xonu
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Weird Styphnic Acid Behaviour
I keep running into a weird issue with making TNR, after sulphonating resorcinol, I get no exotherm on the addition of HNO3, instead it
tends to "dump" all of that heat after additions (which caused a nitration runaway on my first attempt) I managed to do the synthesis successfully
once without the runaway reaction, but I had the same no-exotherm problem on my latest attempt, which made me quench the reaction mix instead of
carrying on.
Am I "overcooling" the reaction mix or am I simply too fast with my additions? I'm following a scaled-down version of the Powerlabs prep for it and I
can post it here if needed.
Arylia Halide does not exist
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Tsjerk
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I don't know this specific reaction, but it sounds like overcooling indeed. The reaction needs some temperature to proceed and when it does get up to
speed, either because of a higher temperature or a higher concentration of nitric acid, there is already too much nitric available to keep the
temperature under control. I would raise the temperature until you do see the exotherm before adding more nitric.
[Edited on 1-11-2021 by Tsjerk]
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xonu
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Guessed so, I once started the addition outside the icebath and only started cooling when the exotherm started, and it worked out fine with no runaway
during the next step.
Arylia Halide does not exist
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caterpillar
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My first attempt to prepare TNR failed- I tried just like I did it with phenol. But resorcinol after contact with sulfur acid turned to stone. Later I
made TNR, using a two-stage process- nitrosation and then nitration with diluted nitric acid. No concentrated acids at all.
Women are more perilous sometimes, than any hi explosive.
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xonu
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Weird, mine forms a dark red thick goop that feels like a very viscous jam, it thins out on addition of HNO3
Arylia Halide does not exist
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caterpillar
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Quote: Originally posted by xonu  | | Weird, mine forms a dark red thick goop that feels like a very viscous jam, it thins out on addition of HNO3 |
Dark red, yeah, but solid. I threw it away. The method that I described here worked fine.
Women are more perilous sometimes, than any hi explosive.
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