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Author: Subject: Trinitrotoluene preparation
dann2
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[*] posted on 31-7-2009 at 16:29



Jared Jedgard's an asshole (excuse my french as we say around here). All and everything he writes should be ignored. Nitrate the book.
Dann2
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chloric1
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[*] posted on 31-7-2009 at 17:25


@Dann

Wow, it sounds like your disregard for Jared is personal. I thought his stuff was rather suspect and I sent him an email asking if he tried to make anything he wrote about. He briskly said he did and they worked without and further explanation or evidence. One thing that really begs skeptism his lack of references. IRC most of his proceedures are from patents and he does not even state which ones they are. I believe he is just a lack luster chem grad who knew enough to B.S. the sheeple into buying his books.



[Edited on 8/1/2009 by chloric1]




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dann2
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[*] posted on 1-8-2009 at 02:07


Hello,
Never actually purchased the book so it's not THAT personal :P First came accross it on Google when I was looking for something about Chorates etc (my hobby horse).
My favourite is his little ditty regarding Ammonium Chlorate (extremly sensitive, unstable, unusable stuff).
This guy wants to see people loose their bits, or worse. Where on earth did he get the information below? It must surly be making it up off the top of his head after getting well 'jared up' (stoned) ,when he writes his wise words of wisdom. He has a number of books in print.
Going off topic a bit.......
Dann2

jl.JPG - 65kB


[Edited on 1-8-2009 by dann2]
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chloric1
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[*] posted on 1-8-2009 at 06:20


Man alive! Total misrepresentation! You consult the literature of even the turn of the last century you hear many accounts of ammonium chlorate spontaneously exploding. If no explosion then the salt is decomposed in a matter of weeks. Not hardly stable. Secondly, ALL chlorates are at least moderately toxic, definately more so than perchlorates. If I where to use this salt it would only be in solution and it will only be to prepare Ba or Sr chlorate free from K or Na.

But the most shocking was the statement about mixing with chromates, dichromates etc. What a nut job!

[Edited on 8/1/2009 by chloric1]




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argyrium
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[*] posted on 1-8-2009 at 10:53
further afield, yet.


in addition to the incredibly dangerous compatibility allegations, the remarkably novel approach used by Mr. Jedgard to produce NH4ClO3 from NH4OH/NH3 + CO2 should further dispel any credulity in his writing. Pretty frightening.
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[*] posted on 1-8-2009 at 11:02


Quote: Originally posted by dann2  
Hello,
Never actually purchased the book so it's not THAT personal :P First came accross it on Google when I was looking for something about Chorates etc (my hobby horse).
My favourite is his little ditty regarding Ammonium Chlorate (extremly sensitive, unstable, unusable stuff).
This guy wants to see people loose their bits, or worse. Where on earth did he get the information below? It must surly be making it up off the top of his head after getting well 'jared up' (stoned) ,when he writes his wise words of wisdom. He has a number of books in print.
Going off topic a bit.......
Dann2


"It is relatively stable".

This is more material for worst books thread. I've also noticed he used a copy and paste ChemSketch values for density of energetics even where the density is known and easily looked up in something like Federoff or even Meyer and Koehler.

[Edited on 1-8-2009 by Formatik]
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[*] posted on 22-2-2010 at 08:17


Sorry to bring up an old thread, but I didnt want to start a new one as this question is more or less suited for this theme.

I am now making some DNT from MNT, H2SO4 and NH4NO3.
When the reaction is finished I will dilute the mix with water and filter out the DNT. So could I neutralize the DNT with simple water and NaHCO3 washes or is it done some other way?

Edit:
Well my attempt at making DNT failed.

170 ml of conc. H2SO4 (lab grade), 90 g of NH4NO3 (contaminated with approx. 4-5% magnesium nitrate) and 114 g of MNT were mixed and heated in a steam bath for 2 h. Then after it cooled I crashed the mix in cold water. A lot of liquid immediatley settled on the bottom of the beaker, and most of the water layer turned white, as some fine powder was dispersed in it. The upper cm or so of the water layer is transparent. I will let it stand over night. Perhaps the liquid soldifies as I heared that DNT if impure can take some time to soldify :)

[Edited on 22-2-2010 by Zinc]




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[*] posted on 22-2-2010 at 13:49


Contaminating your synthesis with foreign materials makes deduction of what went wrong pretty tough.

Always mix to a clear solution your solid nitrates, making sure that the process is a slow one and that the materials are KEPT COOL (refrigerate all acids maintaining at least 10C) until use in synthesis demands a higher temp. Crude DNT solidifies in needle crystalline shapes very similar to TNT However when washed DNT will retain a yellow where the majority of TNT looks similar to light brown sugar. Continually check your temps. TNT or DNT % are sensitive to temp variations.
DNT will often have a percentage of TNT and visa versa thus you will often have what is commonly called "TNT oil". This washes off with dilute H2SO4 & sodium sulfite. Alkalies often sensitize nitrated toluene. The common "1 or 2-pot synthesis" will pretty much guarantee some DNT.

