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[megalomania]

CodeMason
Frequent Poster
Posts: 383
From: Your Nightmares
Registered: NOV 2000
posted 05-05-2001 10:02 PM
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I want to make some RDX at home, and from what I have gathered from various texts, this is the best procedure for the job:
1. Mix 250 grams powdered hexamine with 50 grams powdered ammonium nitrate.
2. Very slowly add this to 500ml beaker (in ice bath) containing 200ml industrial strength nitric acid.
3. Once all the hexamine/NH4NO3 has dissolved, gently elevate the temperature to 70 degrees celcius, and let it sit until crystals percipitate. Once that happens, lower the temperate to 50 degrees.
4. Decant crystals and wash them with ethyl alcohol. If high acidity, add baking soda until neutral.
Will that work? If not, please point out my mistakes. Thanks.


Demolition
Frequent Poster
Posts: 158
From: Australia
Registered: FEB 2001
posted 05-05-2001 10:52 PM
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Do you have an approximation on what the yield would be?
I have found a good procedure.Although I have never tried it seems to have good results considering the amounts of hexamine and nitric acid used.
Originally posted by pete

quote:
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The procedure is as follows, take 60ml of your conc red nitric acid, cool this to 20 degrees cel. Next you will need 35 grams of hexamine, yes 35 grams. Add to hexamine to the red nitric acid, don't let the temp exceed 30 degrees cel. Once you have added all of the Hexamine then you heat the mixture up to 55-60 degrees cel slowly. Hold it there for 10 minutes, cool the mixture back down to 20 degrees cel. and dump in a large quantity of water eg 400ml for these quantities. The yields are impressive, and on comparing the recrystalized product to RDX made in other more written about methods, the product was found to be at least as good. This method is cool as you can use red nitric acid with it, and hexamine, were i live is cheap and really brought. The yields I have got so far from these quantities have been about 17-18 grams.
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Demolition
[This message has been edited by Demolition (edited May 05, 2001).]



CodeMason
Frequent Poster
Posts: 383
From: Your Nightmares
Registered: NOV 2000
posted 05-05-2001 11:13 PM
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I'm not sure about the yields, but thanks for that procedure. It seems like it's a good one!


Bitter
Frequent Poster
Posts: 290
From: 11 Downing Street, London, England
Registered: SEP 2000
posted 05-06-2001 05:06 AM
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Just in case you hadn't already read the 'nitration runaway' thread, don't use sulphuric acid mixed in with the conc nitric at all- I experimented with it at very low temperature in a hope that it would work. It actually seemed to for the first ten seconds, but the yeild was so pitiful that I just threw the whole lot away. I wasn't even sure that what I got was RDX, so I wouldn't bother.


Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 05-12-2001 09:22 AM
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Codemason, the procedure you describe above which is the K process or derived from the K process sounds good, but there is one point of vagueness such as for how long do you leave it at 50degrees?


CodeMason
Frequent Poster
Posts: 383
From: Your Nightmares
Registered: NOV 2000
posted 05-12-2001 09:38 AM
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I'd say 30-40 minutes.
And by the way, use 300ml hexamine/ammonium nitrate, but use a 1000ml beaker and 500ml nitric acid.

[yt2095]

having just obtained 1Kg of hexamine for camping purposes (yes really for camping!)
i thought i`de try a little bit of it to see if i could make some HE, not a huge amount, just enough for a decent cracker.
i figured this thread was as good as any to post my results.

1) i dissolved pure hexamine in distilled water (standard RTP) to make a saturated soln.

2) fuming nitric and the hexamine soln was then put in the fridge to cool to 7c

3) to the 10ml of cooled hexamine soln, i added 2ml of cooled nitric

**at this point the whole lot almost solidified and warmed slightly??? (herein lies my question/curiosity)**

4) the remainining acid was added after, to a quantitiy of 20ml then stired.

the wax like precipitate then became more mobile after the remainder of the acid was added.
no further warming was detected and it was left for a further hour in the fridge, with intermitant stiring at 5min intervals. there has been no observable change thus far.

heres what i`m fairly sure of, it is not RDX as i`ve never heard of such a yeild in an improvised method before and certainly non instantly! also the smell is that of nirtic acid now.
there were no NOx fumes and i did suffer a little local heating (although only minor)
i`m also positive that the hexamine soln wasn`t re-crystalised by displacement or temperature factors, as hexamine is base and both soln and acid were at same temp.

it`s clearly made a "salt" of some sort with a low water soluability.

could it perhaps benefit from heating now (70c) for 15 mins? could it be a DI or MONO nitrate?
lol, could it even be RDX? (now that IS a dream!) :)
if anyone could shead any light on this little experiment/mess about of mine, i and maybe some others would be gratefull!

cheerz`n`Beerz

[mongo blongo]

There is no way it could be RDX with that much water about diluting the HNO3. This method is quite close to that of making HDN and the product sounds like HDN so it's Heximine Dinitrate me thinks.

