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Effect of Impurity Ions on Solubility and Metastable Zone Width of Lithium Metaborate Salts

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Effect of Impurity Ions on Solubility and Metastable Zone Width of Lithium Metaborate Salts crystals Article Effect of Impurity Ions on Solubility and Metastable Zone Width of Lithium Metaborate Salts Dan Li 1,2 , Yong Ma 1,*, Lingzong Meng 1,2,* , Yafei Guo 2 , Tianlong Deng 2 and Lan Yang 1 1 School of Chemistry and Chemical Engineering, Linyi University, Linyi 276000, China; [email protected] (D.L.); [email protected] (L.Y.) 2 Tianjin Key Laboratory of Marine Resources and Chemistry, College of Chemical Engineering and Materials Science, Tianjin University of Science and Technology, Tianjin 300457, China; [email protected] (Y.G.); [email protected] (T.D.) * Correspondence: [email protected] (Y.M.); [email protected] (L.M.); Tel./Fax: +86-539-7258620 (Y.M.) Received: 12 February 2019; Accepted: 26 March 2019; Published: 29 March 2019 Abstract: The metastable zone width (MZW) of lithium metaborate salts at various concentrations was determined using the laser technique. The solubility data for lithium metaborate salts was nearly the same in the presence of NaCl at various concentrations. The MZW of lithium metaborate salts decreased when the stirring rate increased, but increased remarkably with increasing cooling rates and an increasing concentration of sodium chloride. The apparent secondary nucleation order for lithium metaborate salts was obtained using the Nývlt’s approach. The apparent secondary nucleation order m of lithium metaborate salts is 4.00 in a pure LiBO2−H2O system with an improved linear regression method. The m for lithium metaborate salts was enlarged in the system LiBO2−NaCl−H2O. Keywords: solubility; metastable zone width; lithium metaborate salts; nucleation order 1. Introduction Various borates are widely used in various industries such as nonlinear optical material, fluorescent material, and laser crystal material. The salt lake brines distributed in Qaidam Basinare rich in lithium and boron resources [1]. Borate is hard to crystallize out, but accumulate in the highly concentrated brine during the brine evaporation [2]. The borate usually has an obvious metastable phenomenon because there are many polyborate ions in the borate solution [3]. Lithium metaborate salt crystallizes from the tetraborate solution during the brine evaporation at a low temperature [4], but lithium tetraborate does not crystallize from the tetraborate solution. Therefore, it is meaningful to study the metastable zone width (MZW) of lithium metaborate salt for its comprehensive utilization of boron resources. The metastable zone of salts was influenced with the dissolution temperature, stirring intensity, cooling rate, impurities, and more [5–13]. The MZW of boric acid, borax decahydrate, and potassium tetraborate tetrahydrate have been investigated in many research studies [8–13], but the metastable zone width of lithium metaborate salts were not been studied in the literature. The univalent ions (Na+) 2+ 2+ narrow the metastable zone of H3BO3, while bivalent ions (Mg , Ca ) broaden it [9,10]. For borax decahydrate, the MZW decreased with KCl in the solution [11]. The variation tendency of MZW varies with the impurity concentrations. A noticeable widening of the MZW was found after adding Cl− 2− and SO4 impurities to the solution [12]. The MZW of K2B4O7·4H2O decreases with the impurity concentration (Li+, Ca2+) increasing [13]. The results show that the MZW of a different borate is very different. In this paper, the laser intensity technique was applied to measure the MZW of lithium metaborate salts both in pure and NaCl solutions. Crystals 2019, 9, 182; doi:10.3390/cryst9040182 www.mdpi.com/journal/crystals Crystals 2018, 8, x FOR PEER REVIEW 2 of 9 is very different. In this paper, the laser intensity technique was applied to measure the MZW of Crystals 2019, 9, 182 2 of 9 lithium metaborate salts both in pure and NaCl solutions. 2. Experimental Experimental Section 2.1. Materials Materials and Apparatus The lithium metaborate with purities of ≥ 0.999 (in mass fraction) and sodium chloride with purities of of ≥≥ 0.9950.995 supplied supplied from from Aladdin Aladdin Industrial Industrial Corpor Corporationation (Shanghai, (Shanghai, China) China) were were used used in the in experiments,the experiments, without without any any further further purification. purification. The The experimental experimental equipment equipment for for determining determining the metastable zone width was listed in Figure 11.. TheThe glassglass crystallizercrystallizer waswas aa tripletriple jacketedjacketed vesselvessel withwith the volume of 250 mL and internal diameter of 70 mm.mm. A thermostatic bath from Jintan Guowang Experimental Instrument Factory (Jintan, China) (THD-2006, temperaturetemperature