A ratio of 1:5 is just plain nonsense IMHO. The procedure works well even with 53% HNO3, I used a ratio of 1:2 HNO3 to H2SO4 by volume when I had no
stronger acid available. The cellulose should be added at 0-5°C and the reaction time should not be longer than 3-4 hours, longer reaction time is
contraproductive. Wash well with water and then in Na2CO3 solution, if a acid-free product is wanted you can boil it in ammonia water for a few hours
because NH3 can more easily go into the nitrated cotton-fibers.
There will always be residual acid in your NC, recrystallizing is the only way to neutralise it completely. |