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Author Topic: TNT synthesis
radar
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Icon 1 posted October 05, 2001 03:20 PM      Profile for radar   Email radar   Send New Private Message       Edit/Delete Post 
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


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EventHorizon
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Icon 1 posted October 05, 2001 11:13 PM      Profile for EventHorizon   Email EventHorizon   Send New Private Message       Edit/Delete Post 
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
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CodeMason
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Icon 1 posted October 06, 2001 12:27 AM      Profile for CodeMason   Author's Homepage     Send New Private Message       Edit/Delete Post 
Where did you get the text?
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radar
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Icon 1 posted October 06, 2001 03:40 AM      Profile for radar   Email radar   Send New Private Message       Edit/Delete Post 
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.


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10fingers
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Icon 6 posted October 06, 2001 10:29 AM      Profile for 10fingers   Email 10fingers   Send New Private Message       Edit/Delete Post 
*

[ June 17, 2002, 02:49 PM: Message edited by: 10fingers ]

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Mr Cool
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Icon 1 posted October 06, 2001 01:50 PM      Profile for Mr Cool   Author's Homepage   Email Mr Cool   Send New Private Message       Edit/Delete Post 
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 .

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radar
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Icon 1 posted October 06, 2001 02:15 PM      Profile for radar   Email radar   Send New Private Message       Edit/Delete Post 
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.


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Mr Cool
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Icon 1 posted October 06, 2001 02:38 PM      Profile for Mr Cool   Author's Homepage   Email Mr Cool   Send New Private Message       Edit/Delete Post 
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.

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radar
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Icon 1 posted October 06, 2001 02:50 PM      Profile for radar   Email radar   Send New Private Message       Edit/Delete Post 
I dreamt up about 3 ounces with 100ml.
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CodeMason
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Icon 1 posted October 06, 2001 07:17 PM      Profile for CodeMason   Author's Homepage     Send New Private Message       Edit/Delete Post 
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.
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SafetyLast
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Icon 1 posted October 06, 2001 10:05 PM      Profile for SafetyLast   Email SafetyLast   Send New Private Message       Edit/Delete Post 
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.

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cutefix
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Icon 1 posted October 07, 2001 12:00 AM      Profile for cutefix     Send New Private Message       Edit/Delete Post 
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...
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radar
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Icon 1 posted October 07, 2001 03:49 AM      Profile for radar   Email radar   Send New Private Message       Edit/Delete Post 
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.
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radar
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Icon 1 posted October 07, 2001 03:51 AM      Profile for radar   Email radar   Send New Private Message       Edit/Delete Post 
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
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cutefix
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Icon 7 posted October 07, 2001 05:40 AM      Profile for cutefix     Send New Private Message       Edit/Delete Post 
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.

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Mr Cool
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Icon 1 posted October 07, 2001 06:50 AM      Profile for Mr Cool   Author's Homepage   Email Mr Cool   Send New Private Message       Edit/Delete Post 
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!

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radar
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Icon 1 posted October 07, 2001 07:41 AM      Profile for radar   Email radar   Send New Private Message       Edit/Delete Post 
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.
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CodeMason
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Icon 1 posted October 07, 2001 07:54 AM      Profile for CodeMason   Author's Homepage     Send New Private Message       Edit/Delete Post 
Picric doesn't even come close to PETN.
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a_bab
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Icon 1 posted October 07, 2001 03:27 PM      Profile for a_bab   Email a_bab   Send New Private Message       Edit/Delete Post 
Not even in color....

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

http://move.to/pyromania


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VasiaPupkin
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Icon 1 posted October 07, 2001 03:40 PM      Profile for VasiaPupkin   Email VasiaPupkin   Send New Private Message       Edit/Delete Post 
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.
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EventHorizon
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Icon 1 posted October 07, 2001 10:55 PM      Profile for EventHorizon   Email EventHorizon   Send New Private Message       Edit/Delete Post 
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.

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


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radar
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Icon 1 posted October 08, 2001 08:34 AM      Profile for radar   Email radar   Send New Private Message       Edit/Delete Post 
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.
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wantsomfet
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Icon 1 posted October 08, 2001 09:39 AM      Profile for wantsomfet   Author's Homepage   Email wantsomfet   Send New Private Message       Edit/Delete Post 
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...

