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Low Temperature Activation of Tellurium and Resource‐Efficient Synthesis of AuTe2 and Ag2Te in Ionic Liquids
ChemistryOpen ( IF 2.3 ) Pub Date : 2020-10-19 , DOI: 10.1002/open.202000249
Matthias A Grasser 1 , Tobias Pietsch 1 , Eike Brunner 1 , Thomas Doert 1 , Michael Ruck 1, 2
Affiliation  

The low temperature syntheses of AuTe2 and Ag2Te starting from the elements were investigated in the ionic liquids (ILs) [BMIm]X and [P66614]Z ([BMIm]+=1‐butyl‐3‐methylimidazolium; X = Cl, [HSO4], [P66614]+ = trihexyltetradecylphosphonium; Z = Cl, Br, dicyanamide [DCA], bis(trifluoromethylsulfonyl)imide [NTf2], decanoate [dec], acetate [OAc], bis(2,4,4‐trimethylpentyl)phosphinate [BTMP]). Powder X‐ray diffraction, scanning electron microscopy, and energy‐dispersive X‐ray spectroscopy revealed that [P66614]Cl is the most promising candidate for the single phase synthesis of AuTe2 at 200 °C. Ag2Te 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 [P66614]Cl in dichloromethane or a planetary ball mill. Diffusion experiments, 31P and 125Te‐NMR, and mass spectroscopy revealed one of the reaction mechanisms at 60 °C. Catalytic amounts of alkylphosphanes in commercial [P66614]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 [P66614]Cl was developed.

中文翻译:

碲的低温活化和在离子液体中资源高效合成 AuTe2 和 Ag2Te

在离子液体 (ILs) [BMIm] X和[P 66614 ] Z ( [BMIm] + = 1-丁基-3-甲基咪唑; X  = Cl, [HSO 4 ] - , [P 66614 ] +  = 三己基十四烷基鏻; Z  = Cl - , Br - , 双氰胺 [DCA] - , 双(三氟甲基磺酰基)亚胺 [NTf 2 ] - , 癸酸酯 [dec] - , 醋酸盐 [OAc ] -, 双(2,4,4-三甲基戊基)次膦酸盐[BTMP] - )。粉末 X 射线衍射、扫描电子显微镜和能量色散 X 射线光谱表明,[P 66614 ]Cl 是在 200 °C 下单相合成 AuTe 2的最有希望的候选者。通过将烧瓶中的温度降低到 60 °C,使用相同的 IL 获得Ag 2 Te。即使在室温下,通过使用在二氯甲烷中的 2 mol % [P 66614 ]Cl 或行星式球磨机,也可以实现定量产率。扩散实验、31 P 和125 Te-NMR 和质谱揭示了 60 °C 时的反应机制之一。商业中烷基膦的催化量 [P66614 ]Cl 活化碲并形成可溶性碲化膦,其在金属表面反应生成固体碲化物和初始的膦。此外,还开发了一种方便的纯化 [P 66614 ]Cl 的方法。
更新日期:2020-10-19
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