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离子液体中碲的低温活化及金碲和银碲的资源高效合成

Low Temperature Activation of Tellurium and Resource-Efficient Synthesis of AuTe and Ag Te in Ionic Liquids.

作者信息

Grasser Matthias A, Pietsch Tobias, Brunner Eike, Doert Thomas, Ruck Michael

机构信息

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.

出版信息

ChemistryOpen. 2021 Feb;10(2):117-124. doi: 10.1002/open.202000249. Epub 2020 Oct 19.

Abstract

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.

摘要

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。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/4602/7874243/a7cc499f1cb3/OPEN-10-117-g001.jpg

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