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radar
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Icon 1 posted October 14, 2001 04:02 PM      Profile for radar   Email radar   Send New Private Message       Edit/Delete Post 
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.
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SofaKing
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Icon 1 posted October 18, 2001 08:58 AM      Profile for SofaKing   Author's Homepage   Email SofaKing   Send New Private Message       Edit/Delete Post 
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.

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With Knowledge we find Truth - With Truth we find Freedom


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radar
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Icon 1 posted October 18, 2001 10:29 AM      Profile for radar   Email radar   Send New Private Message       Edit/Delete Post 
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.
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rc
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Icon 2 posted June 17, 2002 02:07 PM      Profile for rc   Email rc   Send New Private Message       Edit/Delete Post 
sorry to bring up an old topic, but i didn't feel like starting a new one, sorry again=)

anyway's the question is:

can you succesfully use nh4no3+a lot of sulfuric acid instead of the nitric acid?

i mean something like this:

100ml toluen
350g. ammonium nitrate
450ml. sulfuric acid(98%)

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PYREX
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Icon 1 posted June 17, 2002 03:14 PM      Profile for PYREX   Email PYREX   Send New Private Message       Edit/Delete Post 
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".

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Burn motherfucker.

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Madog555
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Icon 1 posted June 17, 2002 03:22 PM      Profile for Madog555   Author's Homepage   Email Madog555   Send New Private Message       Edit/Delete Post 
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

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Most people outgrow their pyro tendencies, we are the ones whose tendencies outgrew us.

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BrAiNFeVeR
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Icon 1 posted June 17, 2002 03:44 PM      Profile for BrAiNFeVeR   Author's Homepage     Send New Private Message       Edit/Delete Post 
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 ...

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Madog555
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Icon 1 posted June 17, 2002 06:21 PM      Profile for Madog555   Author's Homepage   Email Madog555   Send New Private Message       Edit/Delete Post 
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.

[ June 19, 2002, 06:01 PM: Message edited by: Madog555 ]

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Most people outgrow their pyro tendencies, we are the ones whose tendencies outgrew us.

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nitriees
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Icon 1 posted June 19, 2002 01:22 AM      Profile for nitriees   Author's Homepage   Email nitriees   Send New Private Message       Edit/Delete Post 
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?

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nitriees

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kingspaz
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Icon 1 posted June 19, 2002 04:50 PM      Profile for kingspaz   Email kingspaz   Send New Private Message       Edit/Delete Post 
the water in lower concentrations of HNO3 would decompose the HDN.

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Madog555
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Icon 1 posted June 19, 2002 05:17 PM      Profile for Madog555   Author's Homepage   Email Madog555   Send New Private Message       Edit/Delete Post 
you need a good concentration for HDN to RDX. people use HDN because you dont need as mutch HNO3 and the yield is better.

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cutefix
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Icon 1 posted June 19, 2002 09:59 PM      Profile for cutefix     Send New Private Message       Edit/Delete Post 
Qoute:
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TNT can be synthesis by multi-step nitration with low conc. HNO3,
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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. [Smile]

[ June 19, 2002, 10:01 PM: Message edited by: cutefix ]

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Madog555
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Icon 1 posted June 19, 2002 10:54 PM      Profile for Madog555   Author's Homepage   Email Madog555   Send New Private Message       Edit/Delete Post 
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.

[ June 20, 2002, 01:05 PM: Message edited by: Madog555 ]

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Icon 6 posted June 19, 2002 10:56 PM      Profile for 10fingers   Email 10fingers   Send New Private Message       Edit/Delete Post 
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?
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nitriees
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Icon 1 posted June 20, 2002 09:24 PM      Profile for nitriees   Author's Homepage   Email nitriees   Send New Private Message       Edit/Delete Post 
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.

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nitriees

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cutefix
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Icon 7 posted June 20, 2002 10:44 PM      Profile for cutefix     Send New Private Message       Edit/Delete Post 
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? [Big Grin]

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.

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Icon 1 posted June 21, 2002 09:43 AM      Profile for mr.evil   Author's Homepage   Email mr.evil   Send New Private Message       Edit/Delete Post 
quote:
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".

