CAJ | 학술논문

研究了LiAlH4与AlCl3在无水乙醚中反应制得固体AlH3醚合物，再在惰性溶剂中加热脱醚制备α-AlH3的方法。考察了脱醚反应中添加LiBH4、温度与时间、溶剂和促结晶剂（聚二甲基硅氧烷）对产品的影响。试验结果表明，最佳工艺条件为试验以LiAlH4∶ AlCl3摩尔比为4∶1反应，减压蒸除乙醚制得固体AlH3醚合物；脱醚反应以甲苯为溶剂，固体AlH3醚合物与LiBH4摩尔比为4∶1，添加适量促结晶剂，在90℃下脱醚反应2 h。采用此工艺可制得结晶为立方体、性质稳定的α-AlH3，纯度为96．0％，收率达96．4％。
연구료LiAlH4여AlCl3재무수을미중반응제득고체AlH3미합물，재재타성용제중가열탈미제비α-AlH3적방법。고찰료탈미반응중첨가LiBH4、온도여시간、용제화촉결정제（취이갑기규양완）대산품적영향。시험결과표명，최가공예조건위시험이LiAlH4∶ AlCl3마이비위4∶1반응，감압증제을미제득고체AlH3미합물；탈미반응이갑분위용제，고체AlH3미합물여LiBH4마이비위4∶1，첨가괄량촉결정제，재90℃하탈미반응2 h。채용차공예가제득결정위립방체、성질은정적α-AlH3，순도위96．0％，수솔체96．4％。
α-AlH3 was synthesized in an inert solvent by desolvation of solid AlH3-etherate,which was obtained from the reac-tion of LiAlH4 and AlCl3 in ether.The effects of LiBH4 addition,temperature and time,solvent,crystallizing agent in desolvation on the product were discussed.The optimum process conditions were as follows:the molar ratio of LiAlH4 and AlCl3 was 4 ∶ 1,the solid AlH3-etherate was obtained by vacuum distillation;the desolvation was operated in toluene at 90 ℃ for 2 hours in the presence of crystallizing agent,the molar ratio of solid AlH3-etherate and LiBH4 was 4 ∶ 1. In this process,α-AlH3 with cubical crystallization and high stability was prepared in the purity of 96.0 % and yield of 96.4 %.