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ManyInterests
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I can make some. I usually aim for WFNA or RFNA, but that can be diluted down to 70% easily.
Edit: On a dumb note. I am doing a synth with Dugan Boomfax's reagents and method... and I feel quite silly that I didn't review the video and I let
it reflux at 82C instead of 92C. Nothing that a little more time can handle.
Also for my 2nd synth, due to time constraints and fatigue, when I added the toluene I couldn't do the heating step, so I had an MNT layer form on top
for two days before I started heating today. While I did break it up, I still see a visible layer despite decent stirring from the stirbar in my
mantle. It'll be exciting to see what happens next.
Edit2: I think the heating was what caused the problem with a lot of the yield in my first synth. I was using a hotplate stirrer since my new mantle
didn't arrive yet. Again, it will be interesting to see what will happen on my third synth when I do it all in one go instead of having a multi-day
wait.
[Edited on 23-7-2025 by ManyInterests]
[Edited on 23-7-2025 by ManyInterests]
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Radiums Lab
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I recommend you to dilute your fuming HNO3 for for first two nitrations and then use fuming HNO3.
Reasons:
- Fuming nitric acid decomposes easily and you are practically wasting your HNO3 where you could just add some water and save it instead using excess
of it.
- There is a high chance of runaway with fuming one.
- You will be exposed to lesser NO2.
Why use HNO3 instead of NH4NO3+H2SO4?
Reason:
-If you are using TNT for just testing then it's fine. If you want to actually see how pure TNT works and clean up is not done properly, the spare
ammonium nitrate messes up the VOD and other parameters.
So for the next run I suggest you to synthesize the HNO3 seperately.
Water is dangerous if you don't know how to handle it, elemental fluorine (F₂) on the other hand is pretty tame if you know what you are doing.
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ManyInterests
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Quote: Originally posted by Radiums Lab  | I recommend you to dilute your fuming HNO3 for for first two nitrations and then use fuming HNO3.
Reasons:
- Fuming nitric acid decomposes easily and you are practically wasting your HNO3 where you could just add some water and save it instead using excess
of it.
- There is a high chance of runaway with fuming one.
- You will be exposed to lesser NO2.
Why use HNO3 instead of NH4NO3+H2SO4?
Reason:
-If you are using TNT for just testing then it's fine. If you want to actually see how pure TNT works and clean up is not done properly, the spare
ammonium nitrate messes up the VOD and other parameters.
So for the next run I suggest you to synthesize the HNO3 seperately.
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Thanks, I will look into the earlier posts on this thread to see the proportions. Before I dilute the acid, I will bubble dry air through it to purge
of NO2. The NO2 caused runaways in my RDX and destroyed everything, and I wasted a LOT (and I mean a LOT) of HNO3 that way.
BTw, I am looking at the flask I have now (I let it cool down in the flask) I still see the layer on top... I'm not sure what is going on. I wonder if
I failed entirely or what? I will take a photo of it in a bit before decanting.
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ManyInterests
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OK... so I filtered out my crude yield, and so far it is clogged in my separatory funnel. Nothing hot water can't handle... but I have something a
little more urgent to ask about. As I diluted the waste acid and began neutralizing, I saw some yellow (and later brown and red) substance start to
float on top of the water. It doesn't seem to be water soluble so I don't want it to clog up my pipes. Is this stuff crude TNT? I did hear that if TNT
mixed with waste water was neutralized with sodium bicarbonate, it forms brown TNT which is more sensitive to detonation on heating (around 120C or
so). Is this stuff it? How do I neutralize it safely if it is? If it isn't... then what is it exactly and how do I safely get rid of it?
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Radiums Lab
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U tried methanol wash?
Water is dangerous if you don't know how to handle it, elemental fluorine (F₂) on the other hand is pretty tame if you know what you are doing.
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ManyInterests
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I feel like a dumbass... but no. So while I scooped out a decent amount of the stuff (well not as much looking back) as I put in more bicarbonate
solution, it turned more red and a lot of it just dissolved. I have a little bit left and it is in the trash... and I kinda don't wanna take it out
(it isn't that much) the rest fully dissolved and is gone now. I rinsed and washed out my sink to make sure it is fully sanitized.
