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Author: Subject: Trinitrotoluene preparation
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thumbdown.gif posted on 3-5-2005 at 11:30


finally the reaction is over. the results are really bad. the liquide seperated in the warter trap was the mainly the nitric acid from the begining wich evaporated during the process. the main product seems to be a mixture of MNT and DNT. not even a half tea spoon full of TNT was swiming on top of the liquid. i used 40ml toluene, 180ml 53% nitric acid and 200ml hexane. the setup has been run for approx 8h. may be hexane is not a suitable solvent for this reaction. the patent recommends lite gasoline but i'm not sure whats meant with lite gasoline.
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[*] posted on 4-5-2005 at 01:21


Did you measure the temperature? Don't take it above 80°C... what did you use as watertrap, something like MgSO4?

I cannot find the topic of NBK now, it is probably not cached by google...




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[*] posted on 5-5-2005 at 03:21


the temperature was at 70°C the whole process because the hexane limits the reaaction temperature to it's boiling point. the wartertrap is not a chemical just a part of the still. the condensate (should be warter and hexane) from the reflux cooler drips in the wartertrap and divides in two phases because of it's different density and it's inmiscibility.
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[*] posted on 5-5-2005 at 04:04


That temperature is about right, I was worried that it could be too high, since you have a mixture of 2 organic solvents, the temp could do strange things...

Anyway, I don't know or you've got more time on your hands, but maybe you have give it a shot by refreshing you nitric, and do the nitration agian on the mixture you're left with.
Don't you have any NA at a higher conc than 52%, maybe that might improve.
Please remember that TNT is normally made by reacting DNT with 100% HNO3 in the present of a lot of sulphuric, the concentration of the nitronium ion must be rather strong to get the last NO2 attached.

Keep the good work going!

[Edited on 5-5-2005 by Taaie-Neuskoek]




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[*] posted on 5-5-2005 at 10:58


i have 68% nitric too but i want to use the 53% because it's easyer to get. if the patent is rigt the concentration should not play an important role because the warter should be removed during the process until the concentration is high enough for the nitration. i think the problem is that not only the warter collects in the trap but also the nitric do.
i still have some cyclohexane may be i give it a second try with this. has anyone an idea for an other suiteble solvent wich boils in the range of 70-80°c, forms an azetrop with warter an is innert to nitric acis at this temperatures?
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[*] posted on 13-5-2005 at 13:25


I have been thinking about and working towards a method of removing water from a nitration using my dean-stark trap.
I am looking for a water azeotrope that meets the following criteria:

(1) Based on the experiences of someone from the E&W Forum who used cyclohexane (bp 80 degC) to form the azeotrope and experienced the formation of excessive NO2.

The solvent must have a boiling point less than about 76 C.

(2) The solvent must be inert toward NO2, HNO3, sulfuric acid, and air under reflux.
This means that you cant use alkenes, alcohols, esters (are in equlibrium with the alcohol) , or ethers (form peroxides with air).

My first thought was to use n-hexane because it has a bp of 68.7 C and forms an azeotrope with water bp 61 C.
Then I read an MSDS that stated that n-hexane explodes when mixed with NO2 at 36 deg C!! IIRC. I understand that almost anything combustible will explode if mixed with NO2 and exposed to the shock of a detonator, or perhaps to a flame, but at room temperature?.
The idea that NO2 from decomposing nitric could mix with the hexane and explode makes me worry.

Now, carbon tetrachloride (bp 76.4 C) is most likley inert and forms an azeotrope with water bp 66.8 C that contains 4.1% water. However, 75 C is probably to hot, and will probably decompose to much nitric. Also, CCl4 is heavier than water and will require a different and hard to find type of water trap.

Chloroform (bp 61 C) also forms an azeotrope with water bp 56.1 C but it only contains 2.8% water, is denser than water, and might not be inert.

THF is hard to get ahold of, and forms peroxides in air.
My hope is that the MSDS was wrong about the hexane and NO2.
(If I got a dollar from every inaccuracy I have found in an MSDS I would probably have a lot more lab equipment. )
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[*] posted on 13-5-2005 at 15:07


Maybe trichloroethylene , bp 86.9 C would be a good candidate solvent . It is or was a commonly available nonflammable degreaser and cleaning solvent . I can't recall if it is one of those solvents which has fallen out of common use because of environmental regulations or not , but I think it is still available OTC , and may even be the solvent which they use in those recirculating bath " parts washers "
at automotive shops .