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?

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cutefix
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Icon 1 posted June 25, 2002 02:25 AM      Profile for cutefix     Send New Private Message       Edit/Delete Post 
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...

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da man
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Icon 15 posted June 25, 2002 06:10 AM      Profile for da man   Email da man   Send New Private Message       Edit/Delete Post 
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?

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cutefix
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Icon 1 posted June 25, 2002 04:39 PM      Profile for cutefix     Send New Private Message       Edit/Delete Post 
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.

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Icon 7 posted June 28, 2002 03:46 AM      Profile for mr.evil   Author's Homepage   Email mr.evil   Send New Private Message       Edit/Delete Post 
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! [Smile]

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...


http://www.geocities.com/tshadowpp/MNT.html?1025250302490

Edit: some spelling errors

Cya

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

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Icon 18 posted June 30, 2002 07:49 AM      Profile for mr.evil   Author's Homepage   Email mr.evil   Send New Private Message       Edit/Delete Post 
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 [Roll Eyes]

By the way,
my lab stinks like Almond now, Yak! [Razz]

Edit: some spelling mistakes

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andreas
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Icon 5 posted July 19, 2002 07:05 AM      Profile for andreas   Author's Homepage     Send New Private Message       Edit/Delete Post 
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.
http://www.boomspeed.com/kramrak/tnt1.JPG http://www.boomspeed.com/kramrak/tnt2.JPG http://www.boomspeed.com/kramrak/tnt3.JPG
I think I stepped a step in the synthesis and went almost directly to tnt

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Mr Cool
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Icon 1 posted July 19, 2002 07:18 AM      Profile for Mr Cool   Author's Homepage   Email Mr Cool   Send New Private Message       Edit/Delete Post 
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...

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nbk2000
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Icon 1 posted July 19, 2002 09:42 AM      Profile for nbk2000   Email nbk2000   Send New Private Message       Edit/Delete Post 
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.

 -

[ July 19, 2002, 09:46 AM: Message edited by: nbk2000 ]

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andreas
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Icon 1 posted July 20, 2002 08:44 PM      Profile for andreas   Author's Homepage     Send New Private Message       Edit/Delete Post 
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

[ July 20, 2002, 08:49 PM: Message edited by: andreas ]

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Icon 1 posted July 23, 2002 05:14 AM      Profile for Einstein   Email Einstein   Send New Private Message       Edit/Delete Post 
I'm dreaming to make some TNT after I will get my lab apparatus. I'm going to distill some car battery acid (37% -> 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 [Big Grin]

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.

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Icon 1 posted July 23, 2002 06:52 AM      Profile for rikkitikkitavi   Email rikkitikkitavi   Send New Private Message       Edit/Delete Post 
68,3 % by weight.

/rickard

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Einstein
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Icon 5 posted July 25, 2002 11:32 AM      Profile for Einstein   Email Einstein   Send New Private Message       Edit/Delete Post 
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 [Big Grin]

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Icon 1 posted July 25, 2002 11:51 AM      Profile for ALENGOSVIG1   Email ALENGOSVIG1   Send New Private Message       Edit/Delete Post 
Considering the amount of acids that are needed to nitrate the toluene 3 times, the yeilds arent that good.

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nbk2000
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Icon 2 posted July 25, 2002 03:08 PM      Profile for nbk2000   Email nbk2000   Send New Private Message       Edit/Delete Post 
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.

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The knowledge that they fear is a weapon to be used against them.

Download the RTPB from here. Change .txt to .pdf to read with Adobe Acrobat.

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Icon 1 posted July 25, 2002 03:26 PM      Profile for spydamonkee   Email spydamonkee   Send New Private Message       Edit/Delete Post 
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?

[ July 25, 2002, 03:43 PM: Message edited by: spydamonkee ]

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Icon 2 posted July 28, 2002 11:35 AM      Profile for Einstein   Email Einstein   Send New Private Message       Edit/Delete Post 
I forgot to post link to my TNT calculations...everyone can understand it, but the text is only readible for Finnish guys... TNT calculations

[ July 28, 2002, 11:37 AM: Message edited by: Einstein ]

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