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Author: Subject: hexamethylenetetramine dinitrate
Rosco Bodine
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[*] posted on 22-12-2005 at 15:59


Quote:
Originally posted by quicksilver
Quote:
Originally posted by Rosco Bodine
Now there is a different reaction which might be interesting . There is a parallel reaction as is used for making guanidine nitrate from dicyandiamide and ammonium nitrate , substituting ammonium perchlorate and getting guanidine perchlorate as the product .


Wasn't that a "solid & solid " synthesis from Organic Synth web site...the one with the "warning"...? As I remember it was a heating of two solids, which I found interesting. But the "warning" was strange; something about guanidine nitrate being quite dangerous and utilizing a blast wall...(?) do you remember which one I mean?



chemoleo pointed out a guanidine nitrate synthesis which uses calcium cyanamide and ammonium nitrate in aqueous solution and is supposed to be a safer method . The same reaction probably would work substituting ammonium perchlorate , which would produce guanidine perchlorate .
Maybe this is the method which was in mind when the
author mentioned a parallel reaction in PATR .

See the following thread :
http://www.sciencemadness.org/talk/viewthread.php?tid=2762#p...
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[*] posted on 22-12-2005 at 17:37


Quote:
Originally posted by palpy
yes, it's a fairly insensitive explosive - thus NO PRIMARY. As far as I know, it should be more sensitive than AN, I'd guess something like urea nitrate.


You can det UN without a booster.




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[*] posted on 22-12-2005 at 19:06


i think he ment to use UN as the primary booster for the AN mix
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[*] posted on 27-1-2007 at 17:29


i made some time ago , some grams of HDN shiny crystals with easy: dissolving hexamine in water with some nitrate ,cooling this and adding to it and mixing this in well cooled nitrate/dilute HCl/H2SO4 solution.. quickly filtering the precipitate ,washing with acetone and putting in a plastic bag hermetically closed.. my great problem (like urea nitrate) is drying this compound..
my stuff looks as this (celtick page):

http://www.angelfire.com/goth/celtick/HDN_bestanden/HDN_Crys...

i tried put over a incandescent lamp but not works very well(still releasing a strong formaldehyde smell ...heating is probably a bad thing.. what about?) other question is: anyone know how much this stuffs can be well stored (validity)???
some time ago i (tried) thinking about this HDN : if i have a success in perfectly dryness of this stuff , can i add a small amount of a compatible and hydrophobic substance (an especific oil probably (eh?)) in the HDN to prevents it to absorbs moisture from air and increases storage time..
about the "compatible substances". what i must avoid allow together with this compound? e.g. copper powder ?

thanks and sorry about my ignorance or any mistake..




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[*] posted on 27-1-2007 at 17:47


HDN is pretty sensitive to decomposition with temperatures above 100-120 deg C. When you use even a small excess of nitric acid, it can become occluded in the crystals, making them even more unstable even if you wash them thoroughly. Best to use a sligh excess of hexamine and temperatures of 70 deg C max for drying...

Not sure though about the H2SO4-HCl method, where did you get it from? Excess HCl would yield methylamine salts as well...

[Edited on 28-1-2007 by nitro-genes]
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[*] posted on 27-1-2007 at 18:17


i get first time this synth from Alengosvig page on explosives... my HCl is too weak (9.75%), so i mix some conc. H2SO4 to raise the H3O+ conc and make more prone to interacte with NO3- from nitrate and possible increases the HDN yield .. i used excess of nitrate (added after cooling mix to avoid precipitate the (K-Na)NO3 (double nitrate))..
about the methylamine, i tried says which i added hexamine to water with nitrate in a separate container ( and this cooled added to also cooled another container with HCl/H2SO4/nitrate ) . and i also believe which methylamine can form, but HDN is predominant because (probably) hexamine react with the HNO3 much before than HCl and precipites instantaneously... recently (some weaks ago) i searched mainly on Ac2O and visited several files atributed to Rodhium , among many of these has a good section on methylamine manufacture.. i also looked in the Mr Cool page on MMAN section and also org. synth collection... the bad part for make methylamine is the waste in the methylamine chloride step, yielding also in NH4Cl (NH3 from hydrolisis of hexamine reacting with HCl), i think..

nitro-genes , thanks about notes on temperatures..i really need buy a efficient thermometer type.. :mad:
my worry about using heat is if some water is present and melt away the HDN... using vacuum for drying maybe helps a lot...

sorry about the link, only now i see which this not shows the images.. go to celtick page and click on "photo's":

http://www.angelfire.com/goth/celtick/HDN.html

[Editado em 28-1-2007 por Aqua_Fortis_100%]

[Editado em 28-1-2007 por Aqua_Fortis_100%]

[Editado em 28-1-2007 por Aqua_Fortis_100%]




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[*] posted on 28-2-2007 at 18:28


What. My HDN allways have been very very tiny crystals. Not like yours.
I have tried to detonate it sometimes. 5 grams with 1g APAN blastingcap.
50 grams with 10g of APAN.
I have allso made PBX with it. I used 89,3% HDN + 6,4% PiB + 4,3% chainsaw oil.
The HDN/PiB had very good consistent. I pressed it and was using only 4 grams of APAN.
It was a long time ago now, and next sesson I wil try to detonate some HDN/PiB with homemade #8 blasting caps with PETN instead.
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[*] posted on 4-3-2008 at 12:30


I made 30g HND with hexamine, HCl and NH4NO3. I mixed it with 120 g of ammonium nitrate and tried to detonate it with around 8 g of lightly pressed AP. The detonation failed. Does anyone know why? I have heard that smaller detonators have been use on this mixture and it did detonate.