You can govern the reflux temperature lower if needed by pulling a little bit of regulated vacuum on the apparatus .

[Edited on 13-5-2005 by Rosco Bodine]
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[*] posted on 13-5-2005 at 16:44


I have my doubts that trichloroethylene is suitable, though it is still OTC (or was a couple of years ago, when I last bought some). I bought it to attempt hydrolysis via H2SO4, which was an older industrial process to monochloroacetic acid. I had some partial success but haven't tried anything more in a long time due to shuffled priorities and pure forgetfulness. It is not entirely inert to acids, that is sure. I suppose it depends somewhat on temperature and concentration, but I'd be wary.



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Rosco Bodine
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[*] posted on 13-5-2005 at 21:51


Chloroform looks like it should work the best among the other choices of chlorinated solvents . And it is stable in contact with concentrated acids .

Nitric acid is four times as soluble in the chloroform as in carbon tet . And you likely won't find or make carbon tet . It is pretty much gone the way of carbon disulfide , disappeared for the most part from commercial use and availability .
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[*] posted on 13-6-2006 at 06:47


Quote:
Originally posted by trinitrotoluene
No i dont think low concentration acids will work. I've heard that its very dificult to get the Mono form with low concentration acids.


I know this is a VERY old thread but I wanted to add that both TNT and PETN may be produced by lower concentrations of acid than what one would normally expect (distilled HNO3, etc). I guess I have seen time and again that 70% HNO3 could not be used or that mixed solid nitrates could not be used for both benzene ring nitrations and nitric estors, that I wanted to post an example or two.

**************
for TNT synth:
**************
Trinitrotoluene - single batch method.
Yield is approx. 85% of theory, crude product.
Patent supports the only singe batch method in current usage.

NOTE: alkaline (sodium hydroxide) will sensitize TNT, Sodium Sulfite is used to bring the crude product to a technical chemical level. The product below is some rather crude stuff but MAY be brought up to higher purity level. However the end result will work.

Procedure: Place 191 grams of 70% nitric acid into a beaker, and then gradually
add over a period of 2 hours, 420 grams of 98% sulfuric acid. (Total; 611gr of
mixed acid) Then place the beaker into a cold-water bath and cool to 10 to 15
Celsius. When the acid mixture reaches a temperature of about 10 to 15 Celsius,
pour 96 milliliters of this acid mixture into a clean separate beaker, and then
cool to 10 to 15 Celsius by means of a cold water bath. When the temperature of
this 96-milliliter portion of acid mixture reaches 10 to 15 Celsius, slowly add
46 grams of toluene over a period of 4 hours while rapidly stirring the acid
mixture and maintaining its temperature at 10 to 15 Celsius. After the addition
of the toluene, continue stirring the reaction mixture for an additional 2 hours
while keeping the reaction temperature at 10 to 15 Celsius. After which, add the
remaining acid mixture obtained at the start of the procedure, to the reaction
mixture and then after the addition, raise the temperature of the reaction
mixture to 70 Celsius, and hold this temperature while rapidly stirring the
reaction mixture for 2 hours. After 2 hours, raise the temperature to 80
Celsius, and heat at 80 Celsius for 2 hours while rapidly stirring the reaction
mixture. After heating the reaction mixture to 80 Celsius for 2 hours, remove
the heat source, and allow the reaction mixture to cool to room temperature.
Then add the entire reaction mixture to 1000 milliliters of cold water, and then
filter-off the precipitated TNT product. After which, wash the TNT precipitate
with 1000 milliliters of water, and then vacuum dry or air-dry the TNT
precipitate. Then, place 400 grams of 70% sulfuric acid into a beaker, and then
add the dry TNT product. Afterwards, stir the mixture to form a slurry. Continue
to stir the slurry for 2 hours at room temperature, and then filter-off the TNT
product, wash with 1000 milliliters of cold water, and then vacuum dry or air
-dry the TNT product

Extrapolated from Legard's book and one of the FEW patents that could actually be varified :P IIRC it was a guy working for ISCC who developed it.


