TNT synthesis

[radar]

Hi, I just recently made some mononitrotoluene, or so I think, I made it using this lab:


This Document And The Information Contained Herein Is Provided For INFORMATIONAL PURPOSES ONLY. It has been verified to work with the materiels available to us - This does not ensure everyone will have the same results. Results may vary, And we WILL NOT BE HELD LIABLE FOR YOUR RECKLESSNESS.
Outline
Despite What Some Preceding Documents May have stated, Crude 2,4,6 TrinitroToluene Can be prepared from less concentrated, more commonly available, easily produced acids. The Process is a Modified Three Step Nitration, Whereby Toluene is converted into MonoNitroToluene, Dinitro, And Finally Trinitro by the addition of fresh portions of Mixed Nitric/Sulfuric Acid. An External Source of heat is neccesary
Purification is accomplished through the usage of a boiling water liquidation, Whereby impurities float to the surface, which are easily decanted.. It can be scaled up or down depending upon materiel availability.
Materiels
Sulfuric Acid 99~%
This can be Found in Home Depot, In White Plastic Containers, Marked "Instant Power Drain Opener" Marketed By Scotch Corporation Of Dallas, Texas - 64Oz Containers of Concentrated Sulfuric Acid Found in the plumbing section. It is of 93% Purity - It must be concentrated via heating at 100C+ For 10 minutes. Water will boil off yielding Theoretically pure H2SO4 - This should be done OUTSIDE, As all Experiments should be.
Nitric Acid 70~99 % Concentration
The ~70% Materiel is available commercially, 99~ materiel is available via 88~C Distillation of Potassium Or Sodium Nitrate With Sulfuric Acid. The 70 % materiel will work, although yields will be less.
Toluene
This is found in the Solvent section of Home Depot in Gallon cans
It is used as a specialty solvent. ACE May carry it if it is unavailable in Home Depot
3 Glass, Heat Resistant Container(Pyrex, Kimax Beaker or Flask Preferably)
Acid Resistant Volume Measurement device( Graduated Cylinder Or Etched Beaker)
Glass Stirring Rod
Plastic Spaluta
Plastic Baster
Heat Source
Thermometer(Optional)
This Item would greatly increase reproducibility - But TNT Will still form without careful temperature control and based on subjective sensory perception. Celsius Has been included for those who do have the luxury of a thermometer. TNT is not a sensitive HE and thus there is no danger of temperature based runaway reactions leading to detonation.
Procedure
Measure Out 300 Milliliters Of ~99% Sulfuric Acid into the heat resistant glass container. It should be able to hold at 1000 ML. Add To This 100 Ml Of Nitric Acid 70%. If One is using 99~ Distillation Acid then 75 ML Of That should be used. Or .75
This is the standard ratio 3/1 Or .75 If 99~ Acid is used. Heat will be generated upon the Nitric acid mixing with the Sulfuric acid and a cloud of barely visible white N0x should be seen wafting over the vessel. Now One adds 100 Milliliters of Toluene. Upon The Toluene contacting the mixed acid, it will convert to a yellowish/Red oil which will float on the surface of the acids - Large Amounts of heat will be generated - This is Good. Just let the vessel sit alone untouched reacting for 2 hours. A very noticeable odor shall appear - This is due to MNT. Do NOT confuse this with the odor of Reddish/Brown N02 which may begin to bubble off the beaker when the reaction temperature reaches a climax. Some reckon it smells like "shoe polish", While others relate to it smelling "Almondish". Personally, it has a completely distinct smell that i do not feel is adequately characterized by any particular description. Let it react for 2 hours
The MNT will be a Aromatic oil on the surface of the acids. It should now have turned cold - Temperature must now be maintained externally. With a bunsen burner, alcohol lamp, or other heating device, heat the beaker to 80C~. If you lack a thermometer, It should be heated to the temperature of the beaker during the vigorous reaction. By this i do not imply one wait around while it is reacting, as Volumes of Nitrogen Dioxide, a reddish Brown gas, is produced, which is quite toxic and will produce pulmonary edema which may go unnoticed for a week, at which point one may die. This does not mean you will die if you take a little whiff, No, But common sense dictates that one should distance themselves from the vessel while it is reacting and avoid inhaling any fumes. It is heated externally for 30 minutes. Now using the Plastic Baster, suck up as much of the now dilute acid from the container and transfer to another suitable container for recycling(See Below) Or should be disposed of properly. Try not to get any of the MNT in with the acid, this will take practice. Now In another container mix another batch of 3/1 acid and add this to the MNT. Repeat above steps involving 2 hour wait and 30 minute external heating. Remove spent acid and add to portion of spent acid recovered form MNT nitration. The DNT will be a Yellow oily liquid, or a waxy yellow solid. Now Comes the final nitration. To The DNT is added a fresh portion of 3/1 acid.
The vessel will get hot and when it cools after 2 hours yellow needles may be visible in addition to some DNT. After allowing the vessel to react for 2 hours, external heating should be applied for 1 hour. When heating is removed the insoluble oil floating on the surface will solidify as it cools, forming a yellow crystalline cake, with many yellow needles embedded into it - This is TNT. Earlier methods involved filtration, but due to economic reasons good filter paper is not used, instead coffee filters - Since corrosion of the cellulose based filters has been shown, a spatula is used to "Fish out" The cake from the surface of the acid and into a separate plastic container like a cream cheese container. This can be done by tilting the container gently and sliding the cake along the side of the vessel and into the empty plastic container.
Purification
The empty cup with the fragments of cake, acid, is covered in about 150 ML Of boiling water - This will melt the TNT into a puddle under the water and cause insoluble droplets of DNT impurity to float onto the surface as an oil. Any Acid Will dissolve in the water. Let this cool, drain off the water and remove the "Wet Cast" TNT from the container, preferably plastic "I Can't Believe Its Not Butter" container, which bends easily allowing the TNT to loosen and fallout without cracking it. Place it on Layers of Paper towel to dry, as TNT will exude a yellow oil. Puddles of such exudate can be found in munitions dumps across the country. You will notice the Paper towels colored yellow. Allow the TNT to lay undisturbed on the towels, and if neccesary fresh portions of towel should be used to dry it. Later Castings should be done dry using a bath of boiling water surrounding a dry container with the TNT in it.
One should not worry too much about possible safety dangers, as TNT is fairly difficult to initiate accidentally. Although it is better to be cautious around explosives paraphernalia.


My MNT, is a yellow waxy solid at about 30 celsius, however when i looked up the msds it said that melted at -16 celsius or something like that. Maybe there are DNT impurities in it? As well some of it is long clearish yellow needle shaped crystals, Im really thinking that it is just contaminated with dnt or tnt which is no problem because i will have a dream about turning it into tnt, however Id like to see if you have any input.


BTW. Used 70% conc. nitric, and 99% sulphuric. Thanks

[EventHorizon]

That looks like the EPID (IIRC) text. The method works.

In the first nitration you get MNT(reddish brown oil), DNT(pale yellow to orange waxy soild), and TNT(pale yellow needles).

------------------
"Chance favors a prepared mind" - Louis Pasteur
PGP ID 0x147CEF54

[CodeMason]

Where did you get the text?

[radar]

I dont remember the website i got the text off of, but it was a pretty shabby website with just that and merc fulm synthesis on it. However the method looked good considering you use new acid at every step and that i only had 70% nitric. I had some dnt from megalomania's lab and thats as far as i could get it nitrated with his mehtod as he specifies 100% nitric, i took that and used the above method to make it into tnt and it worked. The tnt was kind of hard and crumbly and very light yellow whitish.

How many grams of picric acid should i use to detonate it? Thanks.

[10fingers]

*

<small>[ June 17, 2002, 02:49 PM: Message edited by: 10fingers ]</small>

[Mr Cool]

I too have heard that it will work, from quite a reliable source. I think it should, since it uses a lot of sulphuric to get rid of the water... and it sounds like you have TNT.
What about the good old H2SO4/NH4NO3 method for the last step? Seems to work for most aromatics from what I've heard.
I've been wanting to try this, but haven't seen any toluene recently http://theforum.virtualave.net/ubb/smilies/frown.gif.

[radar]

When I was living in the USA (now im in Saudi Arabia), I found toluene in hardware stores in the solvent section labeled toluol, if you are living in Europe or usa or canada, im sure you could find it if you checked a few hardware stores. I just dreamt that i detonated some tnt today, it seems to me the power is comparable to gelatin dynamite without the headache and is much more stable. It seems to me that tnt is an ideal explosive, something that i will dream of making more often and you dont need the goddamn 99% acid like rdx, as well i got a pretty nice yeild with the 70% nitric.


Oh yeah, kinda off topic but i dreamt that i made some lead picrate today with some homemade dreamt up lead monoxide, does anyone have any experience with this one? I used acetone instead of methyl alcohol and it seemed to have worked (deflagrates much l ike Hg fulminate with a flame.

[Mr Cool]

About how much TNT did you get, per 100mL of toluene?
No, I'm pretty sure nowhere near me sells toluene, but I'll keep looking. Perhaps I'll just go to Salisbury plain and find some UXO to take apart!!
Your lead picrate sounds about right to me.

[radar]

I dreamt up about 3 ounces with 100ml.

[CodeMason]

Oh yes, I've been to that site before. I have also heard the information there is reliable. Toluene/xylene is very easy to find where I live, regardless of it being a nasty carcinogen.

[SafetyLast]

Toluene is easy to find in the US it will be in any hardware store (ACE, Home Depot, TrueValue,Scottys,and Lowes) the solvent section is next to the paint aisle along with many other useful solvents ie: Xylene (brand name is Xylol), Denatured Alcohol (around 90% EtOH), and Acetone.
All come in quart and gallon sizes.