Meanwhile I did wash out the TNT that was in my separatory funnel was washed out and is currently being washed of residual acid. Unlike my first
attempt, this one looks like it is much, much better than my first attempt. I think I have basically succeeded in the basic synthesis using this
method. Now all what will be necessary to do is give it a sulfite and acid wash before fully purifying with boiling hot methanol.
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Radiums Lab
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For this run did you do 3 step process?
Water is dangerous if you don't know how to handle it, elemental fluorine (F₂) on the other hand is pretty tame if you know what you are doing.
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ManyInterests
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No, everything was done via the 1 step process and with ammonium nitrate. I might (read might) do a 3 step process sometime down the line... but for
now I am done synthesizing TNT. I made a few batches and am purifying them.
And I need to bring this up:
| Quote: | | I got another cleaning question. I just read DennyDevHE77 post about compressing it in layers of newspaper (newsprint paper is available any art
supply store) if that is actually sufficient to purify the stuff without much more washing that would quite fascinating. |
So this isn't wrong... at all. When I made the first couple of batches, I broke up the chunk into smaller pieces and put it on paper towels. the paper
towels absorbed red fluid or some red substance, and the chunks became less and less red with every change of the paper towels. Towards the end when
they were dried up (they were still staining the paper towels, but giving it a yellowish tint and not reddish. There was some red on some of the TNT
chunks, and I decided to separate those from the ones that were purely yellow.
I gave them a sodium metabisulfite wash separately, and the ones with no red produced no red water, and I need to mention that there was no NO2 stench
from the water (which is choking and I hate it). The ones that did have some redness DID have red water and smell produced. But due to draining it via
the paper towels, 2 small washes was all what was needed to fully get rid of the red water (only yellow water was produced, which is produced anyway
if you wash TNT with water).
Now... there was another batch I made, and unlike the others, I didn't break up the chunk or do a paper towel change... and right now I am still
washing it with sodium metabisulfite! Good thing I bought a good supply of that, otherwise I would be in a mild pickle.
So yes, using lots of paper towels can work towards purifying the TNT, and it is better than making red water. The paper towels can be put in a
plastic trashbag and taken away to be burned later, red water is bit trickier to deal with.
[Edited on 26-8-2025 by ManyInterests]
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ManyInterests
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OK, I return asking for a little help, since I am not sure if all my efforts have gone to waste.
So after performing my synths, all done with ammonium nitrate and using the 1-pot method. I washed out the crude TNT to remove residual acids,
followed by the sodium metabisulfite and dilute sulfuric acid washes (I gave it as many metabisulfite washes as it needed until all red water was
gone) and after drying it, I recrystalized it with hot ethanol (using 2ml of 95% ethanol per 1g of TNT). The 2nd 'bad' batch I made needed a hell of a
lot more washes and recrystalization to get the yellow crystals out. The first batch did not.
After all this, I was left with very fine pale yellow crystals, it looked like pure TNT. After drying everything I wanted to give it a melting point
test, but either I am not doing the test correctly or my TNT is very impure or it is not TNT (and either DNT or still MNT...) The melting point
appears to be around 72C. I did this by heating up a beaker of water and putting 1g of TNT in a cheap test tube (I got it from the arts and crafts
section of a dollar store. I am not sure if it is actual borosilicate glass) and waiting for the water to heat up. I heated the water fairly quickly.
I did a few such tests, once on my hotplate, and another on my mantle. Both had much lower melting points than expected.
Is it TNT? Or was it not nitrated enough and my batches need a 2nd nitration? Or am I just not doing the tests properly. I am confused and need help.
I asked duck.ai's chatbots for help, but I really, REALLY don't trust LLMs for chemistry work, since they said so many things that I know are bullshit
that I swear they're going to get someone killed some day.
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davidfetter
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| Quote: Originally posted by ManyInterests | | I asked duck.ai's chatbots for help, but I really, REALLY don't trust LLMs for chemistry work, since they said so many things that I know are bullshit
that I swear they're going to get someone killed some day. |
Statistically speaking, it's certain that they have already done so. Too many Bernouilli coins have already flipped to avoid this.