***********
for PETN synth
***********
Verified efficient method of preparing PETN from diluted HNO3

use
32,7 ml of 70% HNO3 (75% excess)
18,9 ml of 96% H2SO4
10,0 g of Pentaerythrite
------------------------

or
34,0 ml of 65% HNO3 (66% excess)
24,8 ml of 96% H2SO4
10,0 g of Pentaerythrite
------------------------

or
34,8 ml of 58% HNO3 (48% excess)
36,3 ml of 96% H2SO4
10,0 g of Pentaerythrite
------------------------


Nitration:
1. Cool nitration mixture during mixing of acids, thus minimalize even minimal decomposition of HNO3. Nitration mixture must be cooled before nitration process to temperature of 10°C.
2. While stiring, add pentaerythritee in small portions (1-2g) to nitration mixture, always after previous batch is dissolved. Nitration mixture gradually thicken as PETN forming in solution.
3. Constantly monitor reaction temperature and maintain it in 10-15°C range. Interval of adding pentaerytritol conform to reaction temperature, must not rise over 15°C, leave beaker in cold water.
4. Stir with mixture for next 5 minutes after all pentaerythrite is added and dissolved. Mixture is now thick, but stirring is going well. During nitration process must not be developed any brown fumes of NOx!
5. Now put beaker with mixture into water bath and maintain temperature at 50°C, continuously stir with mixture. During 20 minutes at this temperature, all of possible sulfoesters come into PETN for maximal yield of nitration.
6. While maintaining mixture at higher temperature, mixture must be monitored for developing of NOx fumes. Only light brown colour can be in shrouded beaker. Raised development of NOx pointing to higher temperatures used (even during previous nitration) or insufficient chmemicals purity and further heating may end up in uncontrolled reaction and oxidation of formed PETN. In this case it is better to do not heat at all and end just after nitration (if brown fumes apperas during nitration), the yield will be lower. In case of accidentally runaway reaction during heating, immedialtely pour mixture into cold water, don't try stop reaction by cooling beaker, it will not help.
7. When heating after 20 minutes pass off, pour reaction mixture into cold water and follow standart procedure of filtration, neutralization and purifying of PETN.

Yield was 22,1g of PETN from 10g of pentaerythrite, ~95% of theoretical yield (with 65% HNO3 used).

This procedure is result of research of most effective method preparing PETN from diluted HNO3. Acid ratios are precisely calculated on data from PETN nitration graph published by T. Urbanski in his book vol. IV. Look at the graph from the FTP and it makes a great deal of sense. Generaly said, PETN is forming to maximum 30% of water portion in nitration mixture. But, when also H2SO4 is contained in nitration mixture, minimum amount of water must be keep, or oxidation with small yields occur. With this acid ratios 20% of H2O is minimum. So, this nitration mixture has 20% of water on nitration start and 30% at the end, area for most effective nitration, but again only with this ratios. For other acid ratios must be all recalculated. Excess of HNO3 is used to controll amount of reaction water. Only amount of nitration mixture can be extended for lower mixture thickness, but it lower utilization of acids and overall efficiency. But it isn't necessary.


-=-=-=-=-=-
The TNT synth is somewhat scaleable - the PETN is not due to the above stated issues. (both of these have been floating around for a few years, I believe)





[Edited on 14-6-2006 by quicksilver]




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[*] posted on 2-7-2006 at 17:42


@quicksilver

Quote:

"Extrapolated from Legard's book and one of the FEW patents that could actually be varified IIRC it was a guy working for ISCC who developed it."


What is the patent number ?
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[*] posted on 3-7-2006 at 11:50


The stepwise nitration of toluene

Journal of chemical education


article online


http://www.jce.divched.org/cgi-bin/JCE/jce-idx.pl?type=goto&...
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[*] posted on 3-7-2006 at 12:08


Do not sneeze during the process or the entire sample
will be gone with the wind :P


Here is a good reaction vessel for microtek ;)


http://cgi.ebay.com/Large-reactor_W0QQitemZ110003787509QQihZ...
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[*] posted on 3-7-2006 at 13:09


Rosco,

I have the second edition of Jared Ledgard's book,
"The Preparatory Manual of Explosives" in front of me,
which I assume is the book Quicksilver extrapolated the synthesis from, which is located in chapter 11 of that book and NO PATENT NUMBER IS GIVEN. At least not in the edition I have.

As for the nitration to tnt in a "single pot" reaction starting from toluene without the further addition of concentrated acids it just doesn't seem the reaction kenetics are very favorable or economical which is why it seems in the literature it's done in a three step process.