[cutefix]

Radar,were you able to make explosives secretly while in Saudi Arabia?It is hard to believe,I have lived there for some time and it is really difficult to obtain chemicals for explosive manufacture.As far as I know any purchase of suitable chemicals, say even sodium nitrate and nitric acid requires license from the authorities,and people who procure it are subjected to interrogation by the pigs.People there are extremely prone to suspicion.Or you made it as part of your job in commercial explosive manufacture affiliated with Saudi Chemical Industry,I am just curious...

[radar]

Hehe, thats funny that you ask, did you here about the bombing last night? Well it was in khobar, and i just happened to be there getting some nitric and sulfuric when it happened, as it is however, i live on an American compound for a company called Aramco, its so fucking easy to get chemicals here, i just go down to a chemical supply and can buy techincal acetic anhydride, nitric sulfuric, drug precursors, you name it. They have NEVER been suspicous of me. However when you buy some kind of nitrate they look at you with a funny look probably cuz thats the only boom stuff they know of (ie gunpowder) and why would i want to mess around with nitrates other than ammonium nitrate? So i just buy things like toluene, phenol, benzene, and other things and it is no problem at all. But fuck i was about 1/2 mile away from the explosion and it was pretty loud, id estimate about 1.5-3 pounds of HE. I went to the scene and saw the dead bodies, there were two guys laying down in a pool of blood all mangled and torn up, as well there was quite a few pieces flesh all smashed onto the walls around the area, it was a fuckikng mess. A saudi that i was talking to thought it was a propane tank that exploded, after seeing that, im kinda like ya fucking right. My only problem with boom materials is actually dreaming of detonating them, i have to do it under water or under ground because they are too fucking loud and will definately spook people out now.

[radar]

Oh yeah, and when they find who did it, the penalty is beheading, if they find them, i will go down and watch the execution and try to secretly take pics and post them on the board. (Now who wants to see that) eheh

[cutefix]

Yeah,you are right,I had seen a few of that both in Jeddah and Riyadh,in how they execute criminals.I think it is difficult to get pictures I was interested in doing that but the heavy cordon of security makes it impossible to smuggle in cameras near the chopping block.It is indeed interesting to watch.the drama of decapitation.
When I was there I was watching some SAS folks(who were assigned there) in the desert during the Guy Fawkes Celebration lighting bonfires andsetting off fireworks which was fortunately given permission by the authorities to do so.
It is really easy to get chemicals there.Other chemicals like Oleum,and acetic anhydride,phenols,pentaerthrytritol,hexamine are easily available also .I could have made my own fuming nitric acid for PETN or RDXbecause the place I was staying have good lab facilities somehow but it did not materialize because of tight security there, made it difficult for me to procure ammonium or other alkali nitrates.

[Mr Cool]

So that's nearly 1g per 1mL, which isn't too bad at all.
Anyone know how TNXylene compares to TNT? Because I can get xylene I think... but it just doesn't have the same appeal as the well known explosives like TNT!

[radar]

Yeah, how is TNxylene, that looks really interesting, and where the hell did you find pentaerythritol? Ive been having trouble finding it, most places only have the basic industrial chemicals(sulfuric, nitric, other shit like that) Id like to make some petn, but i have been using TNP, doenst TNP compare quite equally to petn? Anyway i think im gonna have a dream today with a big boom in it hhee. see ya.

[CodeMason]

Picric doesn't even come close to PETN.

[a_bab]

Not even in color....

------------------
Damn, I got a nitro-headache again...

http://move.to/pyromania

[VasiaPupkin]

TNX has m.p. about 125 C (mixture tech. isomers - "xylil") 182 C(2,4,6-TNX pure). VoD 6600 (at 1.58g/cc). Dens. 1.604 g/cc. Trauzl block test 270ml. Summary nitration process leads better with less temperatures, acids conc. (usually 5-15%H2O in industry) than with TNT. Yeild also some better. Sensitivity and chem. properties comparable. TNX was very useful in I - II WW.

[EventHorizon]

TNX is slightly less powerfull than TNT IIRC and there is something about the nitration that is either difficult or unwanted, I can't remember exactly what. Maybe it was just highly prefered to use pure xylene.

TNP is ~= TNT.

PETN, again IIRC, is 136% TNT.

------------------
"Chance favors a prepared mind" - Louis Pasteur
PGP ID 0x147CEF54

[radar]

Today I didnt have to go to school because a bomb threat was issued, so I slept in, way in, and i was awoken to the sound and feeling of an overpressure wave hitting my house, my house shook and the windows rattled. My sisters just got home from school, and whatever it was knocked the books off their shelves and blew out some windows. Anyway, if you see anything on CNN in saudi that happened today, it was most definately that.

[wantsomfet]

There are ortho- meta- and para-xylene. The m-xylene is the one to nitrate, o- and p- are easily nitrated but also easily oxidised lowering the yield. The trinitro isomers of the o- and p-xylene are quite unstable...

------------------
for best catfood visit:
kangaroooo.cjb.net (http://kangaroooo.cjb.net)

[radar]

10 fingers, Ill send you a pic of some tnt that i found. When i had dreams with big booms involving TNT, I used 1.5 grams of picric initiated with lead azide.

[SofaKing]

http://www.geocities.com/SoHo/Atrium/4758/index.html

That's the website with those instructions. Getting toluene is ify IMO. It sure isn't lable as such. Xylene and Naphelene(sp) though. But I havn't seem Xylene in gallon quantities.

------------------
With Knowledge we find Truth - With Truth we find Freedom

[radar]

If you ask for toluene at a hardware store call it toluol, and if they dont know what that is say you think its called tolue..ne sound kinda broken and dumb so they'll think you wouldn't possibly have any idea it could be used to make explosive, and just totally act like your using it for paint thinner or some other "legitimate" use. As well even ask them about other paint thinnmers they recommend.

[PYREX]

I've got paintthinner containing a mixture of toluene and acetone. The acetone can easily be evaporated. It's manufactured by Colodur and called "Nitroverdünner".

[Madog555]

event horizon. RDX is ~150% the power of TNT so id think that PETN is like 155% because its a well known fact that PETN is a little more powerful than RDX

[BrAiNFeVeR]

I've never seen a recipe involving metal nitrates ...

If you have the materials, I guess you could always give a shot at it.
Maybe in time, I'll try it myself, but I'm in the midst of exams right now, so i don't really have the time for anything more then a few AP crackers ...

[Madog555]

i make my MNT via KNO3/H2SO4 form my rack-a-rock. i originaly used 12g KNO3 20ml H2SO4 and 10ml toluene. i just guessed ratios from experiance. now that i have actualy done the calculations it is supose to be more like 15g KNO3. the yields that i have gotten for 12g KNO3 20ml H2SO4 and 10ml toluene have been like 7-7.5ml of MNT. let it nitrate for like 3 hours. if u let it go overnight the yields will be shit.

edit: oh yeah. i have a PDF on rack-a-rock. it has the recipe i made but it uses 12g KNO3, i should redo that PDF.

<small>[ June 19, 2002, 06:01 PM: Message edited by: Madog555 ]</small>

[nitriees]

TNT can be synthesis by multi-step nitration with low conc. HNO3,
I just think how about RDX.
Is it possible to use this method to produce Hexamethylenetramine
Dinitrate then next step to Trinitrate with low conc. HNO3?
Any catalys needed to do that?

[kingspaz]

the water in lower concentrations of HNO3 would decompose the HDN.

[Madog555]

you need a good concentration for HDN to RDX. people use HDN because you dont need as mutch HNO3 and the yield is better.

[cutefix]

Qoute:
--------------------------------------------------------
TNT can be synthesis by multi-step nitration with low conc. HNO3,
-------------------------------------------------
To my knowledge this is not true….
First consider that RDX is a nitramine type;the nitrogroups is bonded to the aza nitrogen(N-NO2).In hydrocarbon based explosives like TNT and other arene explosives.The nitro group is attached to the carbon (or C-NO2)..
If you want to make RDX by direct nitration,it will have to pass into hexamine dinitrate as an intermediate (in situ).Further nitration will add the third nitro group.All of these will be attached to the aza nitrogen.And the last reaction needs a highly concentrated acid.
Now your question is the feasibility of using lower concentration of nitric acid,which is not possible;and as you will notice even by nitrating TNT,that further di-and trinitration needs increasingly concentrated acids,that you have to add even oleum in order to attain the desired niric acid concentrations.
In my observation,it is difficult to make nitramine type explosives by direct nitration with nitric acid concentration of lesser than 95%.The best yields bythis method is, if you can use the 100% or absolute nitric acid.
But do not lose hope(there is a expensive way to if you still insist in using your only available 70% nitric acid, you still can make RDX if you add enough phosphorous pentoxide(about 30%) which will generate N2O5 which can then increase the concentration of your nitric acid to enable it to achieve your desires. :)

<small>[ June 19, 2002, 10:01 PM: Message edited by: cutefix ]</small>

[Madog555]

thought that i should post this:

today i was going to make MNT. i decided to use NaNO3 and use extra. i reacted 30ml of toluene 45g of NaNO3 and 60ml of H2SO4. now i have what apears to e a realy shity amount of DNT. i will nitrate it further but i would like to weigh it first to see yield. you will soon have the measurements.

<small>[ June 20, 2002, 01:05 PM: Message edited by: Madog555 ]</small>

[10fingers]

I think the formula given above may be incorrect. It says to use the "standard" nitration acid mixture of 3:1 by volume, sulfuric to nitric. Should it not be 2:1 by volume or 3:1 by weight?

[nitriees]

Thank you Cutefix.
I can't get any HNO3 here, the only possible way to get HNO3 is by
KNO3+H2SO4.
By boiling down drain opener or battery water to high conc.what is the max conc. H2SO4 i can get? Add KNO3 to H2SO4 obtained from this
method, what is the max conc.of HNO3 can be?
By this method is it possible synthesis RDX, since i can't get any
toluene and PE here?
I don't have distillation tool also.

[cutefix]

Nitries,this sulfuric acid from battery acid have been discussed several times already.There had been successful synthesis in many explosives using it.You can refer to the forum archieves for details.

