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Processes 2019, 7, 248 3 of 16 crystals were also reported [9–13]. However, there have been no works concentrating on the reactive crystallization mechanisms of Li2CO3 from Li2SO4 and Na2CO3 solutions and multi-objective optimization of the process. Here, the nucleation and growth kinetics and mechanisms of Li2CO3 in reactive crystallization are investigated and the complex reactive crystallization process is modeled and optimized using a novel method named response surface methodology. First, the induction times for the reactive crystallization of Li2CO3 were measured over a range of supersaturations at different temperatures using a laser method. Then, the effects of supersaturation levels and temperature on the nucleation behavior of Li2CO3 crystals were studied. Further, various mechanisms of crystal growth were examined and the crystal growth mode of Li2CO3 was determined on the basis of data fitting between experiments and theory. Finally, a response surface methodology (RSM) with central composite design (CCD) was developed to understand the effects of various operating parameters on the performance of the process. The significance of models was further revealed by analysis of variance (ANOVA). 2. Materials and Methods 2.1. Materials and Experimental Procedures Lithium sulfate (99.9% metal basis) was purchased from Chemart Chemical Technology Co. Ltd. (Tianjin, China). Sodium carbonate (AR, ≥99.8%) was purchased from Titan Scientific Co. Ltd. (Shanghai, China). Water was filtered through a double-deionized purification system and was used as the solvent in all experiments. All chemicals were used directly without further purification. The induction times were experimentally measured as functions of initial supersaturation and temperature using a laser method. In accordance with a previous work [9], a 100 mL crystallizer with a water bath (CF41, Julabo, Germany), a temperature indicator (Pt-100, Julabo, Germany), an overhead mechanical stirrer (WB-2000C, Julabo, Germany), and a laser apparatus (JSW3-300, Mettler Toledo, Switzerland) were used for induction time measurement. Firstly, a 40 mL Li2SO4 solution was introduced into the crystallizer and then agitation at 300 rpm in a water bath was initiated. When the solution temperature stabilized, the preheated 40 mL Na2CO3 solution was poured into the crystallizer and the laser apparatus was turned on simultaneously; this was recorded as the start time. The same molar concentration of Li2SO4 and Na2CO3 solution was calculated according to the specified supersaturation. In the initial period, the solution was clear and the light intensity stayed constant, whereas when the primary nucleation occurred, the light intensity decreased sharply due to the diffraction and dispersion effect. The induction time can be calculated according to the interval between the start time and the time when the light intensity decreases sharply. During the experiment, the crystallizer was sealed to avoid the occurrence of water evaporation. The experimental set up for optimizing the reactive crystallization process is similar to the induction time measurement set up. Firstly, 40 mL Li2SO4 solution was introduced into the crystallizer, and then water-bath agitation was initiated. When the solution temperature stabilized, the peristaltic pump was turned on to feed the Na2CO3 solution. The molar concentration of the Li2SO4 and Na2CO3 solutions was the same. Upon finishing feeding, the crystallizer was sealed and the solution temperature was kept constant for 150 min to ensure that the Li2CO3 crystals grew sufficiently. After the reaction, the slurry was filtered while hot and the filter cake was washed three times with absolute ethanol and dried in an oven at 50 ◦C for 12 h to remove free water. Finally, the particle size and crystal size distribution of the Li2CO3 product were analyzed using Morphology 3000 (Malvern, UK).PDF Image | Reactive Crystallization Process of Lithium Carbonate
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