Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
 Pages:  1  ..  9    11
Author: Subject: Trinitrotoluene preparation
NeonPulse
National Hazard
****




Posts: 417
Registered: 29-6-2013
Location: The other end of the internet.
Member Is Offline

Mood: Isolated from Reality! For Real this time....

[*] posted on 1-11-2015 at 15:17


Don't trust anything from ledgards book- it is notoriously full of inaccuracies and dangerous procedures which were poorly researched. You would be much better off deleting it off your hard drive and using the space for something better. There are much more accurate synthesis described in this thread.



Where there is a will
there is a way.

AllCheMystery!
https://www.youtube.com/channel/UCWbbidIY4v57uczsl0Fgv7w?vie...
View user's profile View All Posts By User
greenlight
International Hazard
*****




Posts: 689
Registered: 3-11-2014
Member Is Offline

Mood: Energetic

[*] posted on 2-11-2015 at 09:23


Yeah I made this a couple of years ago using Ledgards book and it is one of the only synthesis i have attempted from it.
I don't use his book as a guide for any explosive synthesis at all now.




The only use for an atomic bomb is to keep somebody else from using one.
George Wald
View user's profile View All Posts By User
greenlight
International Hazard
*****




Posts: 689
Registered: 3-11-2014
Member Is Offline

Mood: Energetic

[*] posted on 3-11-2015 at 10:08


A piece of the product was put in water and the water heated until it melted. Started at 55 Degrees and was fully melted at 60 Degrees.
Very strange, between the melting point of MNT and DNT but nowhere near TNT.




The only use for an atomic bomb is to keep somebody else from using one.
George Wald
View user's profile View All Posts By User
Agari
Banned





Posts: 160
Registered: 8-10-2015
Location: The Amine Group
Member Is Offline

Mood: Lowest Oxidation State

[*] posted on 9-11-2015 at 17:33


There is a mirror of the Megalomania website on the Deep Web:
nope7beergoa64ih.onion
I stumbled across if by accident while searching "Astrolite Synthesis"(The procedure was very close to what I had thought it would be) using the Disconnect Search engine,the default search engine used by the TOR Browser, which can be downloaded here. In case you are wondering,I use TOR because my other browsers are slower compared to it, and I am too paranoid to simply use the HTTPS version of this forum, especially after the phosgene thread that I posted in Organic Chemistry a while ago.
Just a heads-up, I caught a glimpse of a "cooking" section on the website,though I will not visit it for obvious reasons. I am aware that this post does not necessarily concern the preparation of TNT,but I am simply posting the link to a mirror of the now-gone Megalomania website.
Edit:I think that this belongs in another thread, I will start a separate thread linking the Deep Web mirror.

[Edited on 10-11-2015 by Agari]
View user's profile View All Posts By User
NeonPulse
National Hazard
****




Posts: 417
Registered: 29-6-2013
Location: The other end of the internet.
Member Is Offline

Mood: Isolated from Reality! For Real this time....

[*] posted on 10-11-2015 at 16:18


Someone has already taken the time to copy the whole TNT synthesis by mega on the first page of this thread about three posts down so there is no need to visit the link.



Where there is a will
there is a way.

AllCheMystery!
https://www.youtube.com/channel/UCWbbidIY4v57uczsl0Fgv7w?vie...
View user's profile View All Posts By User
Agari
Banned





Posts: 160
Registered: 8-10-2015
Location: The Amine Group
Member Is Offline

Mood: Lowest Oxidation State

[*] posted on 10-11-2015 at 18:58


Quote: Originally posted by NeonPulse  
Someone has already taken the time to copy the whole TNT synthesis by mega on the first page of this thread about three posts down so there is no need to visit the link.

But now we have access to more energetic material syntheses!
Looking at other proposed methods in this thread,we now know which one is the "true" method.




Element Collection Status:
Elements Acquired: 21/91
Latest: Lead (Pb)
Quantity: 12g
-----------------------------------------------------
View user's profile View All Posts By User
Daffodile
Hazard to Others
***




Posts: 167
Registered: 7-3-2016
Location: Highways of Valhalla
Member Is Offline

Mood: Riding eternal

[*] posted on 14-3-2016 at 13:48


Instead of SO3 whatever other route, I added 30ml m-phosphoric acid to my acid mix and DNT. Results look pretty good, except the fumes were worse than normal.

