Synthesis of Anhydrous Acetates for the Components of Nuclear Fuel Recycling in Dialkylimidazolium Acetate Ionic Liquids [plus supplemental information]

Smetana, Volodymyr; Kelley, Steven P.; Titi, Hatem M.; Hou, Xiaomin; Tang, Si-Fu; Mudring, Anja-Verena; Rogers, Robin D.

doi:10.1021/acs.inorgchem.9b03077

Title: Synthesis of Anhydrous Acetates for the Components of Nuclear Fuel Recycling in Dialkylimidazolium Acetate Ionic Liquids [plus supplemental information]

Journal Article · 16 December 2019 · Inorganic Chemistry

DOI: https://doi.org/10.1021/acs.inorgchem.9b03077 · OSTI ID:1592765

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Stockholm Univ. (Sweden)
Univ. of Alabama, Tuscaloosa, AL (United States)
McGill Univ., Montreal, QC (Canada)
Qingdao Agricultural Univ. (China)
Stockholm Univ. (Sweden); Univ. of Alabama, Tuscaloosa, AL (United States); McGill Univ., Montreal, QC (Canada)

A series of anhydrous acetate salts with uranium {[C₂C₁im][UO₂(OAc)₃] (1), [C₂C₂im][UO₂(OAc)₃] (2), and [C₄C₁im][UO₂(OAc)₃] (3)}, lanthanides {[C₂C₂im]₂[La(OAc)₅] (4) and [C₂C₁im]₂[Nd(OAc)₅] (5)}, and strontium {[C₂C₁im]_n[Sr- (OAc)₃]_n (6)} (where C₂C₁im = 1-ethyl-3-methylimidazolium, C₂C₂im = 1,3-diethylimidazolium, C₄C₁im = 1-butyl-3-methylimi-dazolium, and OAc = acetate) have been prepared and structurally characterized. Both lanthanides and strontium are common components of the nuclear fuel waste, and their separation from uranium is an important but still challenging task. A new synthetic method with dialkylimidazolium acetate ionic liquids (ILs) as the solvent has been developed for the direct synthesis of homoleptic acetates from the corresponding hydrates and, unexpectedly, hardly soluble f-element oxides. Although the group of characterized compounds shows perfect structural variability, all actinide and lanthanide metal ions form monomeric complex anions where the metal cation coordinates to five ligands including two oxygen atoms in the case of uranium, as is commonly observed for uranyl compounds. Crystallographic analyses revealed that the complex [UO₂(OAc)₃]^- anions possess rather standard D_3h symmetry featuring a hexagonal-bipyramidal coordination environment, while the lanthanide anions [Ln(OAc)₅]^2- are fully asymmetric and the Ln³⁺ cations are 10-coordinated in the form of a distorted bicapped tetragonal antiprism. This is the first report of lanthanide ions coordinated in this fashion. For Sr²⁺, 9-fold coordination through oxygen atoms in the form of a strongly distorted tricapped trigonal prism is observed. Furthermore, the crystallization of anhydrous, homoleptic, anionic acetate complexes from such a large variety of different metal salts appears to be due to the properties of dialkylimidazolium acetate ILs themselves, including enhanced basicity from the high concentration of free anions and their greater affinity for hydrogen-bonding solutes relative to metal cations.

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Research Organization:: Univ. of Alabama, Tuscaloosa, AL (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES); Swedish Research Council (SRC)

Grant/Contract Number:: SC0019220

OSTI ID:: 1592765

Journal Information:: Inorganic Chemistry, Vol. 59, Issue 1; ISSN 0020-1669

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 10 works

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CCDC 1920431: Experimental Crystal Structure Determination Volodymyr, Smetana,; P., Kelley, Steven; M., Titi, Hatem https://doi.org/10.5517/ccdc.csd.cc22gcdb The current record is supplemented by this dataset	dataset	January 2020
CCDC 1952442: Experimental Crystal Structure Determination Volodymyr, Smetana,; P., Kelley, Steven; M., Titi, Hatem https://doi.org/10.5517/ccdc.csd.cc23jp0c The current record is supplemented by this dataset	dataset	January 2020
CCDC 1952443: Experimental Crystal Structure Determination Volodymyr, Smetana,; P., Kelley, Steven; M., Titi, Hatem https://doi.org/10.5517/ccdc.csd.cc23jp1d The current record is supplemented by this dataset	dataset	January 2020
CCDC 1952444: Experimental Crystal Structure Determination Volodymyr, Smetana,; P., Kelley, Steven; M., Titi, Hatem https://doi.org/10.5517/ccdc.csd.cc23jp2f The current record is supplemented by this dataset	dataset	January 2020
CCDC 1952445: Experimental Crystal Structure Determination Volodymyr, Smetana,; P., Kelley, Steven; M., Titi, Hatem https://doi.org/10.5517/ccdc.csd.cc23jp3g The current record is supplemented by this dataset	dataset	January 2020