aaronkrieg1
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MNT prep - strange result
So I was nitrating some Toluene yesterday and had a strange thing happen. Don't ask how but the nitrating bath was contaminated with a very small
amount of candle wax. I was pissed, but went through with the nitration anyway.
Not long before I could tell something was off, the aqueous acid layer was a dark coffee colored liquid. I kept going anyways, some out of curiosity,
some out of desperation. But it seemed that the Toluene was still on schedule. By the end of the nitration I got an opaque-pumpkin color Organic layer
and a very dark brown coffee colored aqueous acid layer.
I washed it out and now it looks like a bright orange juice. It smells similar to how it should, but last time I did this, I don't think it was quite
that color. (See exhibit A)
The mixture was allowed to seperate at a cool temperature, and when retrieved, contents were solidifying. The brown layer was syruppy and the orange
layer had even developed a little slush. Ugh, what a mess.
So any ideas on what happened? Do you think there may be some salvageable Nitrotoluene in there, if so, any thoughts on extraction methods? Do you
think it would be effective (or safe) to run it through a simple distillation. It took a long time to prep this so I'm grabbing strings here before I
start over
[Edited on 10-11-2013 by aaronkrieg1]
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Ral123
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Wellcome to the world of nitroaromatics.
The dark brown can be a sign of unreacted toluene. The solids can be higher nitrates. Did you stirr well? If you try TNP, it may be quite a bit less
messy.
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aaronkrieg1
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The nitrating bath was added dropwise, so I could see the dark brown forming early in the nitration. I thought I did alright on a consistent stir, but
i didn't have help this time, so it was a little tougher. TNP huh? Interesting. Maybe my next encounter, but I never like to leave a project
unfinished.
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plante1999
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Making nitobenzene by nitrating toluene, I may have missed something here.
I never asked for this.
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aaronkrieg1
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Whoops, my mistake, I've corrected it
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