低熔点晶体叠氮二乙基铝的合成和证明  

Synthesis and Proof of Diethylaluminum Azide being Lower Melting Point Crystal

作　　者：张小航[1] 高占先[1] 

机构地区：[1]大连理工大学化工学院,大连116012

出　　处：《无机化学学报》2001年第3期439-443,共5页Chinese Journal of Inorganic Chemistry

基　　金：中国工程物理研究院基金资助(No.95050332)。

摘　　要：Diethylaluminum azide (DEAA) is an important compound in organoaluminum andes. But the synthesis and property of DEAA were reported a little. The DEAA is a liquid compound in literature that was synthesed by the reaction of diethyl aluminum chloride (DEAC) and sodium azide. The solid product as a colorless crystal was first obtained by the reaction of DEAC and sodium azide in our work. The solid product was characterized as DEAA by IR spectrum and H NMR spectrum. The yield of crystal DEAA was increased as NaN3/DEAC (mol/mol) increased. When NaN3/DEAC = 1. 3 the yield of DEAA is increased from 74% in literature to 83%. The melting point of DEAA is 28 - 29℃ that was determined with two methods in the work. The DEAA containing trace DEAC (about 0. 2% of DEAC) is liquid which has been full proved by varied tests in this paper. The melting point of DEAA is - 130℃ in literature because the DEAA is not pure that may contain DEAC. The - 130℃ may be eutectic point of eutectic mixture forming of DEAA and DEAC. 27,Al NMR of DEAA is determined. At δ = 6. 4 there is a peak that 1/2 of the peak is 834Hz. The structure of crystal DEAA is inferred from 27Al NMR.Diethylaluminum azide (DEAA) is an important compound in organoaluminum azides. But the synthesis and property of DEAA were reported a littler The DEAA is a liquid compound in literature that was synthesed by the reaction of diethyl aluminum chloride (DEAC) and sodium azide, The solid product as a colorless crystal was first obtained by the reaction of DEAC and sodium azide in our work. The solid product was characterized as DEAA by IR spectrum and H-1 NMR spectrum. The yield of crystal DEAA was increased as NaN3/DEAC (mol/mol) increased. When NaN3/DEAC = 1.3 the yield of DEAA is increased from 74% in literature to 83%. The melting point of DEAA is 28 similar to 29 degreesC that was determined with two methods in the work. The DEAA containing trace DEAC (about 0. 2% of DEAC) is liquid which has been full proved by varied tests in this paper. The melting point of DEAA is - 130 degreesC in literature because the DEAA is not pure that may contain DEAC. The - 130 degreesC may be eutectic point of eutectic mixture forming of DEAA and DEAC. Al-27 NMR of DEAA is determined. At delta = 6. 4 there is a peak that W-1/2 Of the peak is 834Hz. The structure of crystal DEAA is inferred from Al-27 NMR.

关 键 词：叠氮二乙基铝 合成 熔点 核磁共振谱 铝工厂 

分 类 号：O627.31[理学—有机化学]