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Issue 5, 2010
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Synthesis and characterisation of ionic liquids based on 1-butyl-3-methylimidazolium chloride and MCl4, M = Hf and Zr

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Abstract

Dialkylimidazolium chlorometallate molten salts resulting from the combination of zirconium or hafnium tetrachloride and 1-butyl-3-methylimidazolium chloride, [C1C4Im][Cl], have been prepared with a molar fraction of MCl4, R = nMCl4/nMCl4 + n[C1C4IM][Cl] equal to 0, 0.1, 0.2, 0.33, 0.5, 0.67. The structure and composition were studied by Differential Scanning Calorimetry (DSC), 35Cl (263 to 333 K), 1H and 13C solid state and solution NMR spectroscopy, and electrospray ionisation (ESI) mass spectrometry. The primary anions of the MCl4-based ILs were [MCl5], [MCl6] and [M2Cl9], whose relative abundances varied with R. For R = 0.33, pure solid [C1C4Im]2[MCl6], for both M = Zr and Hf are formed (m.p. = 366 and 385 K, respectively). For R = 0.67 pure ionic liquids [C1C4Im][M2Cl9] for both M = Zr and Hf are formed (Tg = 224 and 220 K, respectively). The thermal dissociation has been attempted of [C1C4Im]2[HfCl6], and [C1C4Im]2[ZrCl6] monitored by 35Cl and 91Zr solid NMR (high temperature up to 551 K).

Graphical abstract: Synthesis and characterisation of ionic liquids based on 1-butyl-3-methylimidazolium chloride and MCl4, M = Hf and Zr

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Supplementary files

Article information


Submitted
15 Sep 2009
Accepted
26 Oct 2009
First published
01 Dec 2009

Dalton Trans., 2010,39, 1379-1388
Article type
Paper

Synthesis and characterisation of ionic liquids based on 1-butyl-3-methylimidazolium chloride and MCl4, M = Hf and Zr

P. S. Campbell, C. C. Santini, D. Bouchu, B. Fenet, L. Rycerz, Y. Chauvin, M. Gaune-Escard, C. Bessada and A. Rollet, Dalton Trans., 2010, 39, 1379
DOI: 10.1039/B919094E

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