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greenlight
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I had a similar issue to you years ago. Tried a three step process and did not use fuming nitric or oleum for the last step. I instead used 70%
nitric, 98% sulphuric acid, and higher temperature. I believe that last nitro group really requires harsh conditions to push it on to highly
deactivated ring.
I too ended up with what looked very much like TNT after many washings, but the melting point temperature was off, and similar to yours from memory.
Upon detonation, you could tell that the full power was not there.
It is hard to accurately perform the melting point test due to the thermal transfer through the glass between the heat source (water) and the material
being tested (T?NT). I have a thermometer pocket for my still head which registers water boiling at 94°C for quite a delay. I would heat the water
bath alot slower especially when nearing the expected temperature range to allow time for the glass to thermally equilibrate with the bath
temperature. When using an actual melting point apparatus, the heating rate is slowed down in a similar fashion when approaching the expected melting
range for higher accuracy.
The temperature you report (72°C) seems within the range (and only slightly higher) for the melting point of dinitrotoluene.
As stated earlier, that last nitro group is the hardest to get on. Benzene is even worse to nitrate fully. If it werent for the severe bullying
required to synthesise it, its higher VOD qnd power would have made it the favourite and ACDC would have been singing TNB .
Im getting off topic and rambling, but the main point is to fully nitrate that extremely deactivated ring, high concentration acids and high
temperatures are required.
You could do the last step of the three step nitration with fuming nitric acid and concentrated sulfuric acid or oleum (if you have it) and some
temperature and that should complete the nitration.
I have heard of a method involving production of the MNT and then to DNT in one go, before using high concentration acids for the TNT step.
[Edited on 12-9-2025 by greenlight]
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ManyInterests
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| Quote: Originally posted by greenlight | I had a similar issue to you years ago. Tried a three step process and did not use fuming nitric or oleum for the last step. I instead used 70%
nitric, 98% sulphuric acid, and higher temperature. I believe that last nitro group really requires harsh conditions to push it on to highly
deactivated ring.
I too ended up with what looked very much like TNT after many washings, but the melting point temperature was off, and similar to yours from memory.
Upon detonation, you could tell that the full power was not there.
It is hard to accurately perform the melting point test due to the thermal transfer through the glass between the heat source (water) and the material
being tested (T?NT). I have a thermometer pocket for my still head which registers water boiling at 94°C for quite a delay. I would heat the water
bath alot slower especially when nearing the expected temperature range to allow time for the glass to thermally equilibrate with the bath
temperature. When using an actual melting point apparatus, the heating rate is slowed down in a similar fashion when approaching the expected melting
range for higher accuracy.
The temperature you report (72°C) seems within the range (and only slightly higher) for the melting point of dinitrotoluene.
As stated earlier, that last nitro group is the hardest to get on. Benzene is even worse to nitrate fully. If it werent for the severe bullying
required to synthesise it, its higher VOD qnd power would have made it the favourite and ACDC would have been singing TNB.
Im getting off topic and rambling, but the main point is to fully nitrate that extremely deactivated ring, high concentration acids and high
temperatures are required.
You could do the last step of the three step nitration with fuming nitric acid and concentrated sulfuric acid or oleum (if you have it) and some
temperature and that should complete the nitration.
I have heard of a method involving production of the MNT and then to DNT in one go, before using high concentration acids for the TNT step.
[Edited on 12-9-2025 by greenlight] |
I did think about giving it another nitration and making that nitration 125C or so for several hours. I asked duck.ai a question about that and it
told me that I had MNT (which I seriously doubt). I will post what it told me later, but I have one critical question: What about stirring?
I used a stirbar in my 2000ml flask, when the solution was thick and cold, it had a hard time working, but once the solution heated it, I got some
stirring going and I saw a bit of a whirlpool and some stuff moving around... BUT there was something important.
