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Lawagon, Chosel P.,Nisola, Grace M.,Cuevas, Rosemarie Ann I.,Kim, Hern,Lee, Seong-Poong,Chung, Wook-Jin Elsevier 2018 CHEMICAL ENGINEERING JOURNAL -LAUSANNE- Vol.348 No.-
<P><B>Abstract</B></P> <P>With the heightened global demand for lithium, more energy-efficient processes with fast Li<SUP>+</SUP> production rates are essential for sustainable Li<SUP>+</SUP> supply. Electrochemical Li<SUP>+</SUP> recovery is a promising method that could satisfy these process necessities. However, its success requires highly effective electrodes that could selectively capture Li<SUP>+</SUP> at a competitive uptake capacity with minimal energy requirement. Delithiated Li<SUB>1−</SUB> <I> <SUB>x</SUB> </I>Ni<SUB>1/3</SUB>Co<SUB>1/3</SUB>Mn<SUB>1/3</SUB>O<SUB>2</SUB> (NCM) paired with silver (Ag) is introduced as a new electrochemical system for Li<SUP>+</SUP> recovery from brine. NCM is characterized by its high Li<SUP>+</SUP> selectivity and stability in aqueous environment. At an applied current in brine, NCM was able to intercalate Li<SUP>+</SUP> into its lattice while the Ag captured the Cl<SUP>−</SUP> counter-ion. Reversal of the current in a receiving solution prompted the release of LiCl. Under optimal conditions (<I>i</I> = ±0.25 mA cm<SUP>−2</SUP>), NCM can produce 96.4% pure Li<SUP>+</SUP> from brine by expending 2.60 W·h mol<SUP>−1</SUP> Li<SUP>+</SUP>. The NCM/Ag was able to perform consistently and produce an enriched LiCl solution in cycled operations. These promising results indicate that NCM/Ag can be developed as a high-throughput Li<SUP>+</SUP> mining process with low energy requirement.</P> <P><B>Highlights</B></P> <P> <UL> <LI> Li<SUB>1−</SUB> <I> <SUB>x</SUB> </I>Ni<SUB>1/3</SUB>Co<SUB>1/3</SUB>Mn<SUB>1/3</SUB>O<SUB>2</SUB> (NCM)/Ag electrochemically captured Li<SUP>+</SUP> from brine. </LI> <LI> At reverse applied current (<I>i</I>), NCM/Ag released LiCl in recovery solution. </LI> <LI> NCM/Ag energy consumption was minimized at varied <I>i</I>, time, and feed [Li<SUP>+</SUP>]. </LI> <LI> LNCM/Ag operation can be cycled to produce 96% Li<SUP>+</SUP> using 2.60 W·h mol<SUP>−1</SUP> Li<SUP>+</SUP>. </LI> <LI> LNCM/Ag can significantly reduce operation time for Li<SUP>+</SUP> mining from brines. </LI> </UL> </P>
( John Edward L. Sio ),( Grace M. Nisola ),( Rosemarie Ann I. Cuevas ),( Khino J. Parohinog ),( Hiluf T. Fissaha ),( Lawrence A. Limjuco ),( Seong-poong Lee ),( Wook-jin Chung ) 한국폐기물자원순환학회(구 한국폐기물학회) 2019 ISSE 초록집 Vol.2019 No.-
The continuous increase in the number of electronic wastes(e-waste) worldwide has caused awareness to salvage these materials as secondary sources of critical metals. Spent lithium-ion batteries (LIBs) in E-waste, used mobile phones and computers contain Li, Ni, Co, Al, and Mn.Cobalt is considered as a critical metal thatcan be recycled into other materials such as magnets, alloys, electroplating, andin LIB and printed circuit boards (PCBs). Thus, selective Co(II) extraction and recovery from secondary sources is of great importance.Schiff base ligands have so far been used as extractants in liquid-liquid extraction (LLE) for Co(II) recovery. Some examples of Schiff bases are synthesized via condensation of 2-aminothiazoles with substituted benzaldehydes. Synthesis of the ligand for Co(II) adsorption is relatively cheap and convenient. However, Schiff bases are susceptible to acid hydrolysis, especially during desorption of Co(II). Thus, slight modification of the imine group to amine by mild reduction was required to render the ligand acid-resistant while it retains its complexing ability with Co(II). Two starting materials for the synthesis of the Schiff base ligand were prepared, 4-allyloxy-2-hydroxybenzaldehyde (AHB) and 2-amino-4-methylthiazole (ATZ). Condensation reaction between AHB and ATZ was carried out to form the Schiff base product (AHB-ATZ), which was further reduced by NaBH4 (r-AHB-ATZ). All synthetic compounds were confirmed via infrared spectroscopy (FTIR), proton and carbon nuclear magnetic resonance spectroscopy (1H-NMR and <sup>13</sup>C-NMR). While LLE is the conventional system of application, a more practical approach to minimize reagent use and simplify the process is to incorporate r-AHB-ATZ in ion-imprinted polymers (IIPs). IIPs have recently attracted considerable attention in the recovery of metal ions including Co(II). Integration of IIPs with magnetic particles provides the recyclability and reusability of the extracting material after selective adsorption and desorption of Co(II).For the material support, bare magnetite (Fe<sub>3</sub>O<sub>4</sub>) was prepared by co-precipitation method of FeCl<sub>3</sub>/FeCl<sub>2</sub> (2/1) under basic conditions. Its surface was modified with silica by tetraethylorthosilicate(Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>) and alkene by 3- methacryloyloxypropyltrimethoxysilane (Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>-MATES). Then, radical polymerization between the Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>-MATES and r-AHB-ATZ was carried out using azobisisobutyronitrile (AIBN) as radical initiator and ethylene glycol dimethacrylate(EGDMA) as cross-linker in the presence and absence of Co(II) to produce Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>-MATES-IIP and non-ion-imprinted material (Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>-MATES-NIP), espectively.Fe<sub>3</sub>O<sub>4</sub> and its functionalization were characterized by FTIR. Further material characterization and adsorption tests for the selective extraction and recovery of Co(II)are on-going.This work was supported by National Research Foundation of Korea (NRF) funded by the Ministry of Science and ICT (2017R1D1A1B03028102 and 2017R1A2B2002109) and Ministry of Education (2009-0093816 and 22A20130012051 (BK21Plus)).
