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Low Temperature Activation of Tellurium and Resource‐Efficient Synthesis of AuTe<sub>2</sub> and Ag<sub>2</sub>Te in Ionic Liquids

14

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29

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2020

Year

Abstract

The low temperature syntheses of AuTe<sub>2</sub> and Ag<sub>2</sub> Te starting from the elements were investigated in the ionic liquids (ILs) [BMIm]X and [P<sub>66614</sub> ]Z ([BMIm]<sup>+</sup> =1-butyl-3-methylimidazolium; X = Cl, [HSO<sub>4</sub> ]<sup>-</sup> , [P<sub>66614</sub> ]<sup>+</sup> = trihexyltetradecylphosphonium; Z = Cl<sup>-</sup> , Br<sup>-</sup> , dicyanamide [DCA]<sup>-</sup> , bis(trifluoromethylsulfonyl)imide [NTf<sub>2</sub> ]<sup>-</sup> , decanoate [dec]<sup>-</sup> , acetate [OAc]<sup>-</sup> , bis(2,4,4-trimethylpentyl)phosphinate [BTMP]<sup>-</sup> ). Powder X-ray diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy revealed that [P<sub>66614</sub> ]Cl is the most promising candidate for the single phase synthesis of AuTe<sub>2</sub> at 200 °C. Ag<sub>2</sub> Te was obtained using the same ILs by reducing the temperature in the flask to 60 °C. Even at room temperature, quantitative yield was achieved by using either 2 mol % of [P<sub>66614</sub> ]Cl in dichloromethane or a planetary ball mill. Diffusion experiments, <sup>31</sup> P and <sup>125</sup> Te-NMR, and mass spectroscopy revealed one of the reaction mechanisms at 60 °C. Catalytic amounts of alkylphosphanes in commercial [P<sub>66614</sub> ]Cl activate tellurium and form soluble phosphane tellurides, which react on the metal surface to solid telluride and the initial phosphane. In addition, a convenient method for the purification of [P<sub>66614</sub> ]Cl was developed.

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