Speciation of chloroindate(III) ionic liquids

Speciation of chloroindate(III) ionic liquids
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DOI:
10.1039/c0dt00497a
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发表时间:
2010-01-01
影响因子:
4
通讯作者:
Villar-Garcia, Ignacio J.
Villar-Garcia, Ignacio J.
中科院分区:
化学2区
文献类型:
--
作者:
Apperley, David C.;Hardacre, Christopher;Villar-Garcia, Ignacio J.

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通过将1-烷基-3-甲基咪唑鎓氯化物与氯化铟(III)以各种比例混合来制备一系列氯铟酸盐(III)离子液体体系,所述比例表示为氯化铟(III)的摩尔分数X(InCl 3)。对于chi(InCl 3)0.50,产物是两相的(固体在离子液体中的悬浮液)。这些氯铟酸(III)系统的形态进行了使用广泛的技术:差示扫描量热法(DSC),偏光显微镜(POM),液态和固态在-115 NMR光谱,X射线光电子能谱(XPS)和扩展的X射线吸收精细结构(EXAFS)。使用过量的有机氯化物(chi(InCl 3)< 0.5)制备的离子液体含有[InCl 6](3-)、[InCl 5](2-)和[InCl 4](-)阴离子,其比例取决于chi(InCl 3)值。等摩尔混合物产生单一化合物:1-烷基-3-甲基咪唑鎓四氯茚(III)。含有过量氯化铟(III)(x(InCl 3)> 0.5)的系统含有悬浮在中性四氯碘酸盐离子液体中的氯化铟(III)粉末。
A range of chloroindate(III) ionic liquid systems was prepared by mixing of 1-alkyl-3-methylimidazolium chloride with indium(III) chloride in various ratios, expressed as the mol fraction of indium(III) chloride, chi(InCl3). For chi(InCl3) 0.50, the products were biphasic (suspensions of a solid in an ionic liquid). Speciation of these chloroindate(III) systems was carried out using a wide range of techniques: differential scanning calorimetry (DSC), polarised optical microscopy (POM), liquid-state and solid-state In-115 NMR spectroscopy, X-ray photoelectron spectroscopy (XPS) and extended X-ray absorption fine structure (EXAFS). Ionic liquids prepared using an excess of the organic chloride (chi(InCl3) < 0.5) contained [InCl6](3-), [InCl5](2-) and [InCl4](-) anions, in proportions dependent on the chi(InCl3) value. Equimolar mixtures yielded single compounds: 1-alkyl-3-methylimidazolium tetrachloroindates(III). Systems containing an excess of indium(III) chloride (chi(InCl3) > 0.5) contained indium(III) chloride powder suspended in a neutral tetrachloroindate ionic liquid.