- Purification of Ethylenediamine
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Forms a constant-boiling (b 118.5 °C) mixture with water (15%) [hygroscopic and miscible with water]. Recommended purification procedure: to 1L of diamine (CAS NO. ) 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 20:1 reflux ratio) in contact with freshly activated molecular sieves. The fraction distilling at 117.2 °C/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 CO2 and water. Material containing 30% water was dried with solid NaOH (600g/L), heated on a water bath for 10h. Above 60 °C, separation into two phases took place. The hot ethylenediamine layer was decanted off, refluxed with 40g of sodium for 2h and distd. Ethylenediamine is usually distd under nitrogen.
Type 5A Linde molecular sieves (70g/L), then a mixture of 50g of CaO and 15g of KOH/L, 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 (20g/L) before distn.
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