三氢化铝乙醚配合物的稳定性及其固相转晶制备α-三氢化铝

doi:10.11944/j.issn.1000-0518.2019.09.190032

摘要/Abstract

摘要：

针对不同贮存时长三氢化铝醚合物能否转晶制备α-三氢化铝问题进行了深入研究。本文采用传统法制得三氢化铝醚合物并在氮气气氛下储存1~20 d,然后基于此三氢化铝醚合物,采用固相、真空转晶技术制备α-三氢化铝。 X射线衍射(XRD)、热重分析(TGA)和扫描电子显微镜(SEM)分析表明,随着醚合物贮存时间的延长,其乙醚成分逐渐降低,贮存10 d仍然可以制备出纯度较高的α-三氢化铝,然而10 d后,有γ-三氢化铝产生,而且产物粒径变小。证明醚合物中乙醚的含量多少与制备出的α-三氢化铝的品质有直接关联。制备过程摒弃有毒试剂甲苯,也为α-三氢化铝的千克级制备提供了一种可能。

关键词: 三氢化铝, 制备, 贮存

Abstract:

The problem of whether α-AlH₃ crystallized by aluminum hydride etherates(AlH₃·nEt₂O) stored for varying time is systematically studied. First, AlH₃·nEt₂O was prepared by a conventional method and stored under a nitrogen atmosphere for 1 to 20 days, and then α-AlH₃ was prepared by a solid phase and vacuum crystallizing technique based on the AlH₃·nEt₂O. XRD, TGA and SEM analysis show that the ether composition gradually decreases during storage and α-AlH₃ with higher purity can be prepared within 10 days of storage. However, after 10 days, γ-AlH₃ with smaller particle size appeared. Finally, we confirm that the amount of ether in AlH₃·nEt₂O is directly related to the quality of prepared α-AlH₃. Another highlight of this paper is the abandonment of the toxic reagent toluene used in conventional processes. This also provides a possibility for the kilogram preparation of α-AlH₃.

Key words: aluminum hydride, preparation, storage

朱朝阳, 姜艾锋, 夏德斌, 王平, 林凯峰, 樊继壮, 范瑞清, 杨玉林. 三氢化铝乙醚配合物的稳定性及其固相转晶制备α-三氢化铝[J]. 应用化学, 2019, 36(9): 1069-1075.

ZHU Zhaoyang, JIANG Aifeng, XIA Debin, WANG Ping, LIN Kaifeng, FAN Jizhuang, FAN Ruiqing, YANG Yulin. Stability of Aluminum Hydride Etherates and Its Solid-State Conversion to Alpha-Aluminum Hydride[J]. Chinese Journal of Applied Chemistry, 2019, 36(9): 1069-1075.

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