节点文献
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
【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 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.
【Key words】 diethylaluminum azide (DEAA) synthesis melting point 27Al NMR;
- 【文献出处】 无机化学学报 ,Chinese Journal of Inorganic Chemistry , 编辑部邮箱 ,2001年03期
- 【分类号】O627
- 【被引频次】2
- 【下载频次】51