| Autor: |
Wang J; Institute of Condensed Matter and Nanosciences, Université Catholique de Louvain, 1348Louvain-la-Neuve, Belgium., Steenhaut T; Institute of Condensed Matter and Nanosciences, Université Catholique de Louvain, 1348Louvain-la-Neuve, Belgium., Li HW; Hefei General Machinery Research Institute, Hefei230031, China., Filinchuk Y; Institute of Condensed Matter and Nanosciences, Université Catholique de Louvain, 1348Louvain-la-Neuve, Belgium. |
| Jazyk: |
angličtina |
| Zdroj: |
Inorganic chemistry [Inorg Chem] 2023 Feb 06; Vol. 62 (5), pp. 2153-2160. Date of Electronic Publication: 2023 Jan 24. |
| DOI: |
10.1021/acs.inorgchem.2c03810 |
| Abstrakt: |
Metal dodecaborates (M x B 12 H 12 ) are a versatile class of materials used in polymer chemistry and cancer treatment and are promising candidates as electrolytes for solid-state batteries. However, a general and scalable approach has not yet been developed for producing high-purity B 12 H 12 2- derivatives. In this work, we report a simple, efficient, and environmentally benign solvothermal method to prepare diffraction and 11 B NMR pure Na 2 B 12 H 12 (85% yield) and K 2 B 12 H 12 (84% yield). This new synthetic approach is based on the use of the borane dimethyl sulfide complex (DMS·BH 3 ) and borohydrides (NaBH 4 , KBH 4 ) heated at different temperatures in diglyme in an autoclave. It was found that high-purity Na 2 B 12 H 12 ·diglyme solvate is obtained via an intermediate formation of B 3 H 8 - , B 9 H 14 - , and B 11 H 14 - , which are all soluble in diglyme. Heating under vacuum is shown to be efficient for removing the coordinated diglyme, allowing the formation of unsolvated Na 2 B 12 H 12 . Autoclave synthesis starting from KBH 4 directly yields solvent-free K 2 B 12 H 12 , and ball-milling KBH 4 prior to the synthesis enabling us to significantly improve the final yield. The new synthetic method paves the way for large-scale synthesis of M x B 12 H 12 derivatives, enabling to envisage a wider scope of practical applications. |
| Databáze: |
MEDLINE |
| Externí odkaz: |
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