Production Methods
A refrigerated pocket-shaped receiver is used to sublime an excess of N2O5 directly onto Cl2O in a high vacuum. The receiver containing the Cl2O (equivalent to 5 ml of liquid) is placed in liquid nitrogen so that only the portion holding the Cl2O is cooled, and the N2O5 thus deposits on the Cl2O as a solid. After releasing the vacuum, the receiver is removed from the high-vacuum apparatus, closed off using a drying tube, and placed in a refrigerating bath at —78°C. While the bath is slowly warmed to between —20 and 0°C (over 15 hours), the components react slowly. The ClNO3 thus formed is still contaminated with chlorine (an impurity of the Cl2O) and excess N2O5. To eliminate the chlorine, which is difficult to separate, the reaction product is heated to 30°C in a water bath and refluxed for one hour. The upper half of the reaction vessel (serving as a condenser) is cooled by a ring-shaped cup filled with Dry Ice. The chlorine is volatilized in this procedure, while the excess N2O5 is decomposed to NO2 and O2. The ClNO3 is then distilled at — 90°C in a high vacuum, leaving behind the NO2.
Cl
2O+N
2O
5=2ClNO
3
Hazard
Explosive reaction with metals, metal chlorides, alcohols, ethers, and most organic materials.
