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Materials 2019, 12, 1968 9 of 13 Materials 2019, 12, x FOR PEER REVIEW 9 of 13 3..2..SSlulurrryyCoonncceennttrraattioionnooffLLiAiAll--LDHss--11 LiitthiiumiionssweerreeexttrracctteedffrromLiiAll--LDHss--11attdiifffferentt sllurry concenttrrattiionssrrangiingffrrom 10 g//L to 50 g/L. At 10 g/L, the diffffraction line can be indexed to the planes (002),, (110)),, ((022)),, and ((324))offAll(OH))3 ((JJCPDSSCaarrdNo..333--0001188))iinttheeXRDpattterrnss[[34,,35]]..Asstthesllurrryconcenttrrattiion 3 + iinccrreasseed,,tthediissolluttiionoffLii frfroomtthheeLiiAl-l-LDHss-1-1bbeeccaameemoorreeiinccomplleettee,,assttheLiiAll--LDHss ++ ctohnecleitnhtiruamtiorne,ctohverlyithpieurmcenretacgoevedreycrpeearsceedn,toangethdeecorenatsreadry,,oLni thcoenccoenttrrartyio,nLinctohnecfielnttrraatetioincrineatsheed ++ fgilrtaradtueailnlycr.eTashedligtrhaiduumalrleyc.oTvherylitpheiurcmenrteacgoevewryasp8e6rc.2e%nt,aagnedwtahse8c6o.2n%ce,natnrdattihoencofnLceintirnatihoenloiqfuLid ◦◦◦◦◦ phaseexiisttedatt2theta11..59°,,23..21°,,35..74°,,6633.2.200°,,aanndd6644.4.433° (F(FigiguurreeSS33).). Fiigurree 6 showss tthe effffects of slurry concentration on the lithium recovery percentage and Li + cconcenttrrattiionininthtehfieltrfailtter,awteh,icwhhisicchonissistceonntswisitehnXtRwDidthataX.RWDithdiantcar.eaWsinitghsluinrcryrecaosnincgentsrlautrioryn, ipnhtahseelwiqausid14p1h.6asmegw/Lasw1h4e1n.6tmhegs/lLurwryhecnonthcenstlruartrioyncownacse1n0trga/tLio.nCwonatsin1u0ingg/Lt.oCinoncrteinasueinthgetoaminocurenatsoef ++ trheeacatmanotusn(5t0ofg/rLe)actaaunstesd(5th0egl/iLth)icuamusredcotvherlyitpheiurcmenrteacgoevteorybepoenrclyen3t5a.g4%e t,obbuet tohnelyLi35c.4o%nc,ebnutrtatthioenLin ctohnecfielnttrraatteiorenaicnhethde3f1i8lt.r3amtegr/eLa.cAheccdo3rd18in.3gmtogE/Lq.uAatcicoonrd(3i)n,gthteo iEnqcrueatsioenof(3p)r,otdhuecitncorenacseenotrfaptiroondwuciltl caoffnecetntthreatbiaolnanwcielloaffrfeacctttihoen,banladntcheoafmreoaucnttionf,liatnhdiutmhedaismsoluvnedt ofrfolmithtihuemsodlisdsoplhvaesde fdreocmreathsess, othliuds 3+ 3+ ptheasleithdiuecmreraesceosv,etrhyupserthcentlaitgheiudmecreacsoevde.rAylperwceanstnaogteddeteeccrteadseind.thAeldetwecatsionoltimdiettbeyctIeCdP,insotthee dliettheicutmioniolnimsoitlubtyioInCwP,itshoouthteimlitphuiuremioinosnwsoasluotbiotnainweidth, owuhticimh lpeudrteoiothnes ewxtarsacotbiotaninaned, ewnrhiicchmlednttof tlhiteheiuxmtrafcrtoiomnsanltdlaekneribchrimne.nt of lithium from salt lake brine. Figure 6. Lithium recovery percentage (round symbol) and Li+ concentration in the filtrate (triangle symbol) from LiAl-LDHs-1 slurry at varying concentrations of+10 g/L, 20 g/L, 30 g/L, 50 g/L. Figure 6. Lithium recovery percentage (round symbol) and Li concentration in the filtrate (triangle symbol) from LiAl-LDHs-1 slurry at varying concentrations of 10 g/L, 20 g/L, 30 g/L, 50 g/L. The chemical shift of 27Al varies with the slurry concentration according to NMR. The chemical shift was 6.07, 6.30, 6.32, an27d 6.38 ppm at 10 g/L, 20 g/L, 30 g/L, and 50 g/L, respectively (Figure S4) [36]. The chemical shift of Al varies with the slurry concentration according to NMR. The chemical This change was affected by the lithium recovery percentage, which was the same trend as shown in shift was 6.07, 6.30, 6.32, and 6.38 ppm at 10 g/L, 20 g/L, 30 g/L, and 50 g/L, respectively (Figure S4) Figure 4. The chemical shift was clearly more biased toward the low-field with the increase in lithium [36]. This change was affected by the lithium recovery percentage, which was the same trend as recovery percentage (i.e., decreased slurry concentration), which meant that the LiAl-LDHs phase shown in Figure 4. The chemical shift was clearly more biased toward the low-field with the increase convertedmoretotheAl(OH) phase. 3 in lithium recovery percentage (i.e., decreased slurry concentration), which meant that the LiAl-LDHs phase converted more to the Al(OH)3 phase. 3.3. Lithium Recovery Temperature 3.3. LiLthitihuimumRe-ciovnereyxtTreamctpioernatautredifferent reaction temperatures was investigated. With increasing reaction temperature, the LiAl-LDHs phase gradually disappeared, showing the Al(OH)3 phase Lithium-ion extraction at different reaction temperatures was investigated. With increasing (Figure S5). No other phase was detected at 85 ◦C and 95 ◦C. reaction temperature, the LiAl-LDHs phase gradually disappeared, showing the Al(OH)3 phase The temperature dependence of the lithium recovery percentage was investigated over the range (Figure S5). No other phase was detected at 85 °C and 95 °C. of 65 ◦C to 95 ◦C (Figure 7). At lower temperatures (65–75 ◦C), the lithium recovery percentage is more The temperature dependence of the lithium recovery percentage was investigated over the sensitive to temperature, so the lithium recovery percentage increased rapidly as the temperature rose. range of 65 °C to 95 °C (Figure 7). At lower temperatures (65–75 °C), the lithium recovery percentage At 95 ◦C, the chemical reaction reached equilibrium, that is, the amount of lithium dissolved from the is more sensitive to temperature, so the lithium recovery percentage increased rapidly as the temperature rose. At 95 °C, the chemical reaction reached equilibrium, that is, the amount of lithium .PDF Image | Lithium Recovery Pre-Synthesized Chlorine-Ion-Intercalated
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