Read "Plant-Level" TNT production techniques. They often can clarify what in a minor scale, went wrong. Check Davis (pp 141-) and familiarize yourself with the "rule of Crum Brown". Most everything you need is in there.



[Edited on 22-2-2010 by quicksilver]
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[*] posted on 23-2-2010 at 07:05


Tahnk you for the advice.

Well the experiment worked acutaly. Today I checked it and the DNT soldified to a nice yellow mass. I will recristalise it to obtain a powder (the solid mass cant be washed as most of the DNt wont be exposed to the washing solution).




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[*] posted on 23-2-2010 at 12:32
here's a visual comparison


Here you'll see needles of crude TNT and a comparison of DNT to TNT.
Depending upon temp control you can grow needles of TNT up to 3.5cm in length. note the "oil" in crude DNT. This exists in most any crude nitrated toluene. The addition of ammonium nitrate during WWII diminished this (and from getting aircraft maintenance personnel from getting sick.

comparison2.jpg - 64kBneedles2.jpg - 24kB
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[*] posted on 14-3-2010 at 02:31


Well I still havent recryctalised my DNT (didnt have enough time:()

I was thinking, could the DNT be recrystalised by disolving it in hot acetone, and then crashing it in a NaHCO3 solution to neutralize the remaining acid (I know that wont make nice big crystals, but I dont want them, I want powder)?




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[*] posted on 11-4-2010 at 14:01


Hi,
I know this question doesn´t fit here perfectly, but I didn´t want to open a new topic.
I successfully made around 90g of TNT and now I want to test some compositions containing TNT.
One is torpex (42% RDX, 40% TNT, 18% Al, cast), but I don´t know how much PETN/EGDN/Nc is necessary as booster.
Will 5g do the job (I want to use as little as possible, but as much as necessary for a proper detonation, because I will test only 30-50 grams, and don´t want a 100g booster for setting off a 30g charge...) ?
Another explosive I want to try ist cyclotol, same problem.

Thanks for reply, crossbow

[Edited on 11-4-2010 by crossbow39]
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hissingnoise
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[*] posted on 11-4-2010 at 14:24


You have these several compounds in your possession and know nothing of their sensitiveness?
Isn't that strange!

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[*] posted on 12-4-2010 at 05:22


Of course a 100g booster is an exaggeration, but you know what I mean.
RDX isn´t easy to detonate at high density, so is TNT, especially when cast.
So my question is, will 5g of a HE booster suffice for a small charge?
Thanks, crossbow
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[*] posted on 12-4-2010 at 07:22


Quote:
[rquote]Of course a 100g booster is an exaggeration.

So's 5 grams!
TNT, pressed in a detonator capsule is reliably detonated by 0.35g Hg(ONC)2.
Torpex is more sensitive than TNT due to its RDX content and the plastic mixture PETN/EGDN/NC is more powerful and more brisant than C4.



[Edited on 12-4-2010 by hissingnoise]
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[*] posted on 28-12-2010 at 04:02


Sorry to bring up an old thread, but I didn't want to start a new one.

I tried to make nitrotoluene (130 g of AN, 175 ml conc. H2SO4 made by boiling old battery acid and 116 ml of toluene). After mixing the AN and H2SO4 I added the toluene but the reaction didn't want to start so I heated it to cca. 60-70 C. After something like 30 min on that temp I let it to cool down overnight and after that diluted it with 600 ml of water. The toluene is now almost clear-yellow, it floats on water and the smell of nitrotoluene is barely noticeable. It seems that toluene didn't nitrate completely, so could I attempt to nitrate that toluene again, or would it be better to start with fresh toluene?

[Edited on 28-12-2010 by Zinc]




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[*] posted on 28-12-2010 at 07:13


This was (used to be) a common classroom exercise. Kitchen chemistry won't cut the mustard with TNT, TNA, TNB, TXT, etc. The best of mixed acids and excellent temp control makes it a wonderful demonstration in refining one's ability to control conditions. Boiling down H2SO4 is generally used to bring it up a few % and to knock out any contaminants; not to start cold. It could clean up sulfuric acid drain opener becasue that is often used in pickling (metals) and anodizing so that the garbage drops to the bottom of the flask.
Nitrating benzene ring materials are about as "safe"as nitration get. baring fumes and some real jocular stupidity one has to seriously screw up to loose the entire upper half of one's body; but it's happened. I have seen needles grown as long as two full inches but the temp control and time must be monitored with professional accuracy.
The group is also known for it's toxicity. The old bomb loaders on fixed wing aircraft used to ware leather gloves which absorbed what was known as "TNT-oil" and both liver and skin cancer was the result.




