hello,
I recently made some of the above. it worked well, and got about 80% worth of precipitate. when testing it (totally dry) there were no noteworthy
effects at all - i.e. heating resulted in decomposition, and a small flame, shock didnt do anything (i.e. hammer), and high temperature didnt do
anything either (i.e. thermite temperature shock). Is this a low sensitivity primary that requires another low sensitivity primary for it to work?
Guess the method I used was very simple, i.e mixing hexamethylenetetramine with HNO3 at 4 Deg C.
I searched the E & W forum, google, etc, and various books, but found no useful information.
Does anyone know more?
[Edited on 15-10-2005 by chemoleo]palpy - 10-8-2003 at 05:18
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 might try it in a mix with AN (hard crystals increase sensitivity) with a booster charge or just a big blasting cap.
But IMO it's better to save it for some RDX synth...Madog - 19-8-2003 at 23:28
hm, yeah, i agree, something like around urea nitrate.
i set off 10g of hexamine diperchlorate with 0.5g PETN the other day, very impressive for 10g of explosive! i think i musta had moe than 10g somehow.
it was justa bottle of it that i had always thought contained 10g, so its possbile it was morel ike 15, but it wasnt much.Nick F - 20-8-2003 at 05:32
The diperchlorate is meant to be comparable to tetryl, isn't it? I know it is both sensitive and quite powerful.
HDN is certainly more sensitive than AN. There is a composition in KIFE that uses HDN to sensitise AN. Hex is first heated with AN in solution, and
then the product is dried and added to more AN, and maybe a few other things, IIRC. Incidentally, does anyone know where that book can be obtained
online? I've lost my copy.Madog - 20-8-2003 at 07:48
wow, compareable to tetryl... i thought it was good but didnt know it was that good.
i should try doing some tests with it, useing it the way i used PETN for a booster, see if its good for that.
heres KIFE
http://24.128.216.215/KIFE.pdf
that IP will change, die comcast, die
[Edited on 8/20/03 by Madog]Nick F - 20-8-2003 at 08:54
"comparable to tetryl"
Well, that's what I've heard... I'm looking for a reference to support it now.
Downloading KIFE as I type, thanks.chemoleo - 25-8-2003 at 15:30
cool, I think I will try within the next few weeks to set off HDN with HMTD... anyone tried it? anyway i will keep u posted
Btw.. I never understood why people stress the sensitivity of HMTD - I prepared it straight accordign to the book ' chemistry of powders and
explosives'. It worked very well. however, i only managed to achieve detonation with thermite, or a VERY hard hammerblow. it didnt explode when
wet (with EtOH) , flashpowder didnt do, neither did sparkling candles (which should be very hot, as they contain Mg/Al). It just deflagrated. it wasnt
confined in any way. so, the only way to set it off reliably and unconfined turned out to be thermite. any advice??? sorry if this is slightly off
topic..
[Edited on 25-8-2003 by chemoleo]Haggis - 25-8-2003 at 15:46
Well, different batches produce different products. It is a general rule of thumb to always assume extreme sensitivity, and not get careless. Also,
it should be quite a bit more sensitive when it is dry. You will need a blasting cap if you plan to detonate the HDN, you cannot simply mix, but I
bet you already knew that.chemoleo - 25-8-2003 at 16:02
oh, sorry if I didnt make it clear enough. I read somewhere that HMTD can be detonated even when wet. under the conditions described in my earlier
post (i.e hammerblow, thermite), this wasnt possible. I am well aware that different batches have on occasion differnt properties, although I doubt it
in this case - i used different hexamine supplies etc, and 10 year old H2O2 and recent h2O2, and still the same result (just to eliminate the argument
u propose). so I dont think the relative insensitivity is due to old reagents etc.
with all the otha conditions I mentioned, it just burned very very fast, like nitrocellulose or better.
The point was to set off HDN with HMTD (just assume DRY for now). Havnt tried it yet as I said, but as I was able to set off ANFO with 15g HMTD
(unconfined, set off with a small amount of thermite), so I am sure it should be possible with HDN, too (I did the control, once with and without
ANFO, and the results differed significantly).
The only real question there is is whether there are easier ways to set off HMTD (only thermite did it in my case as i said )
[Edited on 26-8-2003 by chemoleo]Madog - 25-8-2003 at 16:51
what? HMTD is flame sensitivechemoleo - 25-8-2003 at 17:18
yes I know... have u tried it (the method from the chemistry and powders of explosives?)? I am very sure that there is nothin wrong with my supplies.
