur, decreasing its permselectivity [26]. This could also be related to a greater chemical potential difference promoting other unwanted transport mechanisms. An example is that osmotic pressure difference between membrane and electrolyte could generate a water flux and pull some co-ions from the membrane to the LiOH solution. Another explanation is based on the Donnan dialysis of Li+, which due to high catholyte LiOH concentrations, would cause lithium transport to the anolyte and transport of other cations from anolyte to catholyte. However, during the whole operation time, Li+ concentration in the anolyte was higher than that in the catholyte, so the concentration Membranes 2020, 10, x FOR PEER REVIEW 17 of 22 difference indicates that transport by Donnan dialysis would not occur under the studied conditions. It is interesting to compare experiment 1 and expe−riment 12, where anolyte 1-catholyte 2 (2.30 wt% 12, chemical analysis showed a 105% higher Cl concentration in final catholyte compared to LiOH) and anolyte 2-catholyte 1 (1.15 wt% LiOH) were used, respectively. At the same current density, experiment 1. experiment 12 with a higher concentration difference of anolyte and catholyte shows a 4.2% lower Regarding production rate, slight differences were observed according to initial catholyte and cell voltage, 3.3% lower specific electrical consumption and a 2.5% lower production rate of LiOH. anolyte concentrations. This suggests that lithium transport rate depends mainly on electric current However, current efficiency was 15% higher for experiment 1. A high concentrated anolyte can cause a (equation (1)), as long as there is sufficient availability of Li+ ions for migration near the surface of the greater concentration of co-ions in the membrane according to Donnan exclusion. This can decrease membrane. efficiency and permselectivity of the membrane. For experiment 12, chemical analysis showed a 105% From a product purity point of view, it is better to use a low initial catholyte concentration and higher Cl− concentration in final catholyte compared to experiment 1. an anolyte with initial concentration lower than LiCl 32 wt%. Figure 11. Impurities of Na, K and Cl in final catholyte according initial concentration of LiOH. Figure 11. Impurities of Na, K and Cl in final catholyte according initial concentration of LiOH. Regarding production rate, slight differences were observed according to initial catholyte and 4.6. Final Product Chemical Characterization anolyte concentrations. This suggests that lithium transport rate depends mainly on electric current + (EquTahtieonre(s1u)l)t,inasglcoanthgoalsytehearfeteirsesaucffihceixepnetraimvaeinlatbwilaitsysoufbLjeicteiodntsofeovrampoigrraatitoionn, cnreyasrtatlhliezasutirofnacaenodf dthryeinmgetmoborbatnaein. solid LiOH·H2O crystals. Subsequently, the crystals were washed and dried again in aCO2Ffrroemeatpmrosdpuhcetrpeu.rCithyepmoicnatloafnvaileyws,isitriessbueltstefrotrothueseoabltoawineinditciraylsctatlhsoalryetepcroensecnentetrdatiinonTabnldea4n. Iamnpoulyrtietywmitihgrinatiitoianl acocrnocsesntthraetmioenmlobwraenrethinafnluLeinCcle3s2thwetp%u.rity achieved in each experiment. The best results were obtained for experiment 4, when current density was 2400 A/m2, temperature was 75 °C, the membrane was Nafion 117 and the cathode was nickel. These conditions allowed the attainment of high purity LiOH solutions with specific electrical consumption in the electrodialysis membrane process of 10.79 kWh/kg LiOH.PDF Image | Battery Grade Li Hydroxide by Membrane Electrodialysis
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