However the conditions for a "one pot" synthesis of TNT directly from toluene may be more easily accomplished if a different nitration agent than nitric acid is used. For example Tetranitromethane in the presence of boric acid or nitrogen pentoxide added directly to toluene. They may be more costly than mixed acids, but may also prove to be greater nitraters when starting from toluene in a single step process or in first sulfonating the toluene, then substituting the nitro groups for the sulfonic groups in a two step process.

Note: see Urbanski Volume I, page 390

[Edited on 3-7-2006 by Sickman]
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[*] posted on 3-7-2006 at 15:47


Here is an old patent which relates to nitration catalysts
which may have some usefulness regarding TNT as well as other nitroaromatics . I have not done any experiments regarding the patent , but the procedure for tetranitronaphthalene is on my " experiments to do list " . Vanadium phosphate is one of the catalysts which I would look at . The TNN would likely make a good stable base charge for caps and is a bit more powerful and sensitive than TNT , about like picric acid but non-corrosive , has a good crystalline form and doesn't have the purification / separation problems of TNT . The patents mention of even higher penta and hexa nitro forms of naphthalene is also interesting , as well as the obscure primary initiating composition which may be formed from the hexanitronaphthalene in combination with an oxidizer . This is an intriguing old patent which may or may not withstand scrutiny . In fact it was the first patent which I communicated here in this forum as being " interesting " :D in its implications . You see if the nitration catalysts do
work as advertised , then higher nitrations of aromatics can be performed under less rigorous conditions for acid concentration and temperature which would be very helpful
for our purposes .

Attachment: GB501034 nitration catalysts.pdf (212kB)
This file has been downloaded 1097 times

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[*] posted on 22-7-2006 at 16:44


@quicksilver

I knew that TNT synthesis looked familiar

It was posted here nearly three years ago
by a one time poster . Strange huh ?

https://sciencemadness.org/talk/viewthread.php?tid=943#pid85...

You mentioned the ISCC ......what is that ?

BTW , WTF is the USASDDS , anybody have a clue ?


[Edited on 23-7-2006 by Rosco Bodine]
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[*] posted on 24-7-2006 at 06:34


Quote:
Originally posted by Rosco Bodine
@quicksilver

I knew that TNT synthesis looked familiar


You mentioned the ISCC ......what is that ?

BTW , WTF is the USASDDS , anybody have a clue ?




OK....I F*cked up there. That was a typo and a hurried job of typing when I was running out the door for work. What I thought was a file from a collection of ISEE stuff (International Society of Explosive Engeneers) was simply another file from Legard's book, it wasn't the correct file - The typo was ISCC. I spent sometime tracking down what the existing citations in that damn book were. Some lead simply no-where - others had some interesting origins but I also have one unholy collection of files and need some way to organize them better. I didn't notice the whole thing until it had been posted quite awhile. - appologies....:(

What I looked for at the time was some US Gov't patents issued to a "H. William Voigt, Jr". of Wharton, NJ and a Mr. Bernard R. Banker, also from NJ. The patent number (like a WHOLE LOT OF STUFF IN LADGARD'S BOOK) was supposedly application # 104,499 12-17-79. That was a dead end. But somewhere I have a patent from 1981 that was a contractor to the gov't that looked like what it could be. That's a long convoluted story; I got that one from a guy who told me he submitted stuff he worked on via a university prof who published stuff for the ISEE.... a volume on nitrobenzenes has the same labs. However; the one-pot process can work; too many people have worked with it and it does produce a scalable, crude product. If I find the EXACT PDF file I'll append this and post it.



[Edited on 24-7-2006 by quicksilver]




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[*] posted on 24-7-2006 at 08:58


Doesn't it seem strange that in a book which proposes
many procedures for syntheses of energetic materials , and given the potential dangers attendant to such business , that there would be such dismal performance in providing the references to sources which were the basis for the procedures being described ?