Else it behaves as it is described in many patents etc. So i DO think its the real stuff. Detonation is quite noticable. what do u suggest?Madog - 25-8-2003 at 20:41
what the hell?! you need thermite to make your HMTD det?! whooeee that is weid! have you tried it confined with a fuse?
thats messed. wow.Microtek - 26-8-2003 at 01:49
My HMTD doesn't make DDT on its own either unless fully confined ( at least not in the small amounts that I have used ), but a tiny speck of
silver acetylide nitrate does the trick very reliably. Of course the double salts must be washed very carefully. When I say fully confined, I mean
that there must be no openings in the confinement, not that the container must be very strong. Thus, a pinch of HMTD wrapped tightly in Al foil and
heated over a flame will detonate violently, but HMTD packed into a detonator and ignited with a fuse will only produce a fountain of flames or
sparks.Nick F - 26-8-2003 at 03:51
That's interesting - what size was the detonator tube that you used? And how much compresssion?
When I used to use HMTD it would always detonate from the spit of a fuse in ~4mm diameter paper tubes, pressed at roughly 1000 psi. The end of the
tube was not closed up in any way.
But maybe you pressed it more or had wider tubes or something...
I also noticed that a large pinch of HMTD pressed between two pieces of tape would not reliably detonate when ignited by a fuse (so it was fully
confined except for a ~3mm fuse hole). Quite surprising, considering that it did detonate in the tubes.
Perhaps my HMTD in the tubes took a little while to DDT, which the stuff in the tape couldn't do since there wasn't enough of it?Douchermann - 14-10-2005 at 23:28
Does anyone know the solubility of this stuff, in water at 4deg C? Also, does anyone know what its NOT soluble in, but ammonium nitrate is?Boomer - 14-11-2005 at 11:17
Bringing up an old thread is not always bad. At least you saved my from being the one who did (more stuff coming soon).
I don't know the solubility, why are you asking? Is it because of the process mentioned above, using only AN in solution? Sounds interesting,
especially for price reasons. IIRC Rosco or Philou said hex is more basic than NH3, so the reaction should be nearly quantitative. At least if you
boil off the ammonia (if HDN does not decompose). Otherwise: repeated fractional crystallisation?ADP - 17-11-2005 at 20:26
Quote:
Originally posted by Madog
hm, yeah, i agree, something like around urea nitrate.
i set off 10g of hexamine diperchlorate with 0.5g PETN the other day, very impressive for 10g of explosive! i think i musta had moe than 10g somehow.
it was justa bottle of it that i had always thought contained 10g, so its possbile it was morel ike 15, but it wasnt much.
Is hexamine diperchlorate prepared in the same manner as hexamine dinitrate substituting perchloric acid?Boomer - 18-11-2005 at 02:51
That would be the 'standard' way.
I wonder if it could be made ala 'HDN via AN+HCl' by dissolving hexa in HCl and adding a perchlorate? You might have to separate from the
(di)hydrochloride, though I guess that is much more soluble.Rosco Bodine - 18-11-2005 at 07:53
Whether or not this would work I have no idea , but you could experiment to find out .
A aqueous solution of 1 mole of HDN plus 2 moles of NH4ClO4 could possibly give the hexamine diperchlorate by double decomposition , precipitating the
product from a supernatant solution of byproduct NH4NO3 . Simply making a paste of the solids with minimal water and stirring thoroughly might be
enough to complete the conversion . Evaporation of the water at low temperature without isolation of the product could perhaps result in a mixed
composition having usefulness .DeAdFX - 23-11-2005 at 09:27
Quote:
Originally posted by Rosco Bodine
Whether or not this would work I have no idea , but you could experiment to find out .
A aqueous solution of 1 mole of HDN plus 2 moles of NH4ClO4 could possibly give the hexamine diperchlorate by double decomposition , precipitating the
product from a supernatant solution of byproduct NH4NO3 . Simply making a paste of the solids with minimal water and stirring thoroughly might be
enough to complete the conversion . Evaporation of the water at low temperature without isolation of the product could perhaps result in a mixed
composition having usefulness .