[Edited on 14-3-2016 by Daffodile]

IMG_20160314_134514.jpg - 705kB

[Edited on 14-3-2016 by Daffodile]

[Edited on 14-3-2016 by Daffodile]

IMG_20160314_141014_1.jpg - 792kB
View user's profile View All Posts By User
Daffodile
Hazard to Others
***




Posts: 167
Registered: 7-3-2016
Location: Highways of Valhalla
Member Is Offline

Mood: Riding eternal

[*] posted on 14-3-2016 at 19:59


Hmm I tried compressing some in foil, and heating lightly. It would just deflagrate, and not detonate at all.
View user's profile View All Posts By User
PHILOU Zrealone
International Hazard
*****




Posts: 2880
Registered: 20-5-2002
Location: Brussel
Member Is Offline

Mood: Bis-diazo-dinitro-hydroquinonic

[*] posted on 15-3-2016 at 03:57


Quote: Originally posted by Daffodile  
Hmm I tried compressing some in foil, and heating lightly. It would just deflagrate, and not detonate at all.

A few grams TNT or DNT will not detonate from heating confined inside aluminium foil...well maybe if you trow it naked onto a 2000-3000°C molten metal bath...the Al foil will act as insulator before acting as a heat transfer media slowing down heat transfer to your TNT/DNT and thus it may vapourize and burn /deflagrate before detonation.

TNT and DNT are relatively insensitive for such low amounts you need a detonator.




PH Z (PHILOU Zrealone)

"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
View user's profile View All Posts By User
Daffodile
Hazard to Others
***




Posts: 167
Registered: 7-3-2016
Location: Highways of Valhalla
Member Is Offline

Mood: Riding eternal

[*] posted on 15-3-2016 at 11:06


I recrystallized the product from Methanol. Strangely, it crystallized in two portions, which I unintentionally separated when I poured the solvent off the first, allowing the second to crystallize separately. The first portion (also the larger one, about 3 times the mass) had a melting point of 81.5 degrees C. The second had a melting point of about 73 ish.

I would highly recommend my phosphoric acid route, even though about 30% yield was lost at some point.

[Edited on 15-3-2016 by Daffodile]
View user's profile View All Posts By User
Hennig Brand
International Hazard
*****




Posts: 1284
Registered: 7-6-2009
Member Is Offline

Mood: No Mood

[*] posted on 15-3-2016 at 11:41


Sulfuric acid is just much more common and normally much cheaper I think, but yes other things can likely be used. For small scale I guess cost really doesn't matter much. The SO3 was just used to prepare 98% sulfuric acid, which works great to produce TNT from DNT, but is actually pretty difficult, and extremely inefficient, to prepare by simply boiling down lower concentrations of H2SO4 because of loss of sulfuric acid as vapor without proper distillation equipment, water absorption and the decomposition that takes place at high temperatures/high concentrations.


[Edited on 15-3-2016 by Hennig Brand]




"A risk-free world is a very dull world, one from which we are apt to learn little of consequence." -Geerat Vermeij
View user's profile View All Posts By User
NeonPulse
National Hazard
****




Posts: 417
Registered: 29-6-2013
Location: The other end of the internet.
Member Is Offline

Mood: Isolated from Reality! For Real this time....

