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Membranes 2020, 10, 198 7 of 21 2.5. Potentiodynamic Sweeps Electrochemical kinetics of anodic and cathodic half-reactions were characterized by potentiodynamic sweeps. Tests were carried out using an Autolab PGSTAT302N potentiostat (Metrohm, Herisau, Switzerland). To study water reduction to gaseous hydrogen, the working electrodes were a bar of nickel and a sheet of stainless steel 316, the counter electrode was a graphite rod. To study water oxidation to oxygen gas and chloride oxidation to gaseous chlorine, the working electrode was graphite and the counter electrode was a nickel bar. The nickel bar, the stainless steel 316 and graphite rod had an apparent surface area of 1.00, 2.70 and 2.87 cm2, respectively. The reference electrode was Ag/AgCl 3 M KCl (0.194 V vs. standard hydrogen electrode (SHE)), the scan rate was 1 mV/s. LiOH as a catholyte and LiCl as anolyte were the solutions used during the experiment. Electrolyte temperatures were kept constant at 75 ◦C and 85 ◦C by a Julabo thermostatic bath, injected through double-jacket recirculation tanks. Electrolyte agitation was kept constant at 120 cm3/min by recirculation using Watson-Marlow 520SN/R2 peristaltic pumps. 2.6. Final Product Characterization Chemical analysis was performed on LiOH·H2O crystal samples to determine chemical composition and concentration range of main impurities. Sodium, potassium, calcium, lithium and magnesium concentrations were determined by atomic absorption spectrometry. Chloride and sulfate were determined by volumetric titration with AgNO3 and BaCl2, respectively. Moisture was determined by drying until constant weight at 40 ◦C was achieved in an inert atmosphere. Sample composition was analyzed by an X-ray Powder Diffractometer. Powdered sample was positioned on a flat plate sample holder after sample powdering in an agate mortar. This technique was used to characterize crystallographic structure by comparing obtained diffraction data with data from a database maintained by the International Centre for Diffraction Data (www.icdd.com). Analysis of X-ray diffraction was performed on an X-Ray diffractometer SIEMENS model D5000 (40 kV, 30 mA); radiation of Cu Ka1 (l = 1.5406 Å); vertical Bragg-Brentano; scan range: 3–70◦ 2q; step size: 0.020◦ 2q; step time: 1.0 s. 3. Results 3.1. Cell Parameter Performance Table 3 shows results obtained in each of the experiments. Production rate, average cell voltage, current efficiency relative to transferred Li+ mass, specific electrical consumption (SEC) and purity of product are presented. Experiments 1, 2 and 3 provide results for different current densities. Experiments 2, 4, 9 and 10 allow comparison of results at four different temperatures. In a similar way, if experiments 2 and 6 are compared and the effect of ion exchange membrane type can be observed. In addition, experiments 2, 8 and 11 show results when using three different initial catholyte concentrations. Experiments 4 and 5 and experiments 6 and 7 provide results for two different cathode types. On the other hand, experiment 12 presents resulting data for high concentration anolyte usage. Each of the different parameters was analyzed. Their effects on parameters such as LiOH production rate, voltage, current efficiency, specific electrical consumption and purity of monohydrate lithium hydroxide were determined.PDF Image | Battery Grade Li Hydroxide by Membrane Electrodialysis
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