You are trying to make a pickle of salts , acids and hexamine? :D

You really have to distill the acid and alkali nitrate mixture in proper equipment order to get the desired nitric acid before you add it to your hexamine.

[mr.evil]

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica"> I've got paintthinner containing a mixture of toluene and acetone. The acetone can easily be evaporated. It's manufactured by Colodur and called "Nitroverdünner".
</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">here, in The Netherlands i can buy bottles of 1L, called just: 'Thinner' on the label it says 'bevat Tolueen(Contains Toluene)'. There's also some Propanol and Butanol in it, but i guess that can be extracted by adding NH4OH and drown the NH4OH/Butanol/Propanol layer...

would 90-95% Toluene work well for TNT?

[cutefix]

Well if these solvents have different boiling point;they can be separated by fractionall distillation.However I doubt if you will get really pure toluene,because of the possible formation of constant boiling azeotrope...Consider these boiling point values:
toluene-111degC
2-propanol -82deg C
2-butanol -94deg C
If you nitrate 90%toluene (containing butanol/propanol)with mixed acids you will get mostly mononitrotoluene and some traces of nitrobutanol and nitropropanol.These nitrated alcohols are more soluble so they will be separated from the MNT and can be found in the mixed acids...
subsequent nitration to the dinitro and trinitro level will be devoid of these contaminants.
Therefore it is possible to use that toluene...

[da man]

the other day i bought some solvent containing:
60% toluene
30% methyl ethyl ketone
10% unknown (it didn't say on the label)
I tried seperating the toluene from the methyl ethyl ketone by adding it to alot of water (methyl ethyl ketone is soluble in water 25g/100ml) and i got an oily layer as expected which was translucent (a kind of whitey colour, opposed to a water clear colour which the original solvent was). I did a very quick test and added this to some nitric/sulphuric acid, and after 10 min, i got a thin layer of red oil (obviousely mononitrotoluene). Im not quite sure if i got pure toluene or not, and if this translucent colour is normal, but i will do a proper batch soon.
So IF it woked for me, it should work for acetone, as it is totally misible with water.
Oh, and if you add the toluene to nitric/sulphuric acids quickly at room temperature, does it normally go nust with the nitrogen dioxide, and spit out acid?

[cutefix]

Preferential solubility of these hydrophilic solvents(e.g acetone and these alcohols) to water will then allow it to be separated from the lipophilic hydrocarbon solvents like toluene

Mixed acids condition favor the generation of nitronium ions which is the reactive specie in many nitration process.
I do not see that more acid is formed;rather the nitration acid(HNO3) is gradually consumed as the nitration proceedsWater that is formed with the removal of the nitrogen oxides(through formation of nitroniumions) is simultaneously absorbed by the sulfuric acid.

[mr.evil]

in a dream i've made MNT. It was made by using 20ml 97% H2SO4, 9grams of KNO3 and 9ml C7H8.
On the link below you can see some pictures of the MNT and the Acid mix in a sep. Funnel. I will do some tests with it in combination with KClO3 or NH4NO3.

The toluene used in the dream was the 'Thinner' brand paint Thinner. And was been purified by shaking it with NH4OH to extract the Butanol/Propanol. I guess the Toluene was about 95% pure. And it worked well! :)

When the acid was added to the Toluene, the fluid became kinda thick, almost like soft solid. When it stand a few hours, it became liquid again...


<a href="http://www.geocities.com/tshadowpp/MNT.html?1025250302490" target="_blank">http://www.geocities.com/tshadowpp/MNT.html?1025250302490</a>

Edit: some spelling errors

Cya

<small>[ June 28, 2002, 03:52 AM: Message edited by: mr.evil ]</small>

[mr.evil]

Fuck!
i've just tried to make MNT with HNO3/H2SO4.
But i guess i added the C7H8 to fast, the temp was aout 36 Celcius... But suddenly it rised to about 45 Celsius(hot spot?) and it started to fume(NO2) and there were some little bubbles in the acid mix... I started to freaking out so i putted the acid/MNT mix(totall 200ml) into 1L of cold water... What a waste of Acids. (i don't care about the C7H8, it is dirty cheap!)

I will try to make MNT again later this day, but this time again with KNO3 as it works always! Also i think it is better to make a few small batches(5-10ml C7H8) then 1 big batch of about 50ml or so...

For the people that are interested please e-mail me so i can show you some pictures... I can't upload now because there's something wrong with Geocities here :rolleyes:

By the way,
my lab stinks like Almond now, Yak! :p

Edit: some spelling mistakes

[andreas]

When I tried to make mnt with h2so4 and nh4no3 with an eccess sulphuric to get rid off the moisture from my ammoniumnitrate I was left with a solid myproduct with wich I was intrigued because tnt synthesis should be a three step nitration I have some foto's so what do you guys think.
<a href="http://www.boomspeed.com/kramrak/tnt1.JPG" target="_blank">http://www.boomspeed.com/kramrak/tnt1.JPG</a> <a href="http://www.boomspeed.com/kramrak/tnt2.JPG" target="_blank">http://www.boomspeed.com/kramrak/tnt2.JPG</a> <a href="http://www.boomspeed.com/kramrak/tnt3.JPG" target="_blank">http://www.boomspeed.com/kramrak/tnt3.JPG</a>
I think I stepped a step in the synthesis and went almost directly to tnt

[Mr Cool]

It does look rather like TNT...
Make sure it is washed very well, to remove any AN or ammonium sulphate.
Then put it in a pan of water, and heat it with very rapid stirring until it melts. Record its melting point with a thermometer, and let us know...

[nbk2000]

Sounds more like para-mononitrotoluene. Mp is 52 degress C, yellow crystalline material. No way you're going to get TNT by one-step nitration like that.

<img src="http://server3001.freeyellow.com/nbk2000/DNT.gif" alt=" - " />

<small>[ July 19, 2002, 09:46 AM: Message edited by: nbk2000 ]</small>

[andreas]

there is that one problem. I have only got a thermometer tha has a range to 40 degrees.
I had the same thought as you Mr Cool, boiling ethenol has a boiling point like 79.?? degrees and as I recall corectly tnt has something like 80.6 so pretty similar. I'll try it someday and post the result. I just thought off the reason Iit may have happened was becouse i added not even a quart of al the tolueen because I was a little bored so anywaythat's my idea

<small>[ July 20, 2002, 08:49 PM: Message edited by: andreas ]</small>

[Einstein]

I'm dreaming to make some TNT after I will get my lab apparatus. I'm going to distill some car battery acid (37% -&gt; 98%) and buy nitric acid from chemical supplier (sp?) and in here Finland, toluene is sold in paint shops, like RTV, Värisilmä, K-Rauta, Rautia etc. as "Thinner". It is 100% pure toluene :D

BTW, I was thinking this: How strong your nitric acid will be if you just boil it like H2SO4? I mean without any other chemicals.

[rikkitikkitavi]

68,3 % by weight.

/rickard

[Einstein]

I could get 65% HNO3 but I'm not sure how good it is going to work. If it works I could do some TNT on this winter.

And BTW, I did some calculations and here is my result: 1000 grams of toluene COULD be nitrated theoretically fully with 100% HNO3, so that you could get about 2,4kilos of TNT! This f....... amazing! (sorry my language) So I think that even if you use 65-70% HNO3 you could get 1 gram of TNT per 1ml of toluene at least. That would be 100% yield...cool...

Oh, almost forgot: Does anyone know how much water can 1 litre of 98% H2SO4 absorb into itself? This would be good to know for calculations :D

[ALENGOSVIG1]

Considering the amount of acids that are needed to nitrate the toluene 3 times, the yeilds arent that good.

[nbk2000]

One thing that allows for making TNT is that you can use the acid left over from the tri-nitration to do the di-nitration, and the left overs from that for the mono-nitration.

Thus, you only need the strong stuff for the final stage. After that, you can use the spent for the previous two steps.

Though I think the acid would be better used for PETN or NG if you have it. The only advantage to TNT is that its castable.

[spydamonkee]

radar:
would you be able to tell us what sort of det you used to initiate your tnt?... IE: filler (grams), casing, fused or electriacal & weather you used a booster or not.
cheers

nbk:
why you say it owuld be better to make PETN, or NG instead of TNT?
seeming i aint able to get my grubby lil hands on any pentaerithrytol i wont be making any PETN, however i could make NG... but i would prefer to make TNT as its a little safer to make,handle & also by the time you have mixed the NG with some sawdust wouldnt the VoD be about the same?

<small>[ July 25, 2002, 03:43 PM: Message edited by: spydamonkee ]</small>

[Einstein]

I forgot to post link to my TNT calculations...everyone can understand it, but the text is only readible for Finnish guys... <a href="http://koti.mbnet.fi/vaakkupr/paukut/TNT.jpg" target="_blank">TNT calculations</a>

<small>[ July 28, 2002, 11:37 AM: Message edited by: Einstein ]</small>

[Trinitrotoluene]

A few days ago i had made a few batches of MNT first batch i used 20ml H2SO4 93% 12 grams of KNO3 and 10ml od toluene.My yeald was 8.5ml that time i didin't cool it useing an ice bath.My second one I used the same ratio my yeald was 5.5ml and i used an ice bath.Today i decided to make MNT in a larger batch so i used 45 grams of NaNO3 60ml of H2SO4 and 30ml of toluene. When I added the toluene a runaway occured and NO2 was given off.I cooled it with a water bath then the temperature rose to 85*C when i took it out of the water bath.I let it react. After that the acid mixture solidified and I extracted the MNT and put it in a 50ml beaker.Then i watered doen the solid mass and DNT started to percipitate. Then i recovered all the DNT that remained. I left everything outside and i went to work when i came back the MNT had turned to DNT. I ectracted everyting my teald od MNT was 2ml and DNT 22 grams.