I wish I could test this but at the moment I am out of ammonium perchlorate. Avoiding strong acids(nitric/perchloric) would be nice as I cannot
aquire them locally(long drive + gas price = waste of $$). Could paraformaldhyde and ammonium perchlorate be used?
Methylamine Perchlorate along with lesser amounts of di and tri methylamine perchlorates would likely be the result .
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 .
There could also be double decomposition reactions in mixtures of glycine nitrate or urea nitrate mixed with ammonium perchlorate . Betaine nitrate
could also work the same way .quicksilver - 23-11-2005 at 17:45
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?Rosco Bodine - 23-11-2005 at 19:50
Excess heating or even hot spots in the reaction mixture could be a serious problem , no doubt .
Maybe it was in PATR or Urbanski where I read about the same method being applicable for guanidine perchlorate which
was described as being a very smooth reaction for the perchlorate . I can't recall ever seeing a detailed description of the process being
published anywhere , beyond a single sentence or two which is the occasional mention of guanidine perchlorate without mention of any synthetic route .
The obscurity of references and the potential value of
guanidine perchlorate does make it interesting .quicksilver - 24-11-2005 at 07:40
Quote:
Originally posted by Rosco Bodine
Excess heating or even hot spots in the reaction mixture could be a serious problem , no doubt .
Maybe it was in PATR or Urbanski where I read about the same method being applicable for guanidine perchlorate which
was described as being a very smooth reaction for the perchlorate . I can't recall ever seeing a detailed description of the process being
published anywhere , beyond a single sentence or two which is the occasional mention of guanidine perchlorate without mention of any synthetic route .
The obscurity of references and the potential value of
guanidine perchlorate does make it interesting .
A suppose a sand bath would be appropriate but with a solid / solid I don't know what would be available to continue a mix other than hand
stirring. And even that would be inefficient.
I did find the Organic Synth material. I dropped it in a text file (see attached).
I even have some cynamide but never attemped it for those reasons.
I wouldn't play with NH4ClO4 and CH2=O in big quantities.... nor with the synthesis of guanidin perchlorate based on the nitrate proces...I have seen
what GP is able to do and believe me it is powerful, sensitive and for sure to handle with care.
I also like the hexamine diperchlorate...the cristals are exceptionnally big and beautiful. I had cristals of 3-8 mm diameter...burn fiercely with a
bright flame after the melting.
Hexamine is not much basic than ammonia...because hexamine is a very stable teriary amine used as diuretic in pharmacology...thus it can be eaten at a
concentration 100% ...
I would dare anyone to drink 30% ammonia...in a few seconds your tongue dubble its volume, your tongue skin and mouth skin peels of leaving naked
flesh (I had once a bad experience with 10% ammonia so I know what it does)...then you get your throat attacked and you can't breathe anymore...your
lungs bleed and produce a lot of liquid...remember that NH3 was used as a wargas...
SO NEVER TRY !!!!
There is stil a chance to get HeDN (HDN is hydrazine dinitrate!) by mixing Hexamine and AN due to solubility differences. And the same process for AP
to get HeDP.
Test is simple...if ammonia evolves than it is a GO ! (Maybe some warming is needed) but again do not try on a big amount....Hexamine
salts suffer from hydrolytic troubles....possible result is methylamine as mentionned Rosco.
Hexamine dichloride turns into methylamine chloride upon warming...
[Edited on 13-12-2005 by PHILOU Zrealone]Rosco Bodine - 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 .
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.Lotek_ - 22-12-2005 at 19:06
i think he ment to use UN as the primary booster for the AN mixAqua_Fortis_100% - 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):
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..nitro-genes - 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]Aqua_Fortis_100% - 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..
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":
[Editado em 28-1-2007 por Aqua_Fortis_100%]up - 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.Zinc - 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.PHILOU Zrealone - 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 compoundsZinc - 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).Pulverulescent - 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!
PPHILOU Zrealone - 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]Pulverulescent - 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.
Pcrazyboy - 15-3-2008 at 09:16
Well I made some HDN and the synth was very fast and easy and got pretty good yields.
I will be happy to supply the synth if anyone is interested.Pulverulescent - 16-3-2008 at 14:01
Aaarrrgggh! The Charring! Ditto residue. . .Still, only two HN03 groups.
P
HDN
~TCM~ - 22-4-2008 at 01:07
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.Boomer - 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.
)
