The key is to let the temperatur not go to RT, it´s better to work at 5°C. After filtering it is better to neutralise the stuff and then
recrystallise,
for increased purity. If you do this, you can cool the filtered solution of ETN in EtOH down to like -20°C and filter the crystals.
These are much better to work with and very pure.
As a additional note, one should nitrate not less than 10g of E to ETN in my opinion. The loss from filtering and such is simply too high.
Your ratios are right.
My experiences with temperature: (same filtering methode and circumstances)
24g E + 85ml HNO3(53%) + 130ml H2SO4(96%) ==> 22g ETN after filtering and recrystallisation (3 hours reaction time (moderate cooling))
24g E + 85ml HNO3(53%) + 130ml H2SO4(96%) ==> 29g ETN after filtering and recrystallisation (6 hours reaction times (strong cooling))
[Edited on 6-4-2013 by Simbani] |