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[*] posted on 5-3-2008 at 06:03


Quote:
Originally posted by Zinc
I made 30g HND with hexamine, HCl and NH4NO3. I mixed it with 120 g of ammonium nitrate and tried to detonate it with around 8 g of lightly pressed AP. The detonation failed. Does anyone know why? I have heard that smaller detonators have been use on this mixture and it did detonate.


You probably got:
1°)either a mix of Hexamethylene dichloride and Hexamethylene dinitrate (minor product because HCl is a stronger acid), the dichloride is not known explosive.
HeDN is thus diluted with HeDC
2°)either insufficiently dried salt
3°)NH4NO3/HCl seems a kind of aqua regia mix…Hexamethylene tetramine can thus oxidize into non explosive ammonium formate and maybe into N chloro methylene compounds




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[*] posted on 5-3-2008 at 10:49


I understand. Well I have to get home HNO3 to make HDN. I have tried to make it with ammonium nitrate and HCl as I have heard that some people made it that way. The reaction worked exactly as described. And I dried the product very good (washed with alcohols and put it on a radiator at around 50 C for some hours).



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[*] posted on 10-3-2008 at 09:19


IMHO, hexamine is fully utilised only when cyclonite is the the end-product! The dinitrate, to me, is way too oxygen-deficient and insensitive to be of any real interest.
And, yes, HMTD *is* a strong primary(mine always smelt fishy(methylamines))but its instability's a downer; nitromannite with perchlorate/al flash initiator makes a safer detonator.
I find it excruciatingly tantalising, though, that NH4N03/formalin solutions contain virtual cyclonite, knowing that the water content is all that separates me from the nitramine.
I've considered dessicating over H2S04, but even if it worked it'd be a slooowww process.
Fuck the drugwar and the fucks who perpetuate it; (Ac2)0 should be as easy to get as GAA.
What one could do is distill the dilute HN03 from NH4N03/formalin, concentrate from H2S04 and nitrate the resultant dinitrate conventionally.
That way, you don't lose any H2S04.
I'm not suggesting that anyone should try this because it could be dodgy; I'll get around to it, myself. . .manana!
P
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[*] posted on 12-3-2008 at 05:38


Quote:
Originally posted by Pulverulescent
IMHO, hexamine is fully utilised only when cyclonite is the the end-product! The dinitrate, to me, is way too oxygen-deficient and insensitive to be of any real interest.
What one could do is distill the dilute HN03 from NH4N03/formalin, concentrate from H2S04 and nitrate the resultant dinitrate conventionally.
P

Actually the dinitrate is of interest...because of its high volume of detonation gases and quite high VOD for such an oxygen unbalanced compound. It is sometimes used as a previous step to cyclonite (RDX) because it can be done with diluted HNO3 and thus reduce heat (neutralisation heat) and amount of concentrated HNO3 needed for the RDX.

HNO3 formalin will only result in NxOy and CO2...Have you ever tried formol with HNO3 or polyformal with HNO3? It simply heats up, boils off NxOy and then goes to runaway...solid (-CH2-O-)n makes it slightly slower but it also goes to runaway

[Edited on 12-3-2008 by PHILOU Zrealone]




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[*] posted on 14-3-2008 at 06:31


I'm not suggesting the dinitrate is devoid of interest, Philou, but it doesn't excite as an explosive quite the way cyclonite does.

When NH4N03 dissolves in formalin, hexamine and dilute HN03 are formed.
Evaporation of the solution gives the dinitrate but the acid that's driven off (enough to fully nitrate the dinitrate), is lost.

If it's recovered by distillation and concentrated the acid obtained will nitrate the dinitrate to give the nitramine in reasonable yield.

You're now getting cyclonite from two easy reagents; the acid required generated in situ.
I don't how dilute the acid will be and a large excess of H2S04 might be required to concentrate it but at least you'll only use up two compounds.

I don't know why you thought I'd put formalin and HN03 together, though, as H2C0 is very susceptible to oxidation.
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[*] posted on 15-3-2008 at 09:16


Well I made some HDN and the synth was very fast and easy and got pretty good yields.

Here is a video of deflagration: http://www.youtube.com/watch?v=lapBSEVl5U8


I will be happy to supply the synth if anyone is interested.




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[*] posted on 16-3-2008 at 14:01


Aaarrrgggh! The Charring! Ditto residue. . .Still, only two HN03 groups.
P
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[*] posted on 22-4-2008 at 01:07
HDN


I recently made a batch of HDN via the HNO3 method, I got a good yield, washed my product thoroughly in acetone then dried in a dessicator. Then I put it in the oven at about 80C, I think this may have been a mistake.It deflagrated exactly the same as the videos I have seen, however when I made the charge I noticed some of the crystals had turned yellowish, 40g failed to detonate with 5g of AP.
The charge was packed very tightly.
I am sure the product was dry, did it begin to decompose from the drying in the oven, or was 5g of AP simply inadequate for 40g of highly compressed HDN.
Any ideas would be greatly appreciated as this is the first failure i've had and would like to pinpoint why it happened.




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[*] posted on 23-4-2008 at 02:20


Maybe the CJ-pressure of lightly pressed TATP is not enough to get HDN going?
I remember never having a problem with compound detonators, with 1.5g MHN base charge, vise-pressed at 10000 PSI to over 1.6g/cc, which should give close to 200 kbar.

Straight HDN pressed at 500PSI (body weight / dowel) went high order over a feet in a 10mm ID, 1mm wall Al pipe at 4,5 km/s, forgot the density but think it was 1.2 or 1.3g/cc with one of those.
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