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Trinitrotoluene preparation

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ManyInterests - 3-2-2024 at 10:22

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.

I was reviewing the synthesis videos and I did see at the end stage when they crash the nitration liquid in water they scoop away the crude TNT from the liquid as it seems to float on the top. How is the rest of that liquid disposed of? Simply dilute, neutralize and flush away, or does it need to be treated like it has some red water?

[Edited on 3-2-2024 by ManyInterests]

OneEyedPyro - 3-2-2024 at 10:58

Quote: Originally posted by ManyInterests  
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.

I was reviewing the synthesis videos and I did see at the end stage when they crash the nitration liquid in water they scoop away the crude TNT from the liquid as it seems to float on the top. How is the rest of that liquid disposed of? Simply dilute, neutralize and flush away, or does it need to be treated like it has some red water?

[Edited on 3-2-2024 by ManyInterests]


Are you referring to purifying crude TNT that has simply been crashed out of the nitration mix and filtered off? I doubt pressing it between paper is going to do much except remove water, you'll still have an acidic product with some lower nitrate and unwanted side product contamination.

If we're trying to be environmentally friendly here then incineration or long term containment are your best options for any kind of TNT waste.

ManyInterests - 3-2-2024 at 11:11

Quote: Originally posted by OneEyedPyro  
Quote: Originally posted by ManyInterests  
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.

I was reviewing the synthesis videos and I did see at the end stage when they crash the nitration liquid in water they scoop away the crude TNT from the liquid as it seems to float on the top. How is the rest of that liquid disposed of? Simply dilute, neutralize and flush away, or does it need to be treated like it has some red water?

[Edited on 3-2-2024 by ManyInterests]


Are you referring to purifying crude TNT that has simply been crashed out of the nitration mix and filtered off? I doubt pressing it between paper is going to do much except remove water, you'll still have an acidic product with some lower nitrate and unwanted side product contamination.

If we're trying to be environmentally friendly here then incineration or long term containment are your best options for any kind of TNT waste.


No I was referring to the left over water from that crash. The crude TNT I know I will need either to recrystalize in alcohol or to wash with sodium bisulfite until no red water is produced.

The red water I am aware now how to get rid of... just evaporate it off and incinerate what is left behind. That isn't difficult. I many containers and a blowtorch and I can find many places to do it easily.

DennyDevHE77 - 4-2-2024 at 01:45

Quote: Originally posted by OneEyedPyro  
Are you referring to purifying crude TNT that has simply been crashed out of the nitration mix and filtered off? I doubt pressing it between paper is going to do much except remove water, you'll still have an acidic product


What I meant is perfectly clear from my comment:
Quote: Originally posted by DennyDevHE77  
it can be compressed in layers of newspapers so that they absorb dinitro derivatives. You can add calcium silicate so that it absorbs TNT oil.


I do not know where you saw here that I claimed that such an operation would allow you to get a product free of acids. I was talking about the purification of TNT from dinitro derivatives, that is, from TNT oil. They make TNT weaker, oily, and can be released during storage. Although I think even this is not particularly important for home use. And then, it will remove a significant amount of TNT oil, but not all of it.

And as for the acidic product, all aromatic explosives are generally acidic, and they are not afraid of acids. If you do not think in the future to fuse them with nitroesters (which are alkaline by nature, and which are just afraid of acids), then I do not see the point in cleaning from acids.

Meanwhile, due to the acidic nature of TNT, the alloy of chemically pure TNT and PETN still leads to decomposition, increased acidity and increased sensitivity after 3-4 years of storage.

[Edited on 4-2-2024 by DennyDevHE77]

ManyInterests - 4-2-2024 at 13:32

Quote:

I do not know where you saw here that I claimed that such an operation would allow you to get a product free of acids. I was talking about the purification of TNT from dinitro derivatives, that is, from TNT oil. They make TNT weaker, oily, and can be released during storage. Although I think even this is not particularly important for home use. And then, it will remove a significant amount of TNT oil, but not all of it.

And as for the acidic product, all aromatic explosives are generally acidic, and they are not afraid of acids. If you do not think in the future to fuse them with nitroesters (which are alkaline by nature, and which are just afraid of acids), then I do not see the point in cleaning from acids.