[Mr Cool]

Check th m.p. of the DNT against the literature; if you started with toluene it could easily be contaminated with large amounts of MNT, which would result in a m.p. below that of pure DNT. If that is the case then you might want to recrystalise it, but you'll need to find a solvent which dissolves MNT well and DNT poorly - any ideas anyone?

[Trinitrotoluene]

I think my first batch I had extracted is pretty pure DNT.But my second batch that had formed after the MNT solidified is pretty contaminated.I left it overnight and it leached out a pool of some yellow substance i think its MNT.Will the method of using NaNO3 and 93% H2SO4 work if I try to convert The Di to Trinitrotoluene?

[Mr Cool]

Yes, although 98% H2SO4 would be better and you'll need quite a lot of it.

[Trinitrotoluene]

2 days ago I had successfully made TNT. I prepeared a soloution of 30ml of 98% H2SO4 and 25ml of yellow HNO3 in a 150ml beaker I think concentration was 93+%. Then added 22 grams of DNT. I droped it in there so some acid splatted out and hit my hand yes I got burned and it was painful. But after that no reaction so I heated the soloution to 80*C a self substained reaction occured and the temperature went up to 110*C and NO2 gas given off. After the reaction subsided I maitained the heating at 100-115*C and at one point it went up to 130*C and lots of NO2 given off. Every time I go above 110*C NO2 id given off. But I maitained heating for 1 hour and 45 minutes. After that I turned off the heat and went to sleep. Next morning I went to see a oily layer floating on top of the acids. I thought it was usless crap. But I extracted it anyways. I extraced the stuff and placed it into 120ml of distilled water in a 150 ml beaker. After that I eat lunch and went back to check on my experiment. I see a tiny yellow crystal floating on the surface and a solid casting on the bottom thats crystaline.With joy I jumped and yelled. After that I purified it but heating it to 80*C then it melted and started stirring and did that a couple of times my TNT turned colors from yellow to peach. Then I took it out and weighed it I got 6.5 grams of TNT out of 22 grams of DNT. But Oh well as least I made TNT. I'm not disappointed with my results The next day I added water to the waste acid, cooled it and waited.After a while I got TNT percipitated and I filtered it. Then I purified it and Weighted it I got 2.5 grams. So total recovered 9 grams of TNT from 22 grams of DNT. I will try again next time with a bigger batch and below 110*C. I think the large volueme of NO2 is to balme for the poor yeald. I will experiment again soon. But as for now I will keep making MNT and DNT.

[ALENGOSVIG1]

I too have recently made some TNT. I found that alot of times i had to apply heat in the steps where the temp is supposd to be controlled by addition rate. I used about 110ml of 98% HNO3 (diluted in some steps) and 50ml of toluene which yeilded 48g of slightly yellow TNT. I dont know the total amount of H2SO4 used.

I got a pretty shitty yield though. I'd take nitro over TNT anyday. NG has better yeild for amounts of acids used, it's more powerful, and you dont stink like almonds after making it :p

Plus TNT takes a long time to prepare. Alot of stirring too! A magnetic stirrer would be a must if you wanted to make alot of TNT.

<small>[ January 28, 2003, 11:25 PM: Message edited by: ALENGOSVIG1 ]</small>

[Trinitrotoluene]

Three days ago I had a dream of prepearing TNT. In my dream I took 70grams of DNT and placed it into a 800ml beaker. In another beaker I mixed 100ml of 98% H2SO4(boiled drain cleaner) with 40ml of 95% HNO3(freshly distilled). Then added it to the beaker with the DNT. No reaction took place. A little heat was applied, and a vigerous reaction took place, temperature was at 130*C alot of NO2. After 15 minutes the reaction stoped, and using a hotplate the temperature was maintained at 113*C for 2 hours and 45 minutes, along with alot of stirring. The stirring part was very boring. After that it was left to sit over night.
In the morning an oily layer on the top, it was placed in the fridge and cooled, a solid mass formed along with some needlelike crystals imbedded under the mass in the soloution.
Then 200ml of water was added the mass was broken and allowed to mix, it was placed outside again and left overnight. In the morning there was some needlelike material floating up on the surface as well the the broken solid mass. One strange thing is the acid/waste soloution turned a blush green, I suspect it is caused by the dye in the H2SO4, when stirred N02 is given off.
I will dream about cooling the mixture in the fridge again, filtering the crystals and weighing the yield.

[Trinitrotoluene]

In my dream I let it sit outside in the sun the temperature raised up to 45*C.Almost everything inside melted, therefore it failed to convert to TNT. I will soon dream of cooling it extracting the DNT and atempting it nitrate it again with more H2SO4 and HNO3.

[rooster]

I made TNT some days ago, and I must say the yield was not impressive. From toluene to MNT, I got a good yield, about 100 mL from 100mL toluene. (I did not weigh it.) The DNT was wierd though. I used 98% HNO3 and 98% H2SO4, and I got a mass of crystals, or at least it was not behaving like wax. I probably got some TNT also, but not solely.

I did one more nitration with the same percentage acids, but freshly distilled nitric and unused sulfuric just to convert the rest of the DNT to TNT. However, it seems that a lot of the TNT dissolved in the acid mixture.

Does anyone know how soluble nitrotoluenes are in nitric and sulfuric acids?

[Mendeleev]

I went to Lowes and asked for "toluol paint thinner". The guy gave me a puzzled look :eek: and said he wasn't sure what that was. He showed me a gallon of Crown brand paint thinner, but I doubt it was toluene because it did not say anything about carcinogen on the back, whereas Crown brand Xylene did. However I don't need Xylene. Does anybody know where to buy this alleged toluol paint thinner in the U.S.?

[Sir Dudalot]

I haven't bought any (no need for it...yet) but I've seen it at Ace Hardware. Also at Lowe's, maybe ont that one, some True Value's may have it (mine doesn't). It really shouldn't be that hard to find. The one at Ace Hardware is "Toluol." It's in a big rectangular can that's bright yellow and grey. It says toluol really big. It should be right next to acetone, xylene, MEK, etc. Happy hunting.

[Versalius]

Your local Sherwin Williams paint store should have gallon sized jugs of toluene, at least mine does. I have not found it pure anywhere else. Hope this helps.

[Trinitrotoluene]

If your in CA it would be more dificuit finding it. From what I heard it's illegal here, thanks to those drug addicts inhailing it to get high. I was lucky enough to find it in a paint store thats still selling it. It was pretty old cans, as they may as well kept selling it after it was banned.

[freaky_frank]

I'm going to give TNT a try soon, but I don't have 70% nitric acid,only 65%....
Could I also make TNT with 65%....
I would then use 1:3 HNO3:H2SO4 and then add toluene, toss it in there all at once, let it react for 2 hours then heat it to 80*C for 30minutes...then extract the oily MNT, then make a fresh nitrating bath (the same as before) and then pour it in there, for 2hours and 30minutes heating and then make another nitrating bath and pour the DNT in there for 2 hours and heat for 60minutes...and collect the solid perticipate right?
Is this right, and don't you have to stirr anywhere in the reaction?

Thanks in advance

[Trinitrotoluene]

From my experience converting toluene to MNT dosen't require heat, heat if no reaction starts, if its reacting theres no need to heat, you will notice it as the mercury in your thermoneter rises.Its always good to keep stirring the mixture. You may even want to moderate your reaction a bit so it dosen't get too hot, after your done, let it cool, collect your layer of MNT.
I don't think converting from MNT to DNT would require heat either, unless it dosen't start reacting, just add the MNT slowly and the reacton would start,keep stirring after your done, let it cool, and collect the DNT which appears like butter. Maybe some crystals of TNT imbedded in it.
From DNT to TNT you will need stronger acids, after the initial reaction you would need constant stirring, and heating after it.

[freaky_frank]

Okay thank you very much, and would 65% HNO3 be good enough to nitrate the DNT to TNT?
And the MNT is made in nitrating bath A and DNT to TNT in nitrating bath B
Could I use nitrating bath A to nitrate the MNT to DNT?
And how powerfull is DNT and MNT....anyone got a VoD or a leadblock expansion test?

[Trinitrotoluene]

I doubt you'll have much of a success with 65%HNO3, maybe if you have fuming H2SO4, that's a different story.
Yes nitrating mix or you mean xNO3/H2SO4 can be used for toluene to MNT, and MNT to DNT, I had heard about someone who tried it with DNT to TNT many times, no success.
MNT isen't even an explosive, although it can be used to senistize chlorates, and AN compostion.
From what I heard DNT is an explosives with a volocity if about 5000m/s, that I'm not too sure about.

[Rosco Bodine]

Actually there is a patent which describes higher nitrations of aromatics
using milder concentrations of acid while azeotroping water from the
nitration mixture . Even TNT from ordinary concentrated nitric is reportedly
produced in high yield . I have not tried this method myself .
It may work to simply azeotrope the water away from a mixture of
toluene with a petroleum solvent like naphtha or Coleman camp stove fuel ,
using ordinary concentrated nitric for the nitration . A reflux setup with
a drain valve equipped Dean Stark trap would be required , or something
equivalent used for trapping and draining away the separated water which
"steam distills" from the mixture as the nitration proceeds . This method
requires no sulphuric acid to be present in the nitration mixture .
The TNT is produced directly in one step , in a highly pure form ,
and 90 per cent yield , with no waste , as the residual liquid can be reused
in subsequent batches .

See US2435314

[Mendeleev]

I just learned what an awesome investment TNT is, because it can be used to produce pentanitroaniline. Add sulfuric acid to TNT to reduce it to 4-amino-2,6-dinitrotoluene, and nitrate that with sulfuric and nitric acid to get pentanitroaniline, which can be used to make hexanitrobenzene. If anyone is interested I can post the ratios of the reactants.

[Microtek]

You can't reduce a nitro group to an amine group with sulfuric acid. You probably mean hydrogen sulfide ( H2S ) right ?

