Anyway, I have been doing some preliminary synthesis experiments with NTNT. I did it once via sulfuric and once via hydrochloric acid. During the
H2SO4 mediated synthesis (scaled down to 1/10 of the reactants) I noted that if the prescribed method is followed using pristine needle crystals of
NQ, large amounts of it are recovered on filtration. I extracted the filtered mass of crystals and amorphous powder several times with acetone,
neutralised the acetone soln with NaHCO3 and evaporated the solvent at room temp in an airstream. This produced 1,766 g of yellow flaky crystals
corresponding to 36% yield, assuming the product to be pure NTNT. I then tested the melting point in a glass capillary, and found an onset of melting
at 75 C, but the bulk of the material remained unmelted at 100 C. I haven't tested any detonics yet.
I then read the papers with the original experiments, and noted that the un-nitrosated triazine must be quite stable (the authors prepare it by
heating at 50-55 C for 3 hours). I then tried the HCl mediated procedure (as per the bit-chute video, and again scaled to 1/10), but did not add ice
or cool the reaction until I was about to add the NaNO2. I also used lab-grade HCl and magnetic stirring instead of intermittent swirling. The NQ was
still not very soluble in aqueous HCl, but when the hexamine was added it evidently reacted and the solution turned clear after about 5 minutes of
stirring. Then ice was added and the nitrite solution was added all at once. Some effervescence was observed, but only slight foaming. After 30
minutes a dense pricipitate had formed, similar to RDX in its tendency to settle. This was easily filtered (I had set up for Buchner filtration, but
that would not have been necessary), washed on the filter and air dried overnight to yield 1,17 g of crude product.
The mother liquor had been set outside to off-gas overnight, and significant amounts of additional precipitate had formed in the morning. I have not
had time to isolate it yet, so I don't know how much. 1,17 g would correspond to about 31% yield.
I don't quite understand why you would assume that ionic derivatives might be formed. I think NTNT must be a very weak base; even the un-nitrosated
parent molecule is a weak base and its HCl salt can be converted to free base by heating with 18% HCl. Even partially nitrosated derivatives must be
orders of magnitude weaker.
I find it much more likely that what you are seeing is either differing degrees of nitrosation or maybe presence of impurities such as sulfuric acid
(which can be notoriously difficult to remove), or maybe unreacted starting materials in differing amounts. |
.... Caution: Keep away from bus, tram, train, open
window, bridge, elevator and similarly. Do not travel anywhere, especially not to Ukraine.
and hopefully find a way to use your invention.