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以Li H和Al Cl3为原料,且采用N,N-二甲基乙胺(DMEA)控制反应合成N,N-二甲基乙胺合氢化铝(DMEAA)。然后进行DMEAA与三乙胺(TEA)胺转换反应,得到三乙胺合氢化铝(TEAA);最后经过真空加热得到目标产物Al H3;同时用红外光谱(FT-IR)、粉末X-射线衍射(XRD)和热重分析(TG)对反应中间物及产物进行分析和表征。实验表明,该合成路线可行,以廉价的Li H代替Li ALH4有效降低Al H3的制备成本。
N, N-dimethylethylamine aluminum hydride (DMEAA) was synthesized by the reaction of LiH and AlCl3 with N, N-dimethylethylamine (DMEA). Then the amine conversion reaction of DMEAA and triethylamine (TEA) is carried out to obtain triethylamine aluminum hydride (TEAA); and finally the target product Al H3 is obtained by vacuum heating; and the product is characterized by infrared spectroscopy (FT-IR), powder X-ray diffraction (XRD) and thermogravimetric analysis (TG) were used to analyze and characterize the reaction intermediates and products. Experiments show that the synthetic route is feasible, and the cheap Li H instead of Li ALH4 can effectively reduce the preparation cost of Al H3.