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Patent Granted PROBLEM TO BE SOLVED: To enable, in producing AlH<SB>3</SB>, the excessive used amount of LiAlH<SB>4</SB>contributing to the separation of diethyl ether to be decreased and the diethyl ether separation performance to be maintained favorably. ; SOLUTION: In diethyl ether, LiAlH<SB>4</SB>is reacted with AlCl<SB>3</SB>in a blending ratio of 3<(LiAlH<SB>4</SB>/AlCl<SB>3</SB>)<4 to synthesize AlH<SB>3</SB>, and then an AlH<SB>3</SB>-containing diethyl ether solvate prepared by the above reaction is heated at higher than 60[deg.]C and lower than 130[deg.]C under vacuum to separate off and recover AlH<SB>3</SB>.