| 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 |
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| 摘要: |
| 关键词: 叠氮二乙基铝(DEAA) 合成 熔点 27AlNMR谱 |
| 基金项目: 中国工程物理研究院基金资助(No.95050332). |
| Abstract: 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 DEAAby IR spectrum and 1H 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.27Al NMR of DEAA is determined.At δ = 6.4 there is a peak that W1/2 of the peak is 834Hz.The structure of crystal DEAA is inferred from 27Al NMR. |
| Keywords: diethylaluminum azide (DEAA) synthesis melting point 27Al NMR |
| 投稿时间：2000-12-12 修订日期：2001-02-06 |
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| 张小航,高占先.低熔点晶体叠氮二乙基铝的合成和证明[J].无机化学学报,2001,17(3):439-443. |
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