[kingspaz]

i agree with mongo. the amount of water in your mixture reulted in a larger dissociation of the HNO3 so it becomes a classic acid/base reaction.

if you filter the HDN out you can use it to make RDX. HDN is also an explosive by itself, but not as good as RDX :)

[yt2095]

cont...

on revisiting my experiment, it would seem that 24 hours in the fridge has produced some changes?
the wax like crystals and clumps have begun to dissolve? leaving a murky white mobile soln with a sweet "ester" type smell, the nitric acid odor has gone now?

i added 10ml of water to test soluability of the precipitate, it dissolved and became a clear liquid. a subsequent ltmus test showed acidity.
i then dissolved more hexamine in this until the soln PH began to rise towards the neutral but still slightly acidic. i plan on crystalising this out to HMD.
if anyone can find a flaw in my plan please let me know :)

the above has generated a few new ideas as for further experimentation as i sit here housebound with a broken leg in my lab and will be for the next 6 weeks :( (so i`m on a mission to explore Hexamine as it`s my latest lab chem).

Ideas:
hexamine chlorate?
electrolysis of hexamine and its compound?
hexamine as a fuel in KNO3 rockets or other oxidisers?
hexamine to ballance O2 in other HE compounds?
Hexamine Borate (maybe a green fire agent)?
etc...

i shall post results here of anything usefull that i find and welcome any further ideas sugestions over the next few weeks, i aint like i`m goin anywhere or got anything better to do!

all the best :)

[kingspaz]

the reason it has disolved is because HDN is decomposed by water. it must therefore be filtered out very soon after it has been made. it then must be washed with a solvent to remove all traces of water (acetone works good for this).

[yt2095]

Kingspaz,

agreed, i`ve had a good 3 hour+ read of similar rellated threads on here also, it would seem that i should have caged the bird while it was in my hands and didn`t :(
i`ve just wasted a few ml of good chems and have no way to recover a usable product now unless i`m into formaldahyde gas (i`m not) :)

but there`s no such thing as a failed experiment, only more data, and so i now know a way NOT to make HDN (or at least know when it`s best to remove it before breakdown).
i won`t dump this soln just yet though as it maybe interesting to experiment with it further if i treat it as a precursor for something yet unknown (maybe electrolysis?).
as for the other experiments mentioned in last post, i feel confident that it would make an interesting fuel with different oxidisers as opposed to plain old ordinary sugar or charcoal! :)
the HMTD result was suprising also, alot faster than TATP and with the same yeild (still waiting to talking the wife round to filtering it for me or at least bring them to me at seating level)

i was curios to know if the tetramine complex was removable/replacable leaving the hexamethalyne complex free to accept other replacements (Chlorates for example)
using the chlorate ions instead of nitrate. it sounds good at face value, as for its practicability? i`ll have to "suck it and see" :)

Stay safe :)

[Mr Cool]

In my (very limited) experience, chlorate salts of amines tend to be very soluble in water, therefore making hexamine dichlorate from the nitrate and sodium chlorate, for example, might be tricky. Although I have never tried making HDC, I don't know why not! Maybe it'll be one of my next experiments, I need to stay out of the pub for a while because it's eating all my money, so I plan to try some things out. I'll give it a go. Oooh, also, aminotetrazole chlorate! *shudders with fear* Damn it, now that the idea's in my head I'll have to try it out of curiosity. I wish I had safer ideas.

Hexamine makes quite a good fuel in slow burning comps, but I haven't managed to make one that burns faster than the charcoal equivalent. Still, have a play about and see what happens. Maybe for rockets it could work well.

[yt2095]

well, I`ve decided to salvage what was left of my failed RDX/HMD synth, and poured in some 30% peroxide (at least it`s not a total watse) and I do prefer HMTP to to TATP anyway, although the last batch of primer I made was 40% HMTP 40% TATP and 20%AN in a plastic drinking straw.
I know the OB was still in the minus but it did seem to be an improvement on TATP alone (based on identical circumstances and using a sound and metal bend test).
so all`s not entirely lost.
I`ve spent the last hour drawing up a chart for intended experiments and their tests.
the tests I have listed so far are:

immediate observations, Impact, heating, storage and burn rate.

if anyone can think of any more that would be helpfull (and practical in a home Lab) and would be of benefit to know in my results please let me know. (try to keep them applicable to indoor lab tests as outdoor activities are boycot for the next 6 weeks).
I may as well make a good job of this, fuck all else do in the day!

