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Mechanism and Modelling of Reactive Crystallization Process of Lithium Carbonate

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Mechanism and Modelling of Reactive Crystallization Process of Lithium Carbonate processes Article Mechanism and Modelling of Reactive Crystallization Process of Lithium Carbonate 1, 2,3, 1 2,3 1 1 1 Shaolei Zhao y, Jie Gao y, Siyang Ma , Chao Li , Yiming Ma , Yang He , Junbo Gong , Fu Zhou 4, Bingyuan Zhang 2,4 and Weiwei Tang 1,* 1 School of Chemical Engineering and Technology, State Key Laboratory of Chemical Engineering, The Co-Innovation Center of Chemistry and Chemical Engineering of Tianjin, Tianjin University, Tianjin 300072, China; [email protected] (S.Z.); [email protected] (S.M.); [email protected] (Y.M.); [email protected] (Y.H.); [email protected] (J.G.) 2 Tianqi Lithium (Jiangsu) Co., Ltd., Zhang Jiagang 215634, China; [email protected] (J.G.); [email protected] (C.L.); [email protected] (B.Z.) 3 Tianqi Lithium Resources Recycling (Jiangsu) Co., Ltd., Zhang Jiagang 215600, China 4 Tianqi Lithium Corporation, Cheng Du 610000, China; [email protected] * Correspondence: [email protected]; Tel.: +86-22-2740-5754; Fax: +86-22-2737-4971 The authors have contributed equally. y Received: 28 March 2019; Accepted: 23 April 2019; Published: 28 April 2019 Abstract: The reactive crystallization of lithium carbonate (Li2CO3) from lithium sulfate (Li2SO4) and sodium carbonate (Na2CO3) solutions is a key process in harvesting solid lithium, whether from ores, brines, or clays. However, the process kinetics and mechanism remain poorly understood and the modelling of the reactive crystallization of Li2CO3 is not available. Hence, this work aims to determine the kinetics and mechanisms of the nucleation and growth of Li2CO3 reactive crystallization by induction time measurements and to model and optimize the crystallization process using response surface methodology. Induction time measurements were carried out as functions of initial supersaturation and temperature using a laser method. It was found that the primary nucleation mechanism of Li2CO3 varies with solution supersaturations, in which, expectedly, the heterogenous nucleation mechanism dominates at low supersaturations while the homogeneous nucleation mode governs at high supersaturations. The transition point between heterogenous and homogenous nucleation was found to vary with temperatures. Growth modes of Li2CO3 crystals were investigated by relating induction time data with various growth mechanisms, revealing a two-dimensional nucleation-mediated growth mechanism. The modelling and optimization of a complex reactive crystallization were performed by response surface methodology (RSM), and the effects of various crystallization parameters on product and process performances were examined. Solution concentration was found to be the critical factor determining the yield of crystallization, while stirring speed was found to play a dominant role in the particle size of Li2CO3 crystals. Our findings may provide a better understanding of the reactive crystallization process of Li2CO3 and are critical in relation to the crystallization design and control of Li2CO3 production from lithium sulfate sources. Keywords: lithium carbonate; reactive crystallization; crystallization mechanisms; multi-response optimization; response surface methodology 1. Introduction Lithium and lithium compounds can be widely used due to their superior physical and chemical performance [1]. Among them, lithium carbonate (Li2CO3) is one important lithium compound used in Processes 2019, 7, 248; doi:10.3390/pr7050248 www.mdpi.com/journal/processes Processes 2019, 7, 248 2 of 16 Processes 2018, 6, x FOR PEER REVIEW 2 of 17 a[2,3]. wide With range the of applicationsdevelopment such of the as rechargeablelithium battery batteries, industry, ceramics, the consumption glasses, and pharmaceuticalsof Li2CO3 will grow [2,3]. Withrapidly the within development the next offew the years, lithium which battery will industry,lead to a shortage the consumption of this resource of Li2CO in 32020will [4]. grow Therefore, rapidly withinit is necessary the next to few develop years, sustained which will production lead to a of shortage Li2CO3 ofto thismeet resource this increasing in 2020 demand. [4]. Therefore, it is necessaryNowadays, to develop exploitation sustained and production processing of Liof2 saltCO 3laketo meet brines this as increasing well as lithium demand. ores and lithium claysNowadays, have been exploitationproven to be and a feasible processing method of salt oflake producing brines as Li well2CO3 as. Compared lithium ores toand the lithiumtreatment clays of haveores and been clays, proven processing to be a feasible of brines method is more of producing economical Li 2andCO 3requires. Compared lower to energy the treatment consumption of