Volitox Ignis - 4-2-2016 at 22:48
In a thread that I started in the Wiki subforum,someone named Jared Ledgard was briefly mentioned. I followed the links posted by another user and
eventually came across a book written by Ledgard titled "The Preparatory Manual of Explosives" and was told that nothing written by Ledgard is to be
taken seriously(Thread: http://www.sciencemadness.org/talk/viewthread.php?tid=65210). I decided to look at the procedure in the book for preparing TNT,since I thought
that it would be one of the easiest to "Fact check". I already shared my thoughts on the TNT procedure in the book,but I would like to know what
others have to say about it. The first procedure for TNT looks perfectly plausible. As for the other methods,the only apparent problem is the amounts
of each reagent used. Are there any other issues with the book (Or at least the TNT section)?
The work in question: https://miningandblasting.files.wordpress.com/2009/09/the-pr...
[Edited on 5-2-2016 by Volitox Ignis]
Microtek - 5-2-2016 at 07:23
Many of the procedures in the book are taken directly from the patent litterature, without much (any) checking of the veracity of the claims. The
first couple of alternate procedures for TNT are a slight variant of a patent process I have tried to reproduce myself. In the patent, a Dean-Stark
trap was used for removing water from the reaction, thus driving the equilibrium to the right (an example of so called reactive distillation). The
attraction was that you didn't need sulfuric acid at all, and only a slight stoichiometric excess of HNO3. Unfortunately, I never got it to work.
It seems as if it is working; an aqueous fraction is collected in the trap, and the organic phase changes color and smells of shoe polish. However,
I'm fairly certain that a lot of the nitric acid ends up in the aqueous phase in the trap, and that most of the toluene doesn't go much past the
mononitro stage. There is also extensive decomposition of the HNO3 with production of NOx at reflux temp for the hexane/heptane blend I was using.
Maybe it will work with just the right combination of solvent and temp/pressure...