Edit: I`ve considered burn temp and gas volume per gram, but without the correct equipment I`de have no way to accurately measure these, so if any improvised ideas regarding this also would be appreciated (I considered a bell jar and water displacement... no bell jar :( )

Additional: (so as to avoid post whoring), I`ve completed and tested an RDX synth, HOLY CRAP! is that stuff powerfull!!!
that brings me to a conclusion though with regards to my H.E experiments. I`m quiting HE but would like to thank ALL of you for satisfying my curiosities with respect to these particular energetic materials, they`re not for me however. It`s nothing to do with being chicken or the drain on my chems or other factors, it`s simply that I`ve made them now
(TATP,HMTP,RDX,NG,NC,ANNM) and am now satisfied with the experience I`ve had with them and it`s time to move on (no NOT to louder things :) ).
I think my heart lies in Pyro and the art of it, and the love of pure Science!
I hope as a result of my quiting HE doesn`t lose me any respect I may have had on the forum.

All the best :)

[froot]

firstly greetings to all, its my first post (please don't kick me off!)
Suppose one tried to make RDX according to the meglomania method using the 2nd method:
I dreamt the following:
The chemicals acquired were as pure as perfect and not cheap! The amounts were accurately measured out according to the method. I wanted this to be perfect. 105g of AN added to the anhydride. It did not all dissolve. So then it was suspected that it would dissolve better when heated as instructed to 90 degrees c. It was heated in a water bath. Well THIS is what happened. At about 65 degrees c the concoction started bubbling and the surface frothed up like a cuppachino. The AN at the bottom became all fluffy. Stank me out of the place. I assume something went wrong!!!??! It didn't even get to the paraformaldehyde stage.
Any speculations?

[yt2095]

re: a few posts ago (and I know it doesn`t technicaly belong here)

hexamine and Boric acid does recrystalise perfectly. it has a HINT of a green color when it burns (not easily self sustaining) and exhibits a "pharohs(sp?) snake" type effect, when forcibly heated.
large amounts of unreacted carbon remains.

conclusion; a waste of good chems and lousey as a Green Star mix.
Additional: KClO3 + hexamine, burns well, but the MPs are too different, the hexamine strats to burn as normal, then eventualy the chlorate kicks in when it`s reached sufficient temprature, very bright though! and virtualy smokeless, leaves a white residue, perhaps a more imtimate mix and finer mesh is needed?

[zeocrash]

I hear that the yield of RDX from the K process can be improved by mixing AN and Hexamine into the nitric acid instead of just hexamine.
i was wondering if anyone had any info on this process.

[kingspaz]

i think it works on the principle that ammonium nitrate in solution is in equilibrium:

NH4NO3 <=> NH3 + HNO3

the ammonia from this reacts with the formaldehyde by-product from the nitration of hexamine to RDX to form more hexamine. since the ammonia is used from the above quilibrium HNO3 is produced which then goes on to help in the nitration.

well, thats the way i think it works.

[mongo blongo]

Yes that's right. I was thinking that in the Hexamine Dinitrate/HNO3 reaction, formaldehyde is also produced. So I wonder what the yield would be like if you used the HDN/HNO3 reaction with ammonium nitrate? ;)

[MBialy]

Does someone know if H2SO4 is soluble in chloroform? I'm thinking about extracting HNO3 from a mixture with H2SO4 using a solvent like chloroform.
HNO3/chloroform mixtures are sometimes used in the laboratories to make nitrosubstances so why not try to use it to make RDX?

[0EZ0]

Very interesting. This might actually help explain why Hexamine can be nitrated to HDN using NH₄NO₃ and HCl. The Hex is decomposed into formaldehyde and ammonium chloride with hydrochloric acid. With the dissociation of NH₄NO₃ into HNO₃ and NH₃, the formaldehyde is taken up by the NH₃ and produces more Hexamine while leaving HNO₃ to nitrate any Hex in the solution. Mind you it probably doesn't happen like that at all. Reading up on the synth of HDN on Mega's site, it says that other metallic nitrates can be used in the nitrating mix with HCl.

I'm sure the dissociation of NH₄NO₃ into NH₃ and HNO₃ only happens when AN is heated in a solid state and not in solution. Like kingspaz noted, the reaction reaches an equilibrium.

NH₄NO₃(s) + Heat <----> NH₃(g) + HNO₃(g)

The below reaction takes place usually inside the molten mass of NH₄NO₃. When held above it's melting point, it decomposes more in favour of the below equation. Industrially this process is used to produce N₂O.

NH₄NO₃(s) + Heat ----> N₂O(g) + 2 H₂O(g)

Although with further searching, I found that the Chloride ions catalyze the decomp of NH₄NO₃ with the following reaction. Again, I think this only happens in solid state.

5 NH₄NO₃ ----> 4 N₂ + 2 HNO₃ + 9 H₂O

With the above equation, it would suggest a different reaction in the NH₄NO₃ and HCl route to HDN.

To try and understand what is going on, I'll just show a few workings below. Since I'm kind of new to this, there are bound to be a few errors. Please feel free to correct any mistakes I have made.

When NH₄NO₃ is added to water, it dissolves endothermically according to the equation below.

NH₄NO₃(s) + H₂O(l) ----> NO₃^-(aq) + NH₄⁺(aq)

When HCl is dissolved in water to get hydrochloric acid, it follows the reaction below.

HCl(g) + H₂O(l) ----> H₃O⁺(aq) + Cl^-(aq)

Also since the concentration of HCl in water is only around 30%, water also adds to the ions in solution.

H₂O(l) <----> H⁺(aq) OH^-(aq)

Below is an equation to show how hex can be re-formed from ammonia and formaldehyde.

CH₂=O + NH₃ ----> CH₂=NH + H₂O
6CH₂=NH ----> C₆H₁₂N₄ + 2NH₃(g)

What do you guys think? Am I just rambling about complete crap?

A few references.
http://www.sciencemadness.org/talk/viewthread.php?tid=24&page=1
http://www.sfc.fr/Guiochon%20VO/decompositionVO.htm
http://www.roguesci.org/megalomania/explo/hexamethylenetetramine_dinitrate.html

[mongo blongo]

MBialy- that will work. Cheak out a patent (which you can find in links and lit) about solvent extraction with Dichloromethane. IIRC it has some additional experements with chloroform or maybe just some experemental data (Can't rember very well :) )

[Mr Cool]

Be warned, you will need a lot of dichloromethane. And I think chloroform was less effective, so you will need even more of that...
But it does work.

[MBialy]

Non-reactive solvents for HNO3;

1) chloroform
2) dichloromethane
3) diethyl ether
4) tetrachloromethane
5) nitromethane

And many more that I don’t now :) The solvent must not dissolve H2SO4. If I’m not wrong ether dissolves H2SO4. For any information about solubility of HNO3 and H2SO4 in those solvents will be very helpful. Mongo-blongo what is this IIRC? A looked a the http://ep.espacenet.com and did not find any patents.
Maybe I wasn’t using the right words? Could you sent me those patents or give
www addresses? I can repay by giving information about TACOT (tetranitrodibenzo-1,3a,4,6a-tetraazapenthalene) it’s nothing special but…

[knowledgehungry]

Dont withold information if you have it, The purpose is not for "trading" information. It is for sharing it.

[yt2095]

if I`m not mistaken, ether is a by product of H2SO4 and Ethanol, it deydrates it by removing the (OH) ion.

and I`m fairly certain (but could be WAY wrong) that Chloroform will decompose in H2SO4 liberating Chlorine gas?
but as I said, I maybe wrong and it`s something else I`m thinking of?

[MBialy]

Originally posted by yt2095
if I`m not mistaken, ether is a by product of H2SO4 and Ethanol, it deydrates it by removing the (OH) ion.

and I`m fairly certain (but could be WAY wrong) that Chloroform will decompose in H2SO4 liberating Chlorine gas?
but as I said, I maybe wrong and it`s something else I`m thinking of?


Your right the solvent also shouldn’t react with H2SO4. Is it sure that chlorofom reacts with H2SO4? If we’ll use stechiometric mixture of H2SO4 and KNO3 (actually with a little excess of the last one) there probably won’t be any problems. But I’m not quite sure if all H2SO4 reacts with KNO3, so even an excess of KNO3 won’t work (see=> KNO3+H2SO4<=>HNO3 + KHSO4)!

[yt2095]

Ether (if pure) would be a safe bet then, I wasn`t 100% sure if I was right though, so thnx also ;)

Chloroform if I remeber correctly was made with "bleaching powder" (probably a HypoChlotare of some sort) and ethanol, then distilled.
I can`t be certain but I THINK it