Grasser Matthias A, Pietsch Tobias, Brunner Eike, Doert Thomas, Ruck Michael
Faculty of Chemistry and Food Chemistry, Technische Universität Dresden, 01062, Dresden, Germany.
Max-Planck-Institut für Chemische Physik fester Stoffe, Nöthnitzer Str. 40, 01187, Dresden, Germany.
ChemistryOpen. 2021 Feb;10(2):117-124. doi: 10.1002/open.202000249. Epub 2020 Oct 19.
The low temperature syntheses of AuTe and Ag Te starting from the elements were investigated in the ionic liquids (ILs) [BMIm]X and [P ]Z ([BMIm] =1-butyl-3-methylimidazolium; X = Cl, [HSO ] , [P ] = trihexyltetradecylphosphonium; Z = Cl , Br , dicyanamide [DCA] , bis(trifluoromethylsulfonyl)imide [NTf ] , 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 [P ]Cl is the most promising candidate for the single phase synthesis of AuTe at 200 °C. Ag 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 ]Cl in dichloromethane or a planetary ball mill. Diffusion experiments, P and Te-NMR, and mass spectroscopy revealed one of the reaction mechanisms at 60 °C. Catalytic amounts of alkylphosphanes in commercial [P ]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 ]Cl was developed.
研究了从元素出发在离子液体（ILs）[BMIm]X和[P]Z（[BMIm] = 1 - 丁基 - 3 - 甲基咪唑鎓；X = Cl、[HSO]、[P] = 三己基十四烷基鏻；Z = Cl、Br、双氰胺[DCA]、双（三氟甲基磺酰）亚胺[NTf]、癸酸酯[dec]、乙酸酯[OAc]、双（2,4,4 - 三甲基戊基）次膦酸酯[BTMP]）中低温合成AuTe和Ag₂Te的情况。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]Cl是在200°C下单相合成AuTe最有前景的候选物。通过将烧瓶中的温度降至60°C，使用相同的离子液体获得了Ag₂Te。即使在室温下，通过在二氯甲烷中使用2 mol%的[P]Cl或行星式球磨机也能实现定量产率。扩散实验、³¹P和¹²⁵Te - NMR以及质谱揭示了60°C下的一种反应机制。商业[P]Cl中催化量的烷基膦激活碲并形成可溶性膦碲化物，其在金属表面反应生成固体碲化物和初始膦。此外，还开发了一种纯化[P]Cl的简便方法。