[bobo]

I found some paint thinner that contains (and smells like) toluene. Now I think, it also contains alcoholics and perhaps other aromatics. Is this problematic? I think, the alcohols can be extracted out with water. Then, a contaminated toluene would remain. The step towards MNT seems not the most dangerous if there is contamination, but would it be possible to get pure MNT or DNT from such a source?

[Mendeleev]

Yeah, you're right Microtek, thanks for correcting me there ;). I just always thought that TNT was a waste of acid when nitroglycerin and RDX can be made using much less, but with this latest development... :cool:

[T_Pyro]

You can reduce a nitro group using metal filings (Sn/Fe) in the presence of a mineral acid (H2SO4/HCl), or using H2 in the presence of Pt catalyst. I think you misread your source in a hurry.

[Mendeleev]

Microtek was right, it said, "reduced with H2S in p-dine", whatever the hell that is. Anyways, it looks interesting, maybe a project for this upcoming Christmas break... :D

[freaky_frank]

Hey bobo, if you would have searched in this topic, on the first page, you would have noticed this.

here, in The Netherlands i can buy bottles of 1L, called just: 'Thinner' on the label it says 'bevat Tolueen(Contains Toluene)'. There's also some Propanol and Butanol in it, but i guess that can be extracted by adding NH4OH and drown the NH4OH/Butanol/Propanol layer...
From Mr Evil.

And this reply from cutefix
Well if these solvents have different boiling point;they can be separated by fractionall distillation.However I doubt if you will get really pure toluene,because of the possible formation of constant boiling azeotrope...Consider these boiling point values:

I'm only just new, but I DO know that I have to search before asking....:p

[MACE]

hi
i also know the patent wich describes the production of TNT with a reflux-setup from diluted NHO3 but i don't have hexane to try this out. do you think it's possible to use cyclohexane as a solvent instead? this procedure should be given a try because if this works this would be a good procedure. a litle time consuming but still good for home use. anyone tryed out this procedure before?

bye MACE

[Microtek]

At the moment I'm developing my glassblowing skills in order to make a Dean-Stark trap for use in such a setup. According to my calculations, using this procedure with 53 mL toluene, 120 mL 62 % HNO3 and 220 mL of diluent such as heptane or other alkane with suitable boiling point, the product would be 110 g TNT. If it works like the patent says. I don't need such large quantities, but it would be interesting to experiment with application of the principle.

[Rosco Bodine]

Microtek

If you have the glass adapters to do the arrangement ,
a regular distillation setup could be rigged in a way that
allows an adjustable depth dip tube to be inserted in the
receiving flask , and provide a distillate return path through
a side vented vacuum adapter into an addition funnel above
the nitration / distilling flask . An aquarium pump could be
used periodically to pressurize the system and pressure
pipet the contents of the receiving flask upwards into the addition
funnel which would serve as a reservoir for returning solvent to
the nitration flask . A vacuum pickup arrangement could also be
devised to provide the same function . The depth of the dip tube
could be adjusted to keep the pickup end in the upper solvent layer
separated from the water layer settled in the bottom of the receiving
flask , where it would remain trapped as it distills from the reaction .
A three necked receiving flask would make this setup possible . The
progress of the reaction would have to be watched , and the return
of distilled solvent done manually , cycled every few minutes , so it would
involve some extra work . The cycling could be automated by a timer
and solenoid valves .

The ideal water trap device for this type of reaction is made similarly
to a soxhlet extraction apparatus , having no siphon tube but only a simple
overflow tube located about two thirds the capacity of the chamber .
The bottom of the chamber is fitted with a three way stopcock which can
either drain the chamber directly back into the distilling flask , or
can drain the chamber outwards through an external delivery tube .
When the apparatus is assembled , solvent is poured through the
top opening of the condenser to fill the chamber to about the overflow
tube , with the stopcock closed . When the reaction is in progress
the separating water accumulates in the bottom of the chamber ,
and the solvent is returned through the overflow . The stopcock
can be used to drain away the waste water from time to time to
prevent the chamber completely filling with water to the overflow .
The draining off of the water can be done dripwise all along so that
the water level in the chamber rises only very slowly and does not
require constant attention on a reaction which may run for hours or
even for days of slow azeotroping .

The water separators which are used on fuel lines between
the fuel tank and an engine do exactly the same task ,
and depending on the materials from which a fuel /water
separator is made , one might be adaptable for this use .
Wetted surfaces of teflon and glass would work for sure ,
but anything less would be undesirable .

[MACE]

hi

there is no need for building an exotic, complicated setup because you can bye a wartertrap for just a few bucks at ebay (thats where i got mine).
i found a site with a table of many different aceotropes this could be of interest
http://infosee.ethz.ch/kilo/tabellen/aceotrope.html
anyone knows if there could be any reactions betwen cyclohexane and nitric acid? i think no because cyclohexane is a saturated hydrocarbon but i'm not sure.

bye MACE

[Rosco Bodine]

MACE ,

There is nothing complicated or exotic about a water trap adapted
to this sort of steam distillation , they are simply hard to find ,
especially on eBay . If you found one , then you got lucky .
Is it a microscale fixed trap for student work , not for larger
batches , or were you were really fortunate to find a better trap ?
Many will either have to have such a trap custom made or
improvise it themselves .

Have you considered using ordinary naphtha , available as
charcoal lighter for charcoal cooking grills , and as generic
"mineral spirits" paint thinner ? Coleman camp stove fuel
might also work . Any saturated hydrocarbon more difficult
to nitrate than toluene at the temperature specified should
work fine , so long as the hydrocarbon forms a similar or
higher water content azeotrope for steam distilling water
at the temperature of the nitration . If the temperature
for steam distillation of the azeotrope is too high for the
solvent chosen , then a partial vacuum can be used to
get the reaction to proceed in the temperature range
specified optimum by the patent .

Trichlorethylene might be a good solvent . There may be
some reference to its use with nitric acid in the literature
and patent references about methylene chloride and
nitric acid . IIRC there were comparisons done regarding
the effectiveness of several chlorinated hydrocarbons in
extracting nitric acid , and trichlorethylene may have been
one of those solvents tested .

I mentined a Dean-Stark trap earlier and there is a
slightly different type trap which would be better .
A suitable trap would be a modified Barrett type like
the larger one on the following page , the larger one
of the two would be best .

http://www.kimble-kontes.com/html/pg-751530.html

[MACE]

hi

i didn't know that thes wartertraps are so hard to find nor that they are so expensive. i just searched at ebay and found one. at last i got it for arround 7€. it looks like these in your link (just a bit longer) and holds 20ml.

yes i tought about using BBQ lighter but the problem is that you never know whats really in that stuff and what side reactions happens if you use it. these chlorated hydrocarbons you mentioned are impossible to come by for me. for this reasons i will try my cyclohexane for the reaction. at first i will do a test (heating chex. and hno3 in test tube) and see what happens. if all looks good i will try to use the chex. in the tnt procedure.

bye MACE

[will]

About how much TNT did you get, per 100mL of toluene?
No, I'm pretty sure nowhere near me sells toluene, but I'll keep looking. Perhaps I'll just go to Salisbury plain and find some UXO to take apart!!
Your lead picrate sounds about right to me.

i to live in england :) and i managed to find my toluen/xylene in B&Q under the name of tinner solvent and it worked well in the synth for TNT and detonated i think it conaned some TNX which did not spoil the proformance.

------------------------------
Use capitalization, keep to orthography and don't quote whole posts. I'm not going to say it again!

Rhadon

[Myrol]

I had a Idea about making Dinitrotoluene! A Mix of 100g Potassiumnitrate and 170-180ml conc. Sulfuric Acid should be enough to make DNT @ 90°C! This method seems like an alternative to the (more) expensive methods with Nitric Acid! 100g PN can Nitrate around 90g Toluen to MNT and a fresh Batch Acid the MNT to DNT! Shit, is there really no way to make TNT without white fuming Nitric Acid? 98% Sulfuric Acid and dry Potassium Nitrate at 120°C should work to make small amounts of (the good old & safe) TNT! Another Question: I've heard about a stopped Bombing-Truck from the ETA-(bastards) Terrororganisation who was loaded with 500kg!!!!!!!!!! :eek: :eek: pure TNT!! How to Hell is it makeble to prepare so much TNT?? I think these bastards must have a source to the local Armysupplier! An other way seems to be impossible in my eyes!

[Microtek]

You are probably right about the ETA having a source for explosives that could be traced to some kind of legitimate industry, but it would not be at all impossible to make 500 Kg of TNT if you had enough money.
There are plenty of factory plans and flow diagrams out there that describes how TNT is made industrially, and with money to buy acid resistant steel parts to make a small "plant", and access to raw materials, I don't think it would be too difficult. You would need some engineering knowledge of course, but since they don't aim to run it with a profit, the "plant" doesn't need to be optimized.
Finally, even if they had to do it batchwise, it's only a question of repeating the process enough times....

[Sonny Jim]

TNT seems a bit of an odd explosive to mass produce like that, don't you think? I would have thought that anyone clever enough to make that much TNT would know that ANNM would be a much easier route to an explosion of that size.

Anyway I might have a look in B&Q to see if that solvent's about. I'm not too bothered about making TNT but I would be interested to see how well DNT sensetises AN. From what I've read, it sounds promising.

Final thought. If Xylene is present in a mixture with toluene, would it not be easier to nitrate and thus bugger up a TNT synth? I'm pretty sure that the extra CH3 group of xylene would make it a better nitration candidate than toluene.

[vulture]

First of all, the truck wasn't loaded with TNT (you should know by now that the media thinks TNT is the only explosive and the main ingredient of dynamite... :rolleyes: ) but with ammoniadynamite and chloratite.

Furthermore, the ETA steals it's explosives from mining sites or buys them from mining suppliers who either don't care or are sympathizing to the cause.

[Boomer]

I had a funny experience when making TNT. The toluene was from thinner, with the alcohol being extracted with water until the top portion stopped getting less with each washing. It said “contains methanol and toluene”.