[*] posted on 21-3-2016 at 00:05


Just this weekend I decided to revisit making TNT and the results were much more satisfying than my first attempt. Once again I used a synthesis devised by Hennig brand a few pages back where ammonium nitrate is the nitric source along with good old drain cleaner of around 93% if my density measurement was correct. However this time I allowed for 20% excess unlike my 1 st attempt. I made up the nitrating mixture and let it sit in the freezer for an hour while I attended something else. This time I was much better equiped for the task since last time I just used a beaker with hand stirring.
The nitration mixture was charged into a 1l RBF with two necks, and a large oval stir bar dropped in, a thermometer adapter in one mouth and a pressure equalising addition funnel to the other and turned the tap to slowly drip 50g toluene into the reaction mixture at a rate of a drop a second slowing occasionally to let the temp not rise too fast and go above 55 yet. For the last 10 mls I just let it rise and 10 mins after the last drop the funnel was switched for a condenser to reflux. Heating was started cautiously and slowly to get up to 80c where it was held for 3 hours with a brief period where it crept up to 90 without me realising. This was soon fixed though. I let the vessel cool a bit and transferred the RBF contents into a 500 ml beaker to cool completely and solidify.
A funny thing happened though, the DNT did not solidify and had me worried that I had somehow effed it up even after an hour n the fridge so I decided to use a syringe to syphon the layer into water and this is where it decided it set solid slowly like the hot ice effect. Scooped this out and quenched the acid into water precipitating a little more DNTthis was placed with the cake into about 600 ml distilled water and heated to melt it while strong magnetic stirring was applied to wash it. The DNT cake was allowed to set cool and fished our out of the beaker, rinsed off and dried for weighing. It weighed 75.1 g and was crystalline with small needles and had very little MNT smell to it. The first batch I made smelt quite a bit like MNT and this one does not at all. There was pretty much no smell during nitration either except when I switched to the condenser so it was well contained in the chosen reactor. I will be completing the final nitration in the next week or so and am actually considering making oleum with some phosphorus pentoxide that I have around, that is if I find the time to otherwise it's just going to be a standard nitration mix of concentrated mixed acids.
T

image.jpeg - 1.8MBimage.jpeg - 1.8MBimage.jpeg - 1.8MB




Where there is a will
there is a way.

AllCheMystery!
https://www.youtube.com/channel/UCWbbidIY4v57uczsl0Fgv7w?vie...
View user's profile View All Posts By User
Hennig Brand
International Hazard
*****




Posts: 1284
Registered: 7-6-2009
Member Is Offline

Mood: No Mood

[*] posted on 21-3-2016 at 17:02


Nice looking setup! Really good that you are using reflux! I think your yield should be closer to 100g of DNT from 50g of toluene however.



"A risk-free world is a very dull world, one from which we are apt to learn little of consequence." -Geerat Vermeij
View user's profile View All Posts By User
NeonPulse
National Hazard
****




Posts: 417
Registered: 29-6-2013
Location: The other end of the internet.
Member Is Offline

Mood: Isolated from Reality! For Real this time....

[*] posted on 21-3-2016 at 23:44


Thanks! it really helps when you have the right equipment for the job.
I did see you got 100g DNT in your earlier post and i expected similar but i guess there was more impurities in my batch that were removed during the washing stage and also i set the cake up onto a few layers of paper towel to wick out moisture and upon leaving it overnight the paper towell was laden with an oily exudation from the cake and i suspect a lot of the extra weight was lost there. maybe there was losses as a result of the extra hour of reflux but that seems unlikely.
but anyway i'm still quite pleased and i must say as far as a synthesis for energetics goes this is quite easy to do and required minimal supervision- just a regular eye on the thermometer and wait. all in all a much better outing than my first attempt




Where there is a will
there is a way.

AllCheMystery!
https://www.youtube.com/channel/UCWbbidIY4v57uczsl0Fgv7w?vie...
View user's profile View All Posts By User
Hennig Brand
International Hazard
*****




Posts: 1284
Registered: 7-6-2009
Member Is Offline

Mood: No Mood

[*] posted on 31-3-2016 at 17:20


I have a suspicion that only one mole of nitrate per mole of toluene was added instead of the required two moles of nitrate per mole of toluene. I added the nitration mixture to the toluene while you did the opposite, I think both can work fine though. Unlike esterifications, aromatic nitrations are not equilibrium reactions, so if the temperature and rate of toluene addition were in line nearly all of the first half of the added toluene would be converted to DNT and most of the rest of the toluene addition would be left un-nitrated. The un-nitrated toluene would act as a solvent as well which probably lowered the yield also. This is my theory anyway.



"A risk-free world is a very dull world, one from which we are apt to learn little of consequence." -Geerat Vermeij
View user's profile View All Posts By User
 Pages:  1  ..  9    11

  Go To Top