高纯α-AlH_3的合成及表征

Synthesis and Characterization of α-AlH_3 with High Purity

为制备高纯α-AlH3,将LiAlH4与AlCl3在乙醚溶液中反应,制备并分离出固体AlH3乙醚络合物,其在甲苯中90℃下脱醚2h可制得纯度为99.5%的α-AlH3,产率96.4%。对高纯α-AlH3进行了XRD、红外、元素分析、TG/DSC、SEM表征,同时考察了α-AlH3的结晶条件和稳定性。结果表明产品结晶性好、纯度高、性质稳定,合成方法具有操作简便、收率高、重现性好等优点。

In order to obtain α-A1Ha with high purity, solid A1H3-etherate was synthesized and separated from the re action of LiA1H4 and A1Cla in diethyl ether, then α-A1H3 with purity of 99. 5 % was prepared via desolvation of the solid A1H3-etherate in toluene at 90 ℃ for 2 hours in the yield of 96. 4 %. The product was characterized by XRD, IR, ele mental analysis, TG/DSC, SEM, meanwhile the crystallization and stability of α-A1Ha was also studied. The results in dicate that the product has good crystallization, high purity and stability, the synthetic method has the advantages of sim ple operation, high yield and good reproducibility.