Meanwhile, due to the acidic nature of TNT, the alloy of chemically pure TNT and PETN still leads to decomposition, increased acidity and increased sensitivity after 3-4 years of storage.


I understand. What I am asking is before purification, the water you use to crash out the crude TNT. Is that anything special or do I neutralize it and pour it down the drain? the same way I neutralize and pour down the drain all the other water from other nitrations I do? (ETN, PETN, RDX, etc,).

DennyDevHE77 - 4-2-2024 at 20:26

I wasn't answering you.

But regarding your question, nitromass with TNT is usually poured into water, the TNT is filtered out, and it is washed several times with water.

All other cleaning, if reasonable, is done after that.

ManyInterests - 7-2-2024 at 03:07

OK, so that water from initial washing is no different than any other nitration. Gotcha.

OneEyedPyro - 7-2-2024 at 08:33

Quote: Originally posted by ManyInterests  
OK, so that water from initial washing is no different than any other nitration. Gotcha.


It contains some amount of TNT, lower nitrates and side products, in my experience the crash water smells awfully strong of those contaminates.
Neutralization and dilution isn't going to remove it.

Dumping it down the drain is irresponsible, even if you're logically just one guy contributing a very tiny fraction of pollution compared to the rest of the world.
Any TNT waste is best off being evaporated down and incinerated.

ManyInterests - 7-2-2024 at 18:14

Quote: Originally posted by OneEyedPyro  
Quote: Originally posted by ManyInterests  
OK, so that water from initial washing is no different than any other nitration. Gotcha.


It contains some amount of TNT, lower nitrates and side products, in my experience the crash water smells awfully strong of those contaminates.
Neutralization and dilution isn't going to remove it.

Dumping it down the drain is irresponsible, even if you're logically just one guy contributing a very tiny fraction of pollution compared to the rest of the world.
Any TNT waste is best off being evaporated down and incinerated.


OK I understand. All water must be evaporated and incinerated.

I will need to put forward my intended plan once I have figured out exactly what I want to do. I've been doing some research and I want to find the most economical and simplest way to do it. Ditto for cleaning it and properly disposing of all the unwanted byproducts. It almost reminds me of how I was during my picric acid synths, being all fretting more over cleaning the product than the synthesis of the product itself.

If there is one thing I am worried about it is the leftover sulfuric acid. Since that is not something that can be evaporated and incinerated away. It can be purified I guess, then I can reuse the acid?

OneEyedPyro - 7-2-2024 at 18:52

Quote: Originally posted by ManyInterests  
Quote: Originally posted by OneEyedPyro  
Quote: Originally posted by ManyInterests  
OK, so that water from initial washing is no different than any other nitration. Gotcha.


It contains some amount of TNT, lower nitrates and side products, in my experience the crash water smells awfully strong of those contaminates.
Neutralization and dilution isn't going to remove it.

Dumping it down the drain is irresponsible, even if you're logically just one guy contributing a very tiny fraction of pollution compared to the rest of the world.
Any TNT waste is best off being evaporated down and incinerated.


OK I understand. All water must be evaporated and incinerated.

I will need to put forward my intended plan once I have figured out exactly what I want to do. I've been doing some research and I want to find the most economical and simplest way to do it. Ditto for cleaning it and properly disposing of all the unwanted byproducts. It almost reminds me of how I was during my picric acid synths, being all fretting more over cleaning the product than the synthesis of the product itself.

If there is one thing I am worried about it is the leftover sulfuric acid. Since that is not something that can be evaporated and incinerated away. It can be purified I guess, then I can reuse the acid?


Some gentle heating, a bit of air flow and time is how I've always done it. The larger the surface area of the liquid the faster it will go. Using multiple evaporating dishes and leaving it in the sun, putting heating pads underneath etc helps.

Sulfuric acid is industrially recycled from nitration waste. I'm not sure how exactly but it likely involves filtration and distillation, I'd have to assume that bringing sulfuric acid to those temps would turn anything left from the nitration into little more than tar.

I'm sure someone here has suggestions.