uncertaintyuncertainty ±±0.10.1 K) K) was applied to control the temperature of the crystallizer.crystallizer. The laser apparatus (GZ-2A, Beijing TuoDa Laser Instrument Co., Ltd. Beijing, China) detected nucleation/dissolutionnucleation/dissolution by by emitting emitting a a light light with a wave length of 632.8 nm into the crystallizer with the solution. The solubilities were measured in a multi-point magnetic stirring thermostatic bath (HXC-500-4A, (HXC-500-4A, Changzhou Nuke Instrument Instrument Co. Co. Ltd., Ltd., Changzhou, China, temperature precision ±0.1±0.1 K). K). Th Thee solid solid phases phases were were identified identified with an Expert PRO X-ray diffractometer (XRD) from Spectris.Spectris. Pte. Ltd., Almelo, The Netherlands. Figure 1. For metastable zone width experiments. 1. Thermostatic bath. 2. Laser generator. 3. Figure 1. For metastable zone width experiments. 1. Thermostatic bath. 2. Laser generator. 3. Electromagnetic stirrer. 4. Photoelectric converter. 5. Numerical indicator. 6. Jacketed glass vessel. 7. Electromagnetic stirrer. 4. Photoelectric converter. 5. Numerical indicator. 6. Jacketed glass vessel. 7. Precise thermometer. Precise thermometer. 2.2. Experimental Method 2.2. Experimental Method The solutions saturated with lithium metaborate salts were obtained with the isothermal dissolutionThe solutions method saturated [14]. The artificialwith lithium synthesized metaborate brines salts were were mixed obtained with some with salts the andisothermal double dissolutiondistilled water. method The [14]. glass The bottles artificial with synthesized brinebrines sand were were mixed placed with insome the magneticsalts and stirringdouble distilledthermostatic water. bath The to obtainglass bottles the equilibrium with synthesized of those brine brines. sand The were clarified placed solutions in the in magnetic each bottle stirring were thermostatictaken out for bath chemical to obtain analysis the equilibrium at least two times.of thos Ife brines. the relative The clarified error among solutions the solution in each contractions bottle were takenfrom theout same for chemical bottle was analysis less than at least 0.3%, two the times. equilibrium If the relative solution error saturated among with the solution undissolved contractions salts can frombe obtained. the same The bottle solid was phases less werethan 0.3%, also separated the equili frombrium the solution solution saturated for the identification with undissolved with XRD.salts canThe be saturated obtained. solution The solid was phases used to were measure also theseparated MZW of from lithium the metaboratesolution for salt.the identification with XRD.The The MZWsaturated of lithium solution metaborate was used to salt me inasure double the MZW distilled of lithium water (DDW) metaborate and thesalt. solution with sodiumThe chlorideMZW of was lithium measured metaborate with the salt laser in DDW transmission and the methodsolution [ 11with]. The sodium saturated chloride solution was measuredwith the volume with the about laser transmission 180 mL obtained method with [11]. the The isothermal saturated dissolution solution wi methodth the volume was placed about into180 mLthe crystallizer.obtained with The the solution isothermal was dissolution cooled with method the settled was coolingplaced into rate untilthe crystallizer. the first visible The solution nucleus wasappears. cooled The with temperature the settled when cooling lithium rate until metaborate the first saltvisible crystallized nucleus appears. was recorded The temperature with Tnuc. D whenTmax lithiumcalculated metaborate with Tnuc andsalt thecrystallized saturation was temperature recorded ( Twithsat) with Tnuc Equation. ΔTmax calculated (1) is considered with T asnuc the and MZW. the saturationThe experiments temperature were carried (Tsat) with out at Equation four constant (1) is cooling considered rates ofas (6.0,the 9.0,MZW. 12.0, The and experiments 18.0) K·h−1 andwere a carriedconstant out stirring at four rate, constant but at cooling various rates saturated of (6.0, solutions. 9.0, 12.0, The and experiments 18.0) K∙h−1 and were a constant run about stirring three times rate, butto ensure at various the accuracysaturated of solutions. the results. The The experiments results of MZWwere run shown about in three this study times wereto ensure the average the accuracy data. of the results. The results of MZW shown in this study were the average data. DTmax = Tsat − Tnuc (1) Crystals 2019, 9, 182 3 of 9 2.3. Analysis Method − The Cl ion concentration was analyzed by titration using an Hg(NO3)2 standard solution with diphenyl carbazone and bromophenol blue as the indicator [15]. The boron concentration was analyzed with the modified mass titration method using NaOH standard solution in the presence of mixture indicators of methyl red plus phenolphthalein and
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