In the mono-step 96% SA + 55% NA was used. After warming the reaction started, and the mix (300ml) got so hot I had to cool it (>80C). It suddenly turned green, then black. Next day it was a clear yellow again, with a good yield of orange/red MNT swimming on top. Could the colours have been caused by contaminants in the toluene (the other chems were industrial).

The second step was done with SA/AN, and gave a waxy substance in perhaps 50% of theory.

The third step was done with 96% SA and freshly destilled NA of density 1.55 (I know this is too high, but I measured it right from the freezer, so it was a little denser). After 3 hours at 110C and cooling I got crystals and a cake with some waxy stuff left (probably un-reacted DNT).

Now comes the funny part: I re-crystallised from ethanol to get pure crystals, and indeed got light yellow crystals. To test the purity, I put a test glass with ¼ gram into a water bath getting slowly hotter. THEY NEVER MELTED, NOT EVEN AT BOILLING !!! :eek:

What have I made? HNS? TNX? TNB? What was in the fucking thinner? :confused:

[Bert]

What have I made? HNS? TNX? TNB? What was in the fucking thinner? :confused:

Perhaps you could give us a bit more physical information on the product...
Can a small ammount be melted on an oil bath, or does it decompose/detonate first? If you can melt some, what is the density?

Can you do a fractional distillation of the thinner, and identify the constituents?

[Boomer]

I did some more tests. 100ml of the thinner were mixed with 300ml water. The upper layer of 62ml was extracted again (each time 400ml total), giving 45ml. 3. step gave 41ml, 4. step 40ml, 5. step 39ml. The 1ml was considered losses and the extraction stopped.
The remaining liquid started boiling slowly at 100C, and boiled constant at 104C. Fractional distillation is beyond my possibilities unfortunately. :(

The yellow crystals were tested in a test glass inside a glycerine bath: they started to clump a little at 170C, and melted to a uniform liquid at 174.5C.
If heated on a spoon, they melt and after more heating (guess: 250-300C) burn with a yellow flame and black smoke. They burn slowly without hissing within 2-3 seconds.

The melting point suggests trinitroresorcinol, but resorcinol is a solid and unlikely to be found in a thinner. I thought of TNX, which would explain the vigorous reaction during the mono-nitration. It is also easier to tri-nitrate than toluene, suggesting that the crystals are mostly TNX, while the wax-like stuff contains TNT and non-reacted DNT.

My guess would be that the thinner contained also xylene, not labelled due to its lower toxicity. The crystals would then be TNX, with the m.p. lowered 10 degrees (from 185.5C) by TNT/DNT impurities. But with the boiling point of toluene (111C) and the 3 xylenes (138-144C), why does the mix boil at 104C? Maybe the riddle will never be solved. :confused:

If not for the bad yields, I would use the unknown stuff as is, even if it is not castable. Or stop with a better yield after the dinitration, and mix the wax-like mass with AN to form donarite. :)

[pdb]

I need to prepare a few grams of TNT to conduct experiments on eutectic mixures with other explosives, like cyanuric triazide. However, I don't feel like going the traditional long and painstaking way starting from toluene... I have access to industrial TNP: does anyone have ideas on a possible route from TNP to TNT ? (I personnaly never heard of it, but that maybe because starting from an HE to prepare a less powerful one makes no sense)

[Mr Cool]

I don't think there'll be a way that's easier than TNT from toluene... PCl5 then MeLi or something? I don't know.

[pdb]

It may not be the best place to post, but I can't find the Shaped Charge thread anymore ?!

These pics are from a shaped charge I made and fired some years ago, with a sharp angle liner (21°). It pierced 6 steel discs 10mm thick, and could have gone through one or two more. When you see the effect with an average HE like TNT, you can imagine what to expect from PETN or
RDX, or even better HMX and the like...

[Mendeleev]

OTC HNO3 is not available to me. I am against buying it online because that defeats the whole purpose, might as well buy the freakin' TNT. Thus I distill it myself, the process from sulfuric acid and nitrate salt yielding roughly 90-95% acid. I wanted to know what ratios you would use for 98% H2SO4 and 95% HNO3 by volume, for MNT, DNT, and TNT based on 100 mL toluene. Those are some pretty impressive pics pdb!

[vulture]

I remember some patent about Zr compounds catalysing nitration of aromatics, might be worth looking into.

Mendeleev, calculate it yourself: 2 moles H2SO4 per mole HNO3 for formation of the nitronium ion + 1 mole H2SO4 for absorbing the water produced in the reaction. It goes without saying that 1 mole of HNO3 is required per NO2 group. Don't forget taking the densities into consideration.

[Rosco Bodine]

GB501034 describes some nitration catalysts and some high nitration
products for naphthalene . I have done no experiments to test the validity
of the patent or to see if it works for TNT .

[Mendeleev]

I had already done the calculations, vulture, nitric acid 90%, density 1.5g/mL and sulfuric acid 98%, density 1.83 = 53 mL of Nitric acid and 186 mL sulfuric acid per 100 mL toluene. The same is to be used for conversion of MNT to DNT, and DNT to TNT. However my issue was not with stoichiometry and unit conversion, but reaction dynamics. In synthesis there are more issues that reacting proper stoichiometric amounts, there's equilibrium and knetics. If you do the conversion to MNT using 1:1 mole ration of nitric acid to toluene, toward the end of the reaction you will have nearly 0 concentration of nitric. I do not know that much about the reaction dynamics of touene nitration, so I don't know if there are any concentration limits. In RDX nitration for example, the acid conentration can't fall to less than 80%, same with PETN I think. What if the nitration of toluene does not proceed beyond a certain nitric acid concentration, say 50%? That would mean you would have to double your amount of nitric acid. That was why I was asking. Furthermore 53 mL nitric to 186 mL sulfuric is greater than the 3:1 ration described at the beginning of this thread even though the acid concentration used was lower. So the 3:1:1 molar amounts aren't the final word, so my question still remains, can anyone confirms the proper ratios using 90-95% nitric acid?

[vulture]

Sorry bout that, as a chemical engineer in training, I consider everyone familiar with the effects of an excess of reagent on reaction kinetics. :o

[Mendeleev]

Excess amount of reagent does not affect kinetics. Kinetics is dependent on concentration. Excess amount of reagent affects equilibrium. The excess reagent will not speed the reaction so much as mantain the speed of reaction because the concentration decreases less, but that's still mainly concentration-related. You can have an equilibrium which will proceed to 99.999999% completion with excess reagent, but if it takes 50 years, that reaction probably isn't of use to you. Besides, a 1:1 mole ratio isn't exactly excess, and even if your sulfuric acid is in excess, your nitric concentration will still decrease as the reaction proceeds, there just won't be as much water, but if you have .5 moles of nitric dissolved in 1 L of water and .5 moles of nitric dissolved in 1 L sulfuric acid, in both cases you still have a .5 molar concentration of nitric acid. As mentioned previously kinetics is dependent on concentration, hence the dillema. I realize that excess sulfuric still advances the reaction because water is the main obstacle, but a 3:1:1 ratio seems to be cutting it close. Also it was mentioned that spent acid from TNT could be used to make DNT and the spent acid from DNT could be used to make MNT. If you used a 1:1 mole ratio as you suggested you that would make those claims of using spent acid false, either that or it is not a 1:1 mole ratio.

[vulture]

Excess amount of reagent does not affect kinetics. Kinetics is dependent on concentration.

Ehm, excess amount of reagent also means higher concentration, thus affecting kinetics. With higher concentration you'll reach your equilibrium faster.

[Mendeleev]

Excess reagent will mean you will have higher concentration of that reagent in the mixed solution, but then that will decrease the concentration of your other reagents. I realize however that sulfuric acid catalyzes the reaction, I was curious because 1 mole of nitric per 1 mole of toluene seems a little close as I've stated in the past three posts. Never mind, I will try the procedure anyway with 200 mL H2SO4 and 75 mL 95% HNO3, and see how it works. It will be easier than asking you for help.

[Myrol]

First, sorry for bringing up an old Thread especially because a similiar one is actually active

Yesterday and today I did some experiments how to reach the best results for Nitrotoluene synthesis and then for TNT. I prepared three Nitration batches at one time the first with 100ml 65% Nitric Acid and 200ml 96% Sulfuric Acid,
the second with 50g Sodium Nitrate and 100ml Sulfuric Acid and the third with 50g Ammonium Nitrate and 100ml Sulfuric Acid too.

I planned to add 150cc Toluene to the first, 60cc to the second and 65cc to the third.......but it came a lot different as I thought.... :(

Because of the size of the first batch I started with the Sodium Nitrate mix. The Nitrate was mostly dissolved so I added 15ml Toluene to start the Game. It worked very nice.....the Toluene got VERY intense Nitrated and after I noticed that the flask cooled down I added another 5ml Methylbenzene to produce a hot climax in the flask. Well the Hell was open.....the reaction went crazy and the temperature was raising till the flask was boiling hot. Some seconds later......presto...I've got a RUNAWAY! I saw how the liquid evolved more and more gas and I was then unable even under chlling with a bucket full of cold water to dimnish the temp down. The mix was over 130°C hot......that's even for TNT to much :eek:

I bumped then the flask IN the bucket and grabbed my next batch....the Ammonium Nitrate mix. I was very careful whilst adding the Toluene....another runaway would be worse :( :p I lacked a cooling bath.....so I was just able to add around 15ml from the 65ml.

The Nitration was smoother but the Temperature was also very high! I was tired because It was 11pm so I stopped any other doings and went to bed.

The next morning after releasing the stress, brushing my teeth and the whole other ALL-DAY boring shit I started to Nitrate 100ml Toluene with my Acid mix.

P.s. Before I went to bed I took over four Vitaminpills because the contamination of myself with DNT and MNT was a littler higher as ordinary. I just need my liver furthermore so I want to save it this way!