The layer at the top didn't mix with everything. When I first added the toluene the stirbar, even when working very hard, didn't seem to mix
everything very well, so what I had to do was pick up the flask myself and give it some swirls by hand (the solution turned red as I did so and the
temperature spiked before settling down). I am sure this is not the proper way to do it, but the typical method of adding toluene to the nitrating
mixture simply would not mix properly if I simply had my addition funnel drip the toluene in. (I am aware that industrially it is the nitrating
mixture that is slowly added to the toluene, but with the ammonium nitrate + sulfuric acid mixture it is much more difficult to do).
After adding all the toluene, I would let it with stirring on for many hours to give it time to fully react, when this happened the MNT layer forms on
top. Sometimes if the solution is cold (I keep my windows and balcony doors open to allow better ventilation), and once it is fully cooled again (I
never let the temperature go above 40C) and all the reaction is done, I then begin the heating step, I slowly heat it from room temperature to 90-95C
and I hold it there for 2 to 2.5 hours (usually the latter), then slowly heat it again to 120-125C and hold it again for 2 to 2.5 hours (usually the
latter again) before I shut off heating and let it cool down slowly to room temperature before pouring it out.
I noticed that Dugan didn't use a stirbar. he used an overhead stirrer and this is... a very expensive piece of equipment. But the stirring it did was
very strong. Could that have been the issue? Was the mixing insufficient?
So what now? According to duck.ai, they recommended a 2nd nitration with 2.2ml of 98% sulfuric acid and 3g of ammonium nitrate per 1g of MNT (this
stuff is DNT, I am confident), but in terms of using plain regular nitric acid (which I will be making. I need to make highly concentrated nitric acid
that is free of NO2. I'll be doing that very soon) I am willing to do that. Sadly I have no oleum and I am not sure if I want to make some, it seems a
little difficult and the chemical itself looks kinda dangerous.
So what to do now?
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greenlight
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Due to the melting point you observed, it is definitely nitrated to a higher degree than mononitrotoluene. I am confident you primarily have
dinitrotoluene.
The two major ways to increase reaction rate (leaving concentration constant), are providing more kinetic energy to the molecules via heating, and
increasing the number of collisions through stirring. Due to the polar nature of the nitrating mixture and non-polar nature of the toluene/MNT/DNT,
you will have a two phase solution that requires thorough mixing during the nitration. The more integration of the two phases through stirring you
can achieve, the more efficient and faster the nitration will be.
One option, like you stated, is the use of an overhead stirrer. I own one and can vouch for the much more vigorous and "aggressive" stirring they
provide, especially with viscous mixtures where a magnetic stir bar would not even move.
The second option is to minimise the height of the reaction mixture layer by using your largest flask (preferably a conical flask) or beaker. The
thinner but much wider layer of reaction mixture requires less power/torque to rotate the stir-bar through at its radius allowing sufficient rpm to be
achieved to get a "vortex" going.
The final major factor in reaction rate is concentration where obviously higher concentration results in an increase.
The best option for your current situation would be another nitration with 99% nitric acid and 98% sulfuric acid (considering oleum being unavailable)
at high temperature. Then you have the kinetic energy from heating, frequent collisions from stirring, and the high concentration harsh conditions.
I am sure this would give complete nitration and if you have the time to distill some high purity acid, this is the route i would take.
The other option is to have a shot with your ammonium nitrate/sulfuric acid nitration mixture with high temperature and good stirring. You don't have
the high concentration nitric acid present and you are fighting an uphill battle with the water byproduct formed from the nitration though. Maybe use
a large excess of this nitrating mixture, like 2 or 3 times what is stoichiometrically required to ensure that there is an abundance of nitronium ions
present. I still don't know if that will be enough to ensure full nitration though.
Be careful of that AI, it is often incorrect and makes up nonsense. I mean, it thinks your product is MNT.
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ManyInterests
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| Quote: Originally posted by greenlight | Due to the melting point you observed, it is definitely nitrated to a higher degree than mononitrotoluene. I am confident you primarily have
dinitrotoluene.
The two major ways to increase reaction rate (leaving concentration constant), are providing more kinetic energy to the molecules via heating, and
increasing the number of collisions through stirring. Due to the polar nature of the nitrating mixture and non-polar nature of the toluene/MNT/DNT,
you will have a two phase solution that requires thorough mixing during the nitration. The more integration of the two phases through stirring you
can achieve, the more efficient and faster the nitration will be.