It doesn't exactly seem to be a trivial failing in my estimation , in fact it is a troubling departure from the accepted convention for technical writing . All the fancy graphics don't mean shit if a writer can't be bothered to cite accurate references to substantiate his proposed synthetic procedures . Such a writing style for describing chemical syntheses should be reassigned to storytelling and banned from technical writing all together :o:D

Is there even one single good patent number given as a reference in that Ledgard work ?
( which we should perhaps rename )
Energetica Ledgerdermainica Acta ....
written by Poofer the Magician :P
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[*] posted on 25-7-2006 at 06:32


Quote:
Originally posted by Rosco Bodine
Doesn't it seem strange that in a book which proposes
many procedures for syntheses of energetic materials , and given the potential dangers attendant to such business , that there would be such dismal performance in providing the references to sources which were the basis for the procedures being described

Is there even one single good patent number given as a reference in that Ledgard work ?
( which we should perhaps rename )
Energetica Ledgerdermainica Acta ....
written by Poofer the Magician :P


To be blunt with you I could only find less than half a dozen and I went through the whole book....I was obsessed with that book as I thought I got ripped off - I agree; there is a serious lack of "science-style" to it. I actually am suprised when one of his citations is correct. I always expect to hunt and hunt and hunt! And that is NOT the way such a book should be written!




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[*] posted on 19-12-2006 at 06:46


Quote:
Originally posted by hector2000
every time that i made tnt it was red.and when i add water to it, again red water.
i done these three steps from rougerscience (without oleum)and i think that information on this site is true.
when i melt my tnt and add some naco3 to it.the color will be brown red.and this step will
repeat if i add naco3 again too.
does tnt made ?


What exactly did you do? I am sure everyone would be happy to help you but there is a wee lack of clarity in youf questions that needs a bit of follow-up.....




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[*] posted on 21-12-2006 at 06:46


Quote:
Originally posted by hector2000
i use this method



The diluting of your nitrating acids may be the biggest problem. It seems that the addition of water serves no purpose. You started off with nice 90% HNO3 and then put water into it.....




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[*] posted on 21-12-2006 at 07:27


The red colour is caused by impurities, most likely they consist of partly nitrated toluene groups that still carry a sulfonic acid group, these can be bright red and it would explain why they are water soluble. At these temperatures, there will also be some oxidation, especially since there is still a lot of water present during the last step. Every TNT synthesis that I have read used oleum during the final nitrating step. As a concequence, I think there may still be a fair amount of DNT present in your final product...

The final yellow colour after the washings is perfectly normal. TNT can be everything from a very pale yellow, like shaved almonds, to a very dark brown, depending upon the amount of impurities...

[Edited on 21-12-2006 by nitro-genes]
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[*] posted on 21-12-2006 at 10:24


Yes, along with dnt and a host of other things it seems.

Why don't you do a melting point determination and find out for yourself the purity, its very easy to do
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[*] posted on 25-12-2006 at 09:09


my TNT did melt around 81°C, wich is pure
the crackling is coming from entraped water in the TNT, u should meld it in a boling water bath and remove the water floating on top of it
than slowly cool it down, let the DNT crystallise out and pour the still liquid TNT out
repeating this two or three times will purify ur TNT to a mp. >80°C (if u make it properly)
than its time for a Na2SO3-treating to remove the last impurities (4% solution at around 95°C whit strong stirring)
if the solution stays clear yellow, not red, its a very pure TNT
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[*] posted on 25-12-2006 at 09:32


Reliable procedures abound.

The Chemistry of Powder & Explosives available free in this site's Library

TNT - a dedicated volume on just this subject also in the Library here freely downloadable.

If memory serves the mononitration uses ordinary mixed acids at moderate temperature; the dinitration uses same at somewhat higher temp; and the final stage is the only one that employs fuming acids again at higher temps. But see the above for all the details

Vogel also has at least steps 1 and 2 in his Practical Organic Chemistry, q.v. From the Library here.

Org.Syn. (Organic Synthesis, books and website with searchable complete set) will also have at least the first two steps, it is noteworthy for the published procedures being scrupulously annotated, checked and verified because it dates from a period during the WWI years when American chemists HAD to make their own organic chemicals simply because they were cut off from the German suppliers and there was no US manufacturing-chemical industry then. Eastman (Kodak) changed that and Org.Syn. is partially an outgrowth of that. Its raison d'etre has shifted since then but its basic format remains: tested proven reliable well annotated procedures that anyone with the skills can replicate.

Nitroaromatics are rather toxic, protect yourself. Beware or NOx as you were given good advice above. A friend of mine spent time in a hospital due to a fume-off of a nitration he was carrying out at home.
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