Well so far so good. After beeing a little scared through the runaway on Friday I Nitrated this batch carefully and got then a real good success. :D I have now a really big layer of DNT floating on the Acid. My Balcony does not smell more that strong after marzipan. I'm a little unsure but I know DNT ís a real killer for your liver and has someone some data about the real toxicity of Nitrotoluene's?

TNT is especially through it's less volatility moderate toxic, MNT more like noxius but what about the intermediate DNT??? Thats the most poisonus Nitro-Toluene and unfortunately my most produced substance actually.......Oh dear :rolleyes:

Now my conclusions from this "battle" (mix vs. Toluene): If you want to Nitrate Toluene in one step to TNT do it with Sodium Nitrate and H2SO4. The reaction is extremly vigorous and if you do not cool effective you get a runaway very fast (like me :D ). The mix with Ammonium Nitrate works a little smoother and slow's down very fast........but watch out! Even this one works effective and violent and go's fast to DNT. To TNT does it need a little extra heat but it's possible!

Well, and my smoothest mix is the good old Nitration Acid mine one 100ml Nitric Acid 65% and 200ml Sulfuric Acid 96%. It worked very good. Relatively slow compared to the other ones but also that hot like the AN-mix. Plus I have nearly no more MNT left after adding some AN to make a pale yellow product instead of the blood red MNT-Oil. I'll see, if the next weekend like this one comes and the Forum enforces my TNT-desire again :D I Nitrate the whole DNT to TNT perhaps with some NaNO3 or HNO3.

[nbk2000]

So did you get any TNT, or just up to DNT, with your experiments?

[Chris The Great]

I'm doing a large amount of reading on the synthesis of MNT, DNT and TNT and what optimizes the reaction. The biggest impression I've got on making TNT in my readings is that the reactions are very picky about conditions, and not having ideal conditions will completely kill the yeild.

I'll write up all the information I've found on the synthesis and such when finals are over and I'm not doing all those big projects teachers assign all at once when the end of the semester comes up.

[Myrol]

Yes of course NBK! My 250ml Round-bottomed Flask was entirely full with lots of Asbestos-like fine snow-white TNT needles :) I melted them with the remaining DNT together, I was able to recover 7g of this yellow stuff!

I think It would been nice if I had made a picture from the bucket where the runaway occured. At the bottom was a big layer with lots of unregular chunks solid DNT. My DNT is vannila-yellow and smells soooo gooood :)

I can see the grade of the Toluene nitration very good. MNT is a blood red oil wich smells similiar like toluene but also after bitter almonds. DNT smells entirely like marzipan. Benzaldehyde comes close, but that's even a little more stronger as DNT.

Oh and my TNT has no smell. If it's pure, washed and dried I can absolutely smell nothing. I think if you stick your nose in a 50kg box of cast TNT rods you will smell something, but my tiny bit is odorless.

In the next time, I will make a lot of DNT because I bought 3Liters very pure Toluene from a Paintshop and the synthesis is very easy! The big plus of DNT and TNT against Acid impurties is the excellent chemical stability where EGDN and NG will decompose steadily with no end :(

I hope I can get my hands on a liter 65% SO3 Oleum....59€ from "Merck" but enough fopr several kilos pure TNT.

If I'm ready with my DNT I will post how good my results in making TNT with NaNO3/H2SO4 mix and mixed Acids are! I definately need some Sodium sulfite to purify my DNT and TNT.....someone an Idea how I can make it, get it or is it possible to produce it from NaOH and SO2?? (without NaHSO3 impurtie's).

[nbk2000]

Sodium sulfite is used in crafts for patinating of copper and other metals. You may also be able to use bisulphite, which is used in rust remover additive, often found in with the laundry detergents and toilet chemicals.

[Myrol]

I tried the "one-pot" TNT synthesis today without Gasoline and some different ratios but I must say it's just wasting time :rolleyes: !

I used for 60ml Toluene 200g Sodium Nitrate and 400ml Sulphuric Acid. The first stage of the Nitration was strangely slow and it heated not that much like with mixed Acid's. So I siwrled everything out until everything didn't reacted more for it's own.

I activated then my Dimroth-Reflux condenser and started to heat the mix but due to lot's of difficulties with the weather I had to abort the Nitration and placed everything beside. (My cooling water began to freeze, the Tube's were stiff like "Big Dick" and I was permanently annoyed with a unpleasant smell of bitter almond an Nitric Vapors. After the smell turned to sweet marzipan, I aborted because the mix was then not to much wasted (DNT was reached).

My conclusion: I stop making Nitrotoluenes for now. It isn't worth the effort, you have a lot to much trouble to make TNT whilst PETN is far more easy :)

The one-step-one-pot TNT Synthesis should work....but it's a nice waste of good Sulphuric Acid. I will use my good H2SO4 now for Esters. Have fired successfully 7g of Pentrinal one hour ago. The flash and the Blast was really good and the effort for such a stuff isn't that big as for TNT, huh :D ?

[Bert]

Could someone direct me to the patent information for the one step TNT synthesis utilizing HNO3 and Dean-Stark trap? I searched for it, but haven't managed to find it yet... Recall seeing it a while back here.

[The_Rsert]

Is it possible to use tri- or dichlormethane or something other as another solvent for toulene instead of gasoline?

[Mumble]

The only proceedures for TNT I have seen using either were to extract fuming nitric acid from a mixture of KNO3 and H2SO4. The nitration was carried out with the DCM still in the mix so I don't see how it could hurt anything. DCM was specifically used. If the proceedure was based upon a real experiment you can use it. If it was just theory, you can still use it. If your DCM/TCM in pure I see no harm or side reactions.

[nbk2000]

So Myrol, you're saying that the One-Pot TNT synth does work, but that (in your opinion) it's a waste of time because it's so much better to make PETN?

Can you melt PETN and cast it? Why no, you can't. But you can melt TNT with PETN and make castable PENTOLITE. :)

I'd also suggest using the specified procedure verbatim, including the gasoline, before condeming it as a failure. Bread doesn't rise without yeast. ;)

[Myrol]

To NBK: Yes that'sright....TNT is a very preferred material if you want a HD casted Explosive....but did you never tried it to cast PETN? It's quite easy!

I tried it with a 4g sample in a test tube....Perhaps I should do another charge, photgraph it and post it until you believe it. I fired the charge with 0,4g AP....it was nicely better as pure NG ;) The flash is more intensive, and the brisance from the charge massive.

Cast TNT is not only good for demolition....it's also a nice fireball-effect substance wich is useful for night-surfaceblasts.....but cast PETN.....thats the fast hell!

P.s. my PETN was recrystallized from Acetone and even after everything was molten and solid back it was a perfectly white substance wich gave off only whilst the melting process some "slight orange" fumes....so casting PETN might be a safe thing. I'll keep on testing!

[bobo]

hmmm.... I think, the NG dangers are in the melting step right? i think of PETN as similar to NG but with higher mp... then I do not like your procedure.

I casted ETN and quit it because I thought of the analogies of it with NG and the freezing point trouble of NG. Perhaps this is folly and superstition.... but why do they always granulate PETN unless casting is dangerous?

[Myrol]

There isn't really much about the NG-friction explosibility wich I would pull toward other Explosives like molten PETN or ETN.

Well, I casted PETN twice now...and it wasn't that problem for me....just heat the Explosive carefully until *nearly* everything is molten and then let it cool back in your own way. PETN doesn't cristyllize very much like Picric Acid. Its just a white block of cast material then.

Lot's of books say that PETN decomposes until it melts...thats right if you look for storable charges....I fired my cast PETN at the same day so further decomposition was no Problem.

PETN (mine one was recrystalized) give off little red fumes or Acid Vapors whilst it's a liquid. Thats why I would say it isn't possible to STORE cast PETN. But if you fire your freshly cast charge within a week or so, it should be ok!

Ok guy's....back on topic.....sorry for screwing this thread a little. :o

[ALENGOSVIG1]

Red fumes/Acid vapors coming off the molten PETN...Yikes!

That must have been slightly nerve wracking. Don't ever have the feeling of "fuck this is going to explode in my face any second now"?

I've always been too chicken to cast anything but TNT, DNN, TNP and a few cast AN formulations. Oh yea and AP once; but that was just a controlled experiment. :)

However, none of this relevant ('cept maybe my comment about casting tnt :)), so get back on topic.

[Myrol]

Hello Men's! Yes my mass of reports about the Nitration become a little annoying ( I think so), but I just want to help finding out the best way for our own TNT.

Well, Last Weekend I tried a very stupid method of Nitrating Toluene but hey...it was a TRY. I weighed up 30g pure NH4NO3 and added 60ml 96% H2SO4 to dissolve the prills. The mix got warm so I addd then just 10ml of Toluene in a whole :eek:

The Reaction was ok, the mix didn't start to boil (ordinary I appreciated that!). So I waited until everything was ready to heat the mix to 125°C. I placed my Erlenmeyer on a Hotplate, turned it on and observed the reactions. The mix boiled hard, but the evolution of NO2 was mild. After nothing much happended then more I switched my hotplate off and let the Flask cool down. The Oil got blood red. But unfortunately, I knew it, it's absolutely NOT TNT. It looks more like Azobenzene. Reddish-Orange. Not even two good washes with Na2CO3 were able to remove the colour totally.

I have to wash it twice with Sodium Sulphite (500g in Stock), and perhaps AGAIN with Na2CO3. If the colour doesn't dissappeared then, I'll do a second Nitration. Some Oily stuff exudated out of the "XNT" so I think the Fusionpoint is now a little higher (52°C for the crude stuff :eek: ).

Ohh yes, and please dont heat DNT to much whilst washing it under water......I've done it yesterday and heated the stuff so much that alway's a delayed boiling occured (=Siedeverzug in German). Once it was so strong that some drops DNT jumped out of the beaker ON the hotplate aaaand poof, pop, PAAM, Boff...I got several Deflagrations and even one small but sharp explosion like a grain AP lit by a match.