One option, like you stated, is the use of an overhead stirrer. I own one and can vouch for the much more vigorous and "aggressive" stirring they
provide, especially with viscous mixtures where a magnetic stir bar would not even move.
The second option is to minimise the height of the reaction mixture layer by using your largest flask (preferably a conical flask) or beaker. The
thinner but much wider layer of reaction mixture requires less power/torque to rotate the stir-bar through at its radius allowing sufficient rpm to be
achieved to get a "vortex" going.
The final major factor in reaction rate is concentration where obviously higher concentration results in an increase.
The best option for your current situation would be another nitration with 99% nitric acid and 98% sulfuric acid (considering oleum being unavailable)
at high temperature. Then you have the kinetic energy from heating, frequent collisions from stirring, and the high concentration harsh conditions.
I am sure this would give complete nitration and if you have the time to distill some high purity acid, this is the route i would take.
The other option is to have a shot with your ammonium nitrate/sulfuric acid nitration mixture with high temperature and good stirring. You don't have
the high concentration nitric acid present and you are fighting an uphill battle with the water byproduct formed from the nitration though. Maybe use
a large excess of this nitrating mixture, like 2 or 3 times what is stoichiometrically required to ensure that there is an abundance of nitronium ions
present. I still don't know if that will be enough to ensure full nitration though.
Be careful of that AI, it is often incorrect and makes up nonsense. I mean, it thinks your product is MNT.
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Thank you, this will be what I must do. I will do my best to make sufficient quantities of WFNA (I am currently making nitric acid with sodium
bisfulfate, which does make it quite red, and the NO2 in it is what lead to runaways with my RDX synths. One thing I want to do with my next nitric
acid distillation is to bubble out the NO2 and then re-distilling it with sulfuric acid or magnesium nitrate in order to make sure it is 99%.
For the nitrating solution. What is the ratio of DNT to sulfuric acid + nitric acid? I won't bother with more ammonium nitrate. I really need to make
sure this works.
Note: I am looking through my notes/video collection on oleum... maybe, just maybe I might make an attempt to make oleum, since the reagents are just
sulfuric acid and sodium bisulfate.
Edit: I won't be getting an overhead stirrer, that stuff is just too expensive. Almost as much as a mantle. But maybe... just maybe... I might make an
improvised version using my power drill. no promises though.
[Edited on 13-9-2025 by ManyInterests]
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greenlight
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Yes, bubbling dry air over a period of time results in completely colourless fuming nitric acid. I have used this process many times.
The reaction equation for toluene to trinitrotoluene uses 3 moles of pure nitric acid (one for each nitro group). Hence, the reaction equation for
one mole of dinitrotoluene to trinitrotoluene requires an equimolar amount (1:1). So one mole (182 g) of DNT requires 63 g of nitric acid.
At the end of the day, that is on paper in a perfect world, and real life is quite different, so an excess of nitric acid will not do any harm at all.
Within reason, an excess would be beneficial as it would probably increase yield and enhance reaction rate.
If you have a slightly lower concentration of nitric acid, that would need to be factored in when calculating the quantity needed.
As for the oleum, I believe with a controlled sulfur dioxide generator, it would be quite simple. I have never tried but someone on here surely has
documented the synthesis.
The only problem with converting a power drill to an overhead stirrer I can think of is overheating due to drill's not being manufactured to run
non-stop for hours on end.
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ManyInterests
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| Quote: Originally posted by greenlight | Yes, bubbling dry air over a period of time results in completely colourless fuming nitric acid. I have used this process many times.
The reaction equation for toluene to trinitrotoluene uses 3 moles of pure nitric acid (one for each nitro group). Hence, the reaction equation for
one mole of dinitrotoluene to trinitrotoluene requires an equimolar amount (1:1). So one mole (182 g) of DNT requires 63 g of nitric acid.
At the end of the day, that is on paper in a perfect world, and real life is quite different, so an excess of nitric acid will not do any harm at all.
Within reason, an excess would be beneficial as it would probably increase yield and enhance reaction rate.
If you have a slightly lower concentration of nitric acid, that would need to be factored in when calculating the quantity needed.