Chosel P. Lawagon,Grace M. Nisola,Rosemarie Ann I. Cuevas,김헌,이성풍,정욱진 한국공업화학회 2019 Journal of Industrial and Engineering Chemistry Vol.70 No.-
Various polymers were systematically screened as matrices for H2TiO3 Li+ adsorbent. H2TiO3/polymerswere electrospun as nanofibers (NF), characterized, and evaluated via response surface methodologywith central composite design for Li+ adsorption experiments. Polyacrylonitrile (PAN) was determined asthe most suitable H2TiO3 support. H2TiO3/PAN hydrophilicity and its favorable NF structure providedsufficient feed interaction. The Li+ adsorption was Langmuir-type with maximum capacity = 72.75 mg g 1and adsorption rate = 1.89 10 4 g mg 1 min 1. H2TiO3/PAN is Li+-selective, with a thermodynamicallyfavorable adsorption. Stable performance and durability during cycled adsorption/desorption runs proveH2TiO3/PAN NF as highly effective composite Li+ adsorbent.
Lawagon, Chosel P.,Nisola, Grace M.,Cuevas, Rosemarie Ann I.,Kim, Hern,Lee, Seong-Poong,Chung, Wook-Jin THE KOREAN SOCIETY OF INDUSTRIAL AND ENGINEERING 2019 JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY -S Vol.70 No.-
<P><B>Abstract</B></P> <P>Various polymers were systematically screened as matrices for H<SUB>2</SUB>TiO<SUB>3</SUB> Li<SUP>+</SUP> adsorbent. H<SUB>2</SUB>TiO<SUB>3</SUB>/polymers were electrospun as nanofibers (NF), characterized, and evaluated via response surface methodology with central composite design for Li<SUP>+</SUP> adsorption experiments. Polyacrylonitrile (PAN) was determined as the most suitable H<SUB>2</SUB>TiO<SUB>3</SUB> support. H<SUB>2</SUB>TiO<SUB>3</SUB>/PAN hydrophilicity and its favorable NF structure provided sufficient feed interaction. The Li<SUP>+</SUP> adsorption was Langmuir-type with maximum capacity=72.75mgg<SUP>−1</SUP> and adsorption rate=1.89×10<SUP>−4</SUP> gmg<SUP>−1</SUP> min<SUP>−1</SUP>. H<SUB>2</SUB>TiO<SUB>3</SUB>/PAN is Li<SUP>+</SUP>-selective, with a thermodynamically favorable adsorption. Stable performance and durability during cycled adsorption/desorption runs prove H<SUB>2</SUB>TiO<SUB>3</SUB>/PAN NF as highly effective composite Li<SUP>+</SUP> adsorbent.</P> <P><B>Highlights</B></P> <P> <UL> <LI> LIS HTO in various polymeric supports were electrospun as nanofibers (NFs). </LI> <LI> Hydrophilic polyacrylonitrile (PAN) as NF is the most suitable HTO matrix. </LI> <LI> HTO/PAN NF has minimal losses in Li<SUP>+</SUP> adsorption capacity (<I>q</I>) and kinetics. </LI> <LI> HTO/PAN NF has excellent Li selectivity, it achieved maximum <I>q<SUB>m</SUB> </I> =72.75mgg<SUP>−1</SUP>. </LI> <LI> HTO/PAN NF is durable, recyclable, and suitable for various aqueous Li<SUP>+</SUP> sources. </LI> </UL> </P> <P><B>Graphical abstract</B></P> <P>[DISPLAY OMISSION]</P>