Sir_Gawain - 7-2-2024 at 19:38

Heating an acid mixture that possibly contains an explosive just seems like a bad idea to me. Even a few milligrams detonating can break your apparatus and send hot sulfuric acid everywhere.

DennyDevHE77 - 7-2-2024 at 21:47

In industry, acids do regenerate. They begin with "denitration", that is, nitrogenous derivatives, nitrogen oxides are extracted, then nitric acid is separated from sulfuric acid, nitric acid is processed (into dilute, into ammonium nitrate) and sulfuric acid is concentrated and returned to the cycle. This is the usual option.

Moreover, in industry, it is ensured that no more than 1% of nitro derivatives are present in the waste acid, and only in "mono" form. Moreover, the monoform can pass into -di and -trinitroproducts in the process of denitration.

So first, the nitro mixture is diluted with water (to reduce the solubility of the nitro compounds), and the nitro mixture is defended, after which the nitro products are separated. Then (sometimes) polyunitro compounds are extracted using solvents, as is done in the production of picric acid and tetryl. Sometimes they are oxidized. Then the nitro mixture is diluted to 68-70%, this is necessary to remove nitrosylseric acid HNSO4. It is fragile in itself, decomposes when heated, but it is very stable in sulfuric acid above 75%.

So they dilute it to 68-70% and heat it up, and everything volatile flies away from sulfuric acid. That is, nitrogen oxides and nitric acid. All this is driven off through a denitration column.

The resulting dilute sulfuric acid is concentrated with flue gases 650-1000C
(obtained by burning fuel oil or methane).

At least that's how the industry goes) at home, you can just dilute the nitro mixture a little, defend, remove the nitro derivatives and surpass the nitrogen mixture. But this is not possible with every nitro compound. For example, a nitro mixture after the synthesis of rdx is extremely thermally unstable and cannot be distilled, and a nitro mixture after the synthesis of EGDN or nitroglycerin contains a lot of them, and it is defended for 8-10 days.

And about sewage. Don't do nonsense. Rinse the TNT on the filter a couple of times with water and rinse in the sink. Laboratories do exactly the same thing. The mass of nitro derivatives that will go into the wastewater is so minimal that it is stupid to think about it, after all, you do not have a plant with the synthesis of tens of thousands of tons.

[Edited on 8-2-2024 by DennyDevHE77]

ManyInterests - 8-2-2024 at 16:18

Quote: Originally posted by DennyDevHE77  


And about sewage. Don't do nonsense. Rinse the TNT on the filter a couple of times with water and rinse in the sink. Laboratories do exactly the same thing. The mass of nitro derivatives that will go into the wastewater is so minimal that it is stupid to think about it, after all, you do not have a plant with the synthesis of tens of thousands of tons.

[Edited on 8-2-2024 by DennyDevHE77]


I always did think that. I guess the same with the red water? The bacteria in the sewer could also make short work for it like it does with hydrazine waste.

B(a)P - 25-6-2024 at 14:41

Quote: Originally posted by sulfuric acid is the king  
Ok. I post this here but if it's some other topic, mods please send this post there.
This was found at local scrapeyard in same town where relatively big xplosive plant is located.
Flange diameter is about 500mm.
Inside of those holes were heating elements, resistance wire coil etc. So this was probably submerged in something to melt it.
Between those heating pipes you can see remains of misterious substance with physical characteristics like TNT, it's yellow, crushy..
But it doesnt want to melt even with the blowtorch, it doesnt want to be dissolved in acetone...
So what the F. can it be?
This thing was used to melt something and now it cant be melted even with the torch..
BTW material is 304 stainless.



It is highly unlikely to be any sort of explosive reside. When explosives plants are demolished/refurbished any scrap material must undergo thorough decontamination and validation to confirm they are residue free.

ManyInterests - 4-8-2024 at 17:15

While at this point I realize that simply neutralizing the red water (since it is acidic) and dumping it down the drain is acceptable. Since as I was told, the nitro derivatives are too minute to harm anything in the sewer system or the water treatment facilities.

But I did see this study that showed that distillation could actually render safe a lot of the stuff? I am not going to do it, but I found it interesting.

Attachment: zhao2010.pdf (328kB)
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