As for the oleum, I believe with a controlled sulfur dioxide generator, it would be quite simple. I have never tried but someone on here surely has
documented the synthesis.
The only problem with converting a power drill to an overhead stirrer I can think of is overheating due to drill's not being manufactured to run
non-stop for hours on end. |
I didn't think about the drill overheating. But that is because I also forgot that I need to be running the thing for hours! I mean when I did my
synthesis, I would time it and it was 9.5 hours! That is an entire day's worth of stuff. I did this synthesis several times and it meant I couldn't
leave my home because you really, REALLY don't want to leave something like unmonitored.
Also the noise of the drill would not be pleasant. I will have to try to use my stirbar at its maximum capacity and not overfill the flask. I used a
2-necked 2000ml flask, and I used the proportions that Dugan used, which was 155 or 160ml of toluene... and the resulting nitrating mixture nearly
reached up to the bottom of the necks.
Simply put... the flask was so full that being able to aggressively stir it with a stirbar was impossible, that was possibly my issue, in addition to
slowly heating it up instead of aggressively heating it up. At any rate, when I do the 2nd nitration, I must make sure that the flask is not so full
that I have this problem again.
One other question: You mentioned the ratio of nitric acid (and I am assuming that concentrations of 90% to 99% would be sufficient?) what about the
sulfuric acid? I will definitely be adding a good surplus of nitric acid, maybe around 90g or 100g for that amount of DNT you specified.
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greenlight
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Yes you definitely never leave a reaction unattended, especially one of this sort.
The flask being that full would indeed cause issues stirring, there's simply no room for the liquid to move with much velocity. Rule of thumb for
round bottom flask's is not more than two thirds full.
The sulfuric acid is there primarily as a donor to produce the nitronium ion but it is also a dehydrating agent with the purpose of dealing with the
water by-product that is formed. Usually for most nitrations it is around a 2:1 ratio sulfuric:nitric, but it varies. Just need a sufficient amount
to ensure protonation of the nitric acid and to scavenge water.
Two or three times the volume of nitric acid I would guess is enough,
I dont know how it stacks up against oleum as a replacement, so I can't give an exact answer here.
[Edited on 15-9-2025 by greenlight]
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ManyInterests
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| Quote: Originally posted by greenlight | Yes you definitely never leave a reaction unattended, especially one of this sort.
The flask being that full would indeed cause issues stirring, there's simply no room for the liquid to move with much velocity. Rule of thumb for
round bottom flask's is not more than two thirds full.
The sulfuric acid is there primarily as a donor to produce the nitronium ion but it is also a dehydrating agent with the purpose of dealing with the
water by-product that is formed. Usually for most nitrations it is around a 2:1 ratio sulfuric:nitric, but it varies. Just need a sufficient amount
to ensure protonation of the nitric acid and to scavenge water.
Two or three times the volume of nitric acid I would guess is enough,
I dont know how it stacks up against oleum as a replacement, so I can't give an exact answer here.
[Edited on 15-9-2025 by greenlight] |
Thanks, I think I got enough information to move forward. Yeah this will be a challenge. But that's what this whole hobby is. I mean TNT is a
challenge to make. It isn't like ETN that can be made very simply.
I assume that the heating must be fairly rapid towards 125C and held there for several hours? Like 2.5 hours? Upon the addition of the DNT to the
nitrating mixture?
I am also assuming that I will need more sodium metabisulfite to clean it! I had already used up all my sodium metabisulfite supply, but that's
another pile of money to spend! 
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greenlight
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Glad I could help. The hobby of the chemistry of energetics is challenging, especially with sourcing of reagents. Once you have synthesised the
easier compounds, you naturally want to move to more challenging ones with multi step synthesises. Unfortunately, many start off with dangerous
primaries and lacking safety, which often results in accidents.
As for nitration time, I am not sure of an exact heating time off the top of my head. I am guessing it would depend on the quality and purity of the
acids and DNT. You can't do any harm heating longer, and it would ensure a proper conversion. I would bring the heat up gently and slowly for
safety reasons.
[Edited on 16-9-2025 by greenlight]
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