Well, If you want to make extremely pure TNT so Nitrate very pure 2.4. DNT with a mix of 25% HNO3, 60% H2SO4 and 15% free SO3 at 95°C under good stirring, reflux and 90min. reaction time...the Fp after purification is 80,6°C.

BUT if you want the better way and a 80% Yield is ok to you then use a mix with 20% HNO3 and 80% H2SO4 (French Method). Nitrate 90min. at 120°C and purify really GOOD. I just love DNT and TNT.....the handling of both substances is very very easy.....no decomposition like with NG, no huge volumes of a PETN slurry. Melt, wash, cast and good. :D

Somebody an Idea how to gt some nice samples TNT in Germany? Are there list's of Ammo-Dumps from Germany or forbidden areas where I could get some old TNT? Damn, I can't wait to see some TNT melting and freezing thousands of times. It's always fun to me!

[K9]

I've read through the thread and seem various similar ratios with slight variations. If someone could tell me if this is correct for MNT it would be a great help. 20 ml 98% H2SO4, 10 g NH4NO3, 10 ml toluene. And just let it react on its own after mixing?

[Myrol]

K9, if you wanna make MNT in a pure Form always use the following mix containing 100ml HNO3 65% and 110ml H2SO4 96%. Ordinary you can Nitrate 145ml of Toluene with this mix, but for me I was just able to Nitrate 125ml Toluene to prevent the formation of a deep reddish Oil.

The Nitration must be carried out at 45°C in the beginning. 50°C in the mainpart and 60°C at the End. But watch out! Dont add in your first step to much Toluene to the fresh Acid....I've done this because I thought the Temp. didn't rose a lot....My mistake, 40ml Toluene within 1min. was to much.....even with very good cooling (5kg Ice+5Liters Water) the Temperature rose to 60°C until she felt down back. But later then, everything went fine.

The Yield looks like around 125ml MNT, I say I think because I didn't even washed the MNT...The Flask is still wrapped inside Al-Foil and get bored on the Balcony :D

I will later Nitrate the MNT to pure DNT via Nitrating with 130g AN and 250ml H2SO4. After lot's of attempts I have the best methods for MNT, DNT and TNT all in one:

MNT: 100ml HNO3 65% and 110ml H2SO4 96% for 125ml Toluene 45°C start-->50°C main-Nitration and 60°C in the End.

DNT: 100ml MNT slowly mixed with 100g AN and 200ml H2SO4-mix-->60°C in the beginning and a slowly increasing to 100°C whilst Nitration for an Hour or so under good stirring. A Reflux-Condenser is prefered but without one you'll get also your DNT (with a little smaller Yield)

TNT: 100g of small DNT chunks are added to 115ml H2SO4 96% and 35ml HNO3 100%. You have to start at 60°C wich means you dont must add the DNT only when the Acid reached 60°C, just watch the reactions when you reach that Temp. Then, slowly increase the Temperature until 105°C are managed and boil then to sharp 120°C under good stirring for an hour.

The Excess of Acid is quite massive. Normally you just need 23ml of white Nitric, but this time.....it's necessary! The TNT will crystallize out in form of super-long fine needles (I know that!). It's advisable to dilute the Acid a little and filter out the remaining TNT dissolved in the Acid. Spill it in a Fitler with lots of Water, melt it in a Beaker with fresh Water and neutralize it excessive with Sodium Carbonate.

It's not bad if you add a little extra Carbonate, Trinitrokresole, Trinitro Benzoic Acid, TNB and Tetan...all these oxidation products go into solution and you'll end up with a much better product. Then do a careful Sulphite-wash (melting, good stirring etc.) and purify your TNT like always further.

I will make an Instruction for the three-step TNT preparation with my way. After I have enough pictures from all three synthesises I'll make it into a .pdf-document and add it to the Roguescience FTP.

P.s. The Picture is from the MNT-Preparation to clarify what I'm brabbling about! ;)

[nbk2000]

From the picture, I'd say you have no problem keeping the reaction cool. :cool:

[Chris The Great]

Just tried making MNT yestrerday and againt tonight, but I'm not sure if I succeeded the second time.

In the first try I mixed 200ml H2SO4 and 90g NH4NO3 together, then added a small bit of urea. I put it in some cold water since it seemed pretty warm and I wanted the clouds of HNO3 fumes to stop (they didn't). I started adding toluene with rapid stirring, and the reaction proceeded instantly giving me a yellow layer floating on top. I added a bit to much toluene at once and got some NO2 condensing on the sides of the jar (looked really cool). No runaway occured and I kept adding toluene, but NO2 was coming off noticably so I added more water to cool my jar, and *crack*
A crack forms going halfway around the jar. I stopped the reaction and left it in the bucket overnight in case it started leaking, with the intent to transfer it to another jar and finish the nitration later. About 50-60ml of toluene had been added. A strong smell, presumably MNT, was present.
The next day it had solidified, so it seems I got DNT instead. I filtered it out, attempted to neutralize some of the acid, but the stuff stuck together so I couldn't. During the filtering and washing, a considerable amount of orange colouring went off with the water, I am not sure what it is since nitrotoluenes are not soluble in water. After an hour of sitting on a paper towel it started to ooze out MNT... so it was obviously a mixture of the two of them.
Pic:
http://img395.imageshack.us/full.php?image=dnt6xw.jpg

Then I tried the following:
I mixed 200ml conc. H2SO4, 90g NH4NO3 and 40ml water together with a salt-ice bath for cooling. It fumed a fair bit of HNO3 fumes, but not as bad as before. I started adding toluene, but there was no evidence of an immediate reaction as there had been before. I added all the 170ml of toluene in about 5 minutes. No immediate reaction, no NO2, just HNO3 fumes. I stirred for about 5 minutes, then realized I was retarded and that 1.5 moles NH4NO3 is 120 grams, so I added another 30 grams to the mixture and stirred it for 35 minutes.
I ended up with a dark layer of (hopefully) MNT on top:
http://img384.imageshack.us/full.php?image=crude7gc.jpg

I dumped into an equavalent volume of water. The MNT lightened considerably. I poured it off, and then added some more water since some acid came over with it. It was now very light and so I am concerned I did not make pure MNT and still have toluene in it. There is still the strong MNT smell.
http://img355.imageshack.us/my.php?image=mnt1jw.jpg

So, did I succeed the second time? Is there an easy way to test, or can someone who has made it before tell from looking at it?

Thanks!

[nbk2000]

The fact that you got a non-water-soluble solid from a liquid and a water-soluble solid would seem pretty good indication that you have MNT.

Try melting a small portion in a test tube in a pan of water that's slowly heated. Note the temperature that the solid melts. That'll be a good proof of MNT if it melts at the reference temp (which I don't know off hand).

[Chris The Great]

Well I'm not concerned about my first try, that is definately nitrotoluenes! I was more concerned with my second attempt. Unfortuntely it has a very noticable toluene smell today :( I guess I shouldn't have added the water to the nitrating acids, and kept the temperature higher as myrol says.

I'd do a mp test but at the moment I lack a thermometer, because I broke my last one and haven't had a chance to get a new one yet.

[Guerilla]

There can't be much MNT's in your second batch judging from the density (it should sink to the bottom as an oily fluid, when added to water) and the low temperatures used. Just save your ice bath for a possible runaway and start adding the toluene somewhere at 40C (not before that) in small and equal portions (170ml/5min might be a bit too fast, even with the added water) a good rule of thumb for this is to not add any new toluene before the previous portion has reacted.

The first drops usually turn blood red immediately upon contact with the nitrating mix, a slight evolution of NOx is inevitable and should not be feared as long as the temp stays within reasonable limits. The acid concentrations for the first step can be very low so it's ok to dilute the acids (not during the nitration) somewhat for an easier temperature control and steadier reaction.

[APChemPayedOff]

Ok so im looking at the process and yes, i think we haf established it working....Umm a source would be wikipedia. Just search for TNT and it will give the nitration equation and everything u wanna know. But about the process, when you say heat to 80C for 30 minutes, does this mean start timing once u start immediately heating or once the mixture hits 80C u start timing? I know this might sound like a dumb question but i was jus wondering since its a pretty important part in the process cuz it is repeated about 3 times or so. Thanks for the response then.
EJ:cool:

[Nic-boleta]

Hi to all...
I hope you can help me in this question:

Normally,the TNT is obtained using the well known three-step method, but I have found in some webpages a text like this:

A terrorist, however, would probably opt for the less economical one step method. The one step process is performed by treating toluene with very strong (fuming) sulfuric acid. Then, the sulfated toluene is treated with very strong (fuming) nitric acid in an ice bath. Cold water is added the solution, and it is filtered.

Any idea on how to do this?

Thanks in advance...and greetings from Catalonia

[Bert]

The best way would be to UTFSE as several one step TNT procedures are discussed here. If you're lucky, you may not be kicked for what ammounts to a "spoon feeding" request. You've been a member close to 3 years... You should know better.

30 seconds of search effort would yield your answer. You owe me a mascletta...
http://www.sciencemadness.org/talk/viewthread.php?tid=29&page=3

The bit about using an ice bath show the author you quote's ignorance of the process he tries to describe, BTW.

[Charles Owlen Picket]

There has been a lot said about The Preparatory Manual of Explosives and the processes therein. The biggest issue I keep hearing about is that the processes don't match the patents they are supposedly extrapolated from.

Lagard has a 3rd edition out now. I suppose that those criticisms got him to proof his previous stuff. This ice issue may be to determine a starting point from which to time an upward advance of temp, etc. However I have read that and it is from the PME (the ice issue) it wasn't a typo as it occurred more than once.

@Nic-boleta; please direct questions on technique to the book "Advanced Practical Organic Chemistry", M. Casey, 1990. <damn nice book for techniques> Some people consider the use of expressions like "3 step" or
"1 step" when talking about nitrations to be misleading. It's a good book!

[Nic-boleta]

Thanks to Bert and Charles Owlen Picket for your help...
Now I must find the reactives I need (I know a chemical suppliers shop and perhaps I will find all I need there)