急! 乙二胺提纯
请教各位高人 怎样才能将乙二胺除水提纯呢我很着急 求详细操作
谢谢各位了 金属钠回流2到3个小时后蒸馏 不能用金属钠吧，
乙二胺有四个活泼氢太危险了。 精留分离怎么样
回复 3# yushouyun 的帖子
从试剂手册上查到的！回复 5# myheric 的帖子
操作方法能不能再说详细一些啊尤其是一些温度等细节方面再详细些
谢谢
另外,还有没有别的方法呢? Ethylenediamine [107-15-31 M 60.1, f.p. l l . O o , b 117.0°, d 0.897, n 1.45677, n30 1.4513.
Forms a constant-boiling (b 118.5O) mixture with water (15%) [hygroscopic and miscible with water].
Recommended purification procedure [Asthana and Mukherjee in Coetzee, 1982 cf p 531: to 1L of
ethylenediamine was added 70g of type 5A Linde molecular sieves and shaken for 12h. The liquid was decanted
and shaken for a further 12h with a mixture of CaO (50g) and KOH (15g). The supernatant was fractionally
distd (at 20:l reflux ratio) in contact with freshly activated molecular sieves. The fraction distilling at 117.2O
/760mm was collected. Finally it was fractionally distilled from sodium metal. All distns and storage of
ethylenediamine should be carried out under nitrogen to prevent reaction with C02 and water. Material
containing 30% water was dried with solid NaOH (600g/L), heated on a water bath for 10h. Above 60°,
separation into two phases took place. The hot ethylenediamine layer was decanted off, refluxed with 40g of
sodium for 2h and distd [Putnam and Kobe Trans Electrochem Soc 74 609 19381. Ethylenediamine is usually
distd under nitrogen. Type 5A Linde molecular sieves (70g/L), then a mixture of 50g of CaO and 15g of
KOHL, with further dehydration of the supernatant with molecular sieves has also been used for drying this
diamine, followed by distn from molecular sieves and, finally, from sodium metal. A spectroscopically
improved material was obtained by shaking with freshly baked alumina (20gL) before distn.
挺详细的，学习了！
谢谢！:) 学习了,,不错:P回复 7# yushouyun 的帖子
非常感谢! 一般分析纯的我都是直接用金属钠精制的，当然像楼上说的先欲除水会更安全一些！页:
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