ores and[5]. clays,However, processing there are of brinescurrently is more few economicalreports on the and tr requireseatment lowerof brines energy with consumption high Mg/Li [ratios,5]. However, which thereincreases are currentlythe difficulty few reportsof recovering on the lithium treatment resour of brinesces from with these high matrices Mg/Li ratios, [6,7]. whichFor this increases reason, the distate-ownedfficulty of recoveringmining company lithium Corporación resources from Minera these de matrices Bolivia [(COMIBOL)6,7]. For this developed reason, the an state-owned alternative miningpilot process company for the Corporaci productionón Minera of Li2CO de3 Bolivia from brines (COMIBOL) with a developedhigh Mg/Li an ratio alternative of 22:1 [5]. pilot As process can be forseen the from production Figure 1, as of one Li2CO of the3 from most brines critical with step as highin the Mg production/Li ratio ofchain, 22:1 the [5]. reactive As can crystallization be seen from Figureof Li2CO1, as3 from one of Li the2SO most4 and critical Na2CO steps3 solutions in the production is the last chain, carbonation the reactive stage crystallization of the pilot of process. Li 2CO3 fromFurthermore, Li2SO4 and this Na reactive2CO3 solutions crystalliz isation the lastsystem carbonation for the production stage of the of pilot Li2CO process.3 is also Furthermore, applied in other this reactivemanufacturing crystallization processes system using for lithium-sulfated the production ofminerals Li2CO3 issuch also as applied lepidolite, in other spodumene, manufacturing and processesamblygonite using [8]. lithium-sulfated minerals such as lepidolite, spodumene, and amblygonite [8]. Figure 1.1. FlowsheetFlowsheet of of the the alternative alternative pilot pilot process process used used to produce to produce Li2CO Li32fromCO3 from brines brines with high with Mg high/Li ratiosMg/Li developedratios developed by COMIBOL. by COMIBOL. Reproduced Reproduced with permission with permission from Paola from G. AguilarPaola G. and Aguilar Teofilo and A. Graber,Teofilo A. Industrial Graber, and Industrial Engineering and Engineering Chemistry Research; Chemistry published Research; by published American by Chemical American Society, Chemical 2018. Society, 2018. Reactive crystallization of Li2CO3 plays a key role in recovering lithium resources, whether from ores, brines, or clays. Hence, this process has received significant interest. Sun et al. [9,10] measured the Reactive crystallization of Li2CO3 plays a key role in recovering lithium resources, whether from unseededores, brines, and or seeded clays. Hence, supersolubility this process data has of Lireceived2CO3 in significant aqueous solution interest. using Sun aet laseral. [9,10] apparatus measured and focused beam reflectance measurement (FBRM), respectively. By comparing the two methods, FBRM the unseeded and seeded supersolubility data of Li2CO3 in aqueous solution using a laser apparatus wasand foundfocused to beam be a betterreflectance apparatus measurement with which (FBRM) to detect, respectively. nucleation By events comparing in the the presence two methods, of seed. WangFBRM et was al. [found11] measured to be a thebetter solubility, apparatus supersolubility, with which andto detect metastable nucleation zone widthevents of in Li the2CO presence3 in mixed of lithium chloride (LiCl)-sodium chloride (NaCl)-potassium chloride (KCl)-sodium sulfate (Na SO ) seed. Wang et al. [11] measured the solubility, supersolubility, and metastable zone width of Li22CO43 solutionsin mixed lithium at different chloride temperatures (LiCl)-sodium andanalyzed chloride (NaCl)-potassium the effects of impurities chloride on (KCl)-sodium the thermodynamic sulfate properties of Li CO . Taborga et al. [12] have investigated the effects of different additives on the (Na2SO4) solutions2 3at different temperatures and analyzed the effects of impurities on the size and morphology of Li CO crystals and have proposed that the presence of polyethylenimine thermodynamic properties2 of Li3 2CO3. Taborga et al. [12] have investigated the effects of different (PEI), polyethylene glycol (PEG), and poly (4-styrenesulfonic acid) (P4SA) can increase the length of additives on the size and morphology of Li2CO3 crystals and have proposed that the presence of Lipolyethylenimine2CO3 crystals. Matsumoto (PEI), polyethylene et al. [13] developedglycol (PEG), a novel and crystallization poly (4-styrenesulfonic technique to acid) produce (P4SA) Li2CO can3 nanoparticles using minute gas-liquid interfaces around CO microbubbles activated by microwave increase the length of Li2CO3 crystals. Matsumoto et al. 2[13] developed a novel crystallization irradiation. The results showed that with the formation of numerous local supersaturation regions technique to produce Li2CO3 nanoparticles using minute gas-liquid
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