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An Improved Method for the Synthesis of M2[B12H12] (M = Na, K) and Their Formation Mechanism
Inorganic Chemistry ( IF 4.3 ) Pub Date : 2024-07-16 , DOI: 10.1021/acs.inorgchem.4c00945 Hui Han 1 , Xin-Ran Liu 2 , Yan-Mei Gao 1 , Sha-Sha Liang 1 , Yi Jing 1 , Hai-Jun Li 1 , Xuenian Chen 1, 2
Inorganic Chemistry ( IF 4.3 ) Pub Date : 2024-07-16 , DOI: 10.1021/acs.inorgchem.4c00945 Hui Han 1 , Xin-Ran Liu 2 , Yan-Mei Gao 1 , Sha-Sha Liang 1 , Yi Jing 1 , Hai-Jun Li 1 , Xuenian Chen 1, 2
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Polyhedral boranes have potential applications in medicine and material science due to their unique structure and stability. However, tedious and low-yield synthetic methods limited their application. Herein, we have developed a facile large-scale synthetic method for M2[B12H12] (M = Na, K) by the reaction of MBH4 with N,N-dipropylaniline borane in diglyme at 120 or 140 °C in up to 88% yield. The mechanistic studies indicated that intermediates, such as [B3H8]− and [B9H14]−, were formed in the formation process of [B12H12]2– anion, similar to previously reported. The formation of B2H6 from the N,N-dipropylaniline borane adducts is most important. The developed method avoided using toxic materials, with high yield, easily scaled up, raw materials are readily available. Additionally, the starting material, N,N-dipropylaniline, could be repeatedly used at least three times with similar yields, which is an economical way to facilitate industrial synthesis. It is believed that this method will support further application of Na2[B12H12] and K2[B12H12] as solid electrolytes for an all-solid-state batteries.
中文翻译：
M2[B12H12](M=Na,K)的改进合成方法及其形成机制
多面体硼烷由于其独特的结构和稳定性在医学和材料科学中具有潜在的应用。然而，繁琐且低产的合成方法限制了它们的应用。在此，我们开发了一种简便的大规模合成方法，通过MBH 4与N , N-二丙基苯胺硼烷在二甘醇二甲醚中在120或140℃下反应来合成M 2 [B 12 H 12 ] (M = Na, K)。收率高达88%。机理研究表明，[B 3 H 8 ] -和[B 9 H 14 ] -等中间体是在[B 12 H 12 ] 2–阴离子的形成过程中形成的，与之前报道的类似。由N , N-二丙基苯胺硼烷加合物形成B 2 H 6是最重要的。该方法避免使用有毒原料，收率高，易于放大，原料易得。此外，起始原料N , N-二丙基苯胺可以重复使用至少3次，且产率相似，这是一种促进工业合成的经济方法。相信该方法将支持Na 2 [B 12 H 12 ]和K 2 [B 12 H 12 ]作为全固态电池固体电解质的进一步应用。
更新日期：2024-07-16
中文翻译：
M2[B12H12](M=Na,K)的改进合成方法及其形成机制
多面体硼烷由于其独特的结构和稳定性在医学和材料科学中具有潜在的应用。然而，繁琐且低产的合成方法限制了它们的应用。在此，我们开发了一种简便的大规模合成方法，通过MBH 4与N , N-二丙基苯胺硼烷在二甘醇二甲醚中在120或140℃下反应来合成M 2 [B 12 H 12 ] (M = Na, K)。收率高达88%。机理研究表明，[B 3 H 8 ] -和[B 9 H 14 ] -等中间体是在[B 12 H 12 ] 2–阴离子的形成过程中形成的，与之前报道的类似。由N , N-二丙基苯胺硼烷加合物形成B 2 H 6是最重要的。该方法避免使用有毒原料，收率高，易于放大，原料易得。此外，起始原料N , N-二丙基苯胺可以重复使用至少3次，且产率相似，这是一种促进工业合成的经济方法。相信该方法将支持Na 2 [B 12 H 12 ]和K 2 [B 12 H 12 ]作为全固态电池固体电解质的进一步应用。
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