Sciencemadness Discussion Board

TNT without Oleum

Turner - 2-6-2014 at 19:28

So back in January, I supposedly synthesized TNT. However I am thinking that my TNT was in fact highly contaminated with DNT because of the lack of SO3 in the nitration mix (100+% sulfuric acid). I ran a nitration of DNT with anhydrous nitric acid and excess 95% sulfuric acid at the maximum temperature before oxidation occurred (NO2 fumes) which was around 115C.

Here is the reaction beaker after it has cooled down to around 70C as you can kind of see in the thermometer, a quick note, I am wondering if the top layer is un-nitrated DNT?:



After cooling to around 30C, note the long crystals formed under the now solid mass of DNT?:



This lime green color went away and turned more brownish/orange after underwater molten neutralization with sodium bicarb, here is a 15g sample, I tested the melting point underwater to be 50C which would indicate this is in fact DNT/TNT perhaps 50/50 mix? you can kind of see a crystalline appearance




So, is the final nitration set-up an equilibrium reaction? The stronger sulfuric acid (SO3) pushes the reaction to the right, my question is if it's possible to attain a reasonable amount of pure TNT without oleum

DNT + HNO3/H2SO4 <-----> TNT

VladimirLem - 3-6-2014 at 08:33

Quote:

my question is if it's possible to attain a reasonable amount of pure TNT without oleum


yes, of course...

there are many 3 step-nitration synthesis texts on the internet...(but havent tried them yet)

some even with no using of high concentrated HNO3 +(95<%)H2SO4....just around (30-65% HNO3) as far as i know...sure, the yields are not that good, but it works...

what do you want with many amounts of TNT...afaik its "wasting" chems...ETN/PETN and so on are much more "effective" at the ratio of chems to final-product


Bert - 3-6-2014 at 16:53

Not sure if this is of practical use to you, but here it is-

https://www.sciencemadness.org/whisper/viewthread.php?tid=24...