tom haggen
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Emergency Please Help
Well I made it all the way through a picric acid synthesis. Using the KNO3 method, I added it slow, and had some nitric acid vapors coming off durning
the addition. Well as I was letting the reaction subside and cool to room temperature, The reaction cooled to about 30C. I added some cold water to
precipitate out the picric acid. To my horror when I added the water, NO2 started billowing off of the reaction. I bolted and went and grabbed my gas
mask. When I came back the solution had turned from a dark red to a yellow color and the reaction put off some intense heat, I felt the side of the
flask. So is my intire synthesis ruined now? Also if it is how should I dispose of this misterious yellow goop that seems extremely dangerous. When I
went back out to check on it i stirred it a couple times and it put off more NO2. Any advice would be greatly appreciated. That was the first time I
have ever seen NO2 and it scared the shit out of me! I never read anywhere that the addition of water would cause such a violent reaction.
[Edited on 22-3-2004 by tom haggen]
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Nick F
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Personally, I cool the reaction in an ice bath first, then dump it into ice/water (reaction into ice/water, not vice-versa).
What may have happened to you is that the first bit of water hydrated the sulphuric in your nitrating mix, resulting in a large rise in temperature
which could have led to a runaway nitration of any unreacted acetylsalicylic acid (asssuming that's what you used?).
Don't chuck out the yellow stuff that you have - it'll be your TNP, byproducts, and probably lots of potassium sulphate. Recrystalise it,
and you'll have fairly pure TNP.
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tom haggen
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It must have been a runaway nitration of what acetylsalicylic acid hadn't been reacted yet. When I recrystalize should I use acetone? I've
read so many different people suggesting so many different solvents that i'm having a hard time choosing one. By the way had I cooled the
nitration mixture properly would I have reduced how much potassium sulfate was produced? Obviously I will cool the nitration mixture much colder next
time before I add the water to prevent a runaway nitration. Man I was having nitemares about my chemical experiments last night.
p.s. I always get that "pour acid into water rule" switched around.
[Edited on 22-3-2004 by tom haggen]
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tom haggen
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My final product is totally orange. does that mean that it is heavily contaminated with potassium sulfate?
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Nick F
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Potassium sulphate is colourless, so that won't be making it orange. It sounds like you have some oxidation products in there perhaps (NO2
release is a sign that something is being oxidised, or that it's got so hot that the HNO3 is decomposing, more likely something is being
oxidised).
"By the way had I cooled the nitration mixture properly would I have reduced how much potassium sulfate was produced?"
No, I'm afraid there's no way of avoiding potassium sulphate with this method.
Unfortunately this isn't a reaction that I perform very often, so I'm not sure if your orange stuff is useful or not. You could try another
recrystalisation... hopefully someone more familiar with making TNP will come and help...
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tom haggen
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I think next time I try this, when I add the water the picric acid precipitates and sinks to the bottom, and all of that goo shit floats to the top,
im going to skim off that goo crap. I'm not a fan of making this stuff. When I washed it I lost a considerable amount of my product. Since mono,
di, and trinitrophenol ard all water soluble all the methods of recrystallization I have read about seem really inefficient. Not to mention it is a
pain in the ass to dry. Anyway heres a pic of just how orange my product really is.
[Edited on 23-3-2004 by tom haggen]
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tom haggen
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sorry I had to post twice to get this pic uploaded. Whatever that orange shit is it seems like it has been nitrated because it burns almost like gun
powder or black powder. however it doesn't really burn that well unless you pick it up with something wooden like a toothpick and char the wood
while you burn it.
It evens smells somewhat like nitrocellulose when it burns. Is that a charactiristic of picric acid, or is this true to all things that have been
nitrated?
[Edited on 23-3-2004 by tom haggen]
[Edited on 24-3-2004 by tom haggen]
[Edited on 24-3-2004 by tom haggen]
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tom haggen
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Is it possible to detonate picric acid with a really strong blow from a hammer?
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Nick F
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Probably, yes.
If the phenolic stuff was oxidised to quinone (or whatever its called), and then that was nitrated, then that could probably give you some quite
sensitive stuff. It might account for the rapid burning you see.
What method did you use exactly? I might try to make some "orange stuff" myself and play around with it a bit...
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tom haggen
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i added the asa to the sulpuric acid and heated it at about 85-90C for 15min, then I slowly add KNO3, then I added it to water way before it was cold
enough and thats when I got the runaway nitration. when it was done there was a bunch of pure looking crystals on the bottom of the beaker and some
grose yellow sludge floating on the top. I almost skimed off the sludge, but I just filtered every thing. Added everything to some fresh water
refiltered and lost a lot of product. Thats about it. I haven't got it to detonate with a hammer yet but I don't think it's completely
dry yet.
[Edited on 24-3-2004 by tom haggen]
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