HDN Troubles

[Lewis]

Today an HDN synthesis was performed.

30g ammonium nitrate (agriculture grade) was dissolved in 100mL of muriatic acid (clean looking, hardware store grade). 15g of purified hexamine was dissolved in 25mL of tap water. The solutions were chilled and mixed.

A brilliant, fine white precipitate immediately appeared, and the suspension was hastily filtered before being washed with a thin stream of acetone (again, hardware store, seems clean but may not be dry).

When it seemed most of the water had been purged from the crystals, they were transferred, wet with acetone, to a pyrex dish. They were then heated on a hotplate (the lowest setting, a hand could be put on the element for a minute, uncomfortably).

The slurry was left to dry on this setting for ~2 hours. After which it had become a runny orange mess which would not hold a flame (implying at the very least that little acetone remained).

http://i282.photobucket.com/albums/kk278/orbital_Saucer/DSCN1731.jpg?t=1227576871
Ugh.

The material was dissolved in hot water and washed down the drain. I realize that there are so many unknowns in this situation that conjecture may be difficult, but I'd like to hear from anyone who has had similar experiences with HDN or could offer a thought.

That's all for now.

[megalomania]

Looks like the remnants of pumpkin pie to me, a conclusion subtly reinforced by the pie plate. Dear god I have the same handwriting, a pie plate just like that, and even a very similar table as in the picture. Not that this statement adds substantively to the question at hand...

If I had to conjecture, and I am doing so right now, I would say your HCl is contaminated with a good deal of iron ions that precipitated. This is what is giving you the muddy orange crud. It is not uncommon for there to be significant contaminating species in "hardware store" brand chemicals. Indeed many of these chemicals are reject lots from the chemical industry suitable for cleaning crud, but not for actual experimentation or manufacturing.

It's cheap for a reason...

[Rbick]

I had similar difficulties making HDN. Everything I was using was reagent grade except for the HCl. Because of this, I assumed it was due to impurities in my HCl. Muriatic acid as it is called in the industry is used to clean stone for masonry and in concrete manufacture. Something about that tells me that it doesn't have to be very pure :D

I gave up the pursuit of attempting to manufacture HDN as I was doing it only out of curiosity and didn't see it as an explosive with much practical use as it is very hygroscopic and not very powerful. If I were to attempt HDN again, I would get higher quality HCl as a start. Hope this helps. Good luck.

[-=HeX=-]

When I tried HDN I used pool grade HCl from E.Leclerc in france. I followed the same route and my product was perfect. No Fe ions in my one euro per litre stuff. Then again, I had tested it on TATP and HMTD and found it perfect. When I get more hexamine I will try it again with photos. Iirc that is the 'Mr Cool' method. I believe cyf531 has had success with this method.

What about hexamine diperchlorate? Do I just replace the nitrate with an equimolar mass of perch? I think someone on SMDB tried it.

[Lewis]

It's cheap for a reason...
Apparently not cheap enough. The industries would pay next to nothing for much more product that was much purer.

I gave up the pursuit of attempting to manufacture HDN as I was doing it only out of curiosity and didn't see it as an explosive with much practical use

Naturally, HDN is the means to an end. I would never try to use it as an explosive in its own right. I could avoid HCl altogether, but I'll be damned if I'm going to start wasting HNO3 on a synthesis that will work with NH4NO3.

Time for a new HCl brand I guess.

[Hinckleyforpresident]

If pure-ish HCl isn't available to you, you could make it from NaCl, H2SO4, and water.

[Alexires]

Couldn't you just heat the HCl you already have and bubble the HCl gas into some distilled water, leaving the contaminant behind?

[Lewis]

/\ This seems like a better idea, as you don't need to separate out the H2SO4.

I tried the above synthesis again (using 1/2 amounts), and a different brand of HCl (again, clear, but for acidifying pools). Again, a nice white precipitate, again, I dry on low heat for a long time.

And again, eventually turns into orange goo that refuses to dry out any more, or burn at all.

What it God's name is going on here...

By the way, although I tried to sparingly wash the water away with a stream of acetone, the slurry was still very acidic. I should probably invest in a vacuum filtration system to remove liquids better.