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chemoleo
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hexamethylenetetramine dinitrate
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]
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palpy
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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...
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Madog
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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.
Most people outgrow their pyro tendencies, we are the ones who\'s tendencies outgrew us.
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Nick F
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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.
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Madog
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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]
Most people outgrow their pyro tendencies, we are the ones who\'s tendencies outgrew us.
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Nick F
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"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.
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chemoleo
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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]
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Haggis
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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.
Great ideas often receive violent opposition from mediocre minds.
<b> <a href=\"http://pgp.mit.edu:11371/pks/lookup?op=get&search=0xEE41A2B1\">PGP Key</a> </b> 0C0A 7486 B97F
92EE AE50 A98C A4F3 087E 8CE9 A782 |
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chemoleo
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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]
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Madog
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what? HMTD is flame sensitive
Most people outgrow their pyro tendencies, we are the ones who\'s tendencies outgrew us.
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chemoleo
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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?
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Madog
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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.
Most people outgrow their pyro tendencies, we are the ones who\'s tendencies outgrew us.
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Microtek
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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.
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Nick F
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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?
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Douchermann
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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?
It\'s better to be pissed off than to be pissed on.
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Boomer
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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?
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ADP
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| 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?
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Boomer
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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.
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Rosco Bodine
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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 .
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DeAdFX
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| 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?
6H2CO + 4NH4CLO4 ---> hexamine tetraperchlorate + 6H2O ?
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Rosco Bodine
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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 .
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quicksilver
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| 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 .
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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?
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Rosco Bodine
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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 .
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quicksilver
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| 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.
Attachment: guanadine-nitrate.txt (16kB)
This file has been downloaded 1906 times
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PHILOU Zrealone
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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]
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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