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[*] posted on 13-8-2011 at 10:18


Just experienced the stranges thing...


I've never made TNT before, so together with a friend of mine we gave the 3 step synthesis a try.

We started off producing mononitrotoluene, after washing and heating the isolated mononitrotoluene at 100 deg C for 15 minutes, lightly yellow coloured oil, density 1.14. So far so good.
Next step dinitrotoluene: mononitrotoluene was added to mixed acids 70% nitric and 97% sulfuric, after slight exotherm at the beginning was heated for 1.5 hours at 90 deg C. Dinitrotoluene was allowed to separate on top of the mixed acids, and pipetted off into 90 deg. hotwater + bicarb, washed and allowed to cool down. It settled at the bottom of the beaker as as solid, melting point approx. 65 deg, density 1.35.

Finally, 1 part 97% Nitric and 2 parts 97% H2SO4 were added at once, the mixture heated up to 50 degrees celcius. The dinitrotoluene was added and the whole mix was refluxed at 100 deg. C. for 2 hours with stirring.

Now the strange part: Whereas the dinitrotoluene was a solid, the resulting oil after the final nitration was a liquid, even at room temperature. I checked density of the resulting oil, and it was 1.46. It is a pale yellow viscous oil, but very milky. After heating to 150 deg. C, it burns with quite yellow luminous soothy flame.

EDIT: It is starting to crystallize now, probably strange eutectic of DNT/TNT. It is unlikely though MNT would still be present. How could I be sure?

EDIT2: Any ways for purification without sodium sulphite?

[Edited on 13-8-2011 by nitro-genes]
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[*] posted on 13-8-2011 at 16:32


12 (!) consecutive washings with boiling water later, melting point has gone up to 73-76 deg C, density 1.53. I lost about 12% of the crude TNT in the process, the yellow wash water turns bright red/brownish with ammonia. The cast end product still has a faint smell of NOx and has become roasted-almond-brown . Amazing how difficult it seems to wash all acid out of the TNT. :-)

[Edited on 14-8-2011 by nitro-genes]
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[*] posted on 14-8-2011 at 07:25


Best to avoid a strong base with TNT as it sensitizes it. Sodium sulfite wash in fairly warm (50C+) water will bet it done. product will be a light beige crystalline. Davis for details.



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[*] posted on 14-8-2011 at 09:04


Yes, I only washed the crude TNT with boiling water, but tested the light yellow wash water with ammonia, it runs a deep brown/red immediately. :) I don't have any sodium sulfite, for washing. Is there some solvent from which TNT will crystallize more easily than DNT and.or other unwanted isomers?

[Edited on 14-8-2011 by nitro-genes]
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[*] posted on 14-8-2011 at 12:31


Shot in the dark, it would be an industry oriented question during war-time or areas where production facilities are not highly funded. I am not sure on this as I have read so many patents on TNT that I really don't remember many but ethyl acetate or acetone might separate your crude nitrated material. Conflict-period patents for UK & USA patents would be an easy find.

I don't have my scans and digital material separated but if you hunt down (via patent searches) something like "TNT, acetone" or "TNT, polar - non-polar solvents" you might find just what you are looking for ( around 1939-1941). In large batch industry, the issue at one time was very common as various methods of production yielded very crude end product. The pictures (above show a near white needle that cleaned up similar to lightly colored "brown sugar" colored material where the lower nitrated heavy crystals had at least 30% DNT (via another acid and sulfite wash). The "steam" method was a very common one also as tri-nitrated material melts at 70C or something close where the lower nitrated materials always run higher.

Your hot water most likely put both into one one: that why your "brown color" was deep. Had you some method to control the heat (steam manipulation, etc) you may have been able to see a separation.




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[*] posted on 14-8-2011 at 13:23


Thanks quicksilver I have found some interesting patents, but how about ethanol? Supposedly DNT's are more soluble in ethanol than TNT at RT. I'll give it a try..:)
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[*] posted on 15-8-2011 at 06:02


Above 50 C, it's quite possible, however I don't know for certain. I'm frankly putting out ideas as I haven't had a chance to really narrow it down either- but I know you won't have a serious problem doing so. What we are discussing is a common industrial issue. My guess is that cost containment, ease of use and common availability will win the day. Now that we're talking about it, I'll bet I find just the right one and if so; I'll post it up here.



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[*] posted on 16-12-2011 at 10:14


i thought it was a little daring to add 99% nitric acid to gasoline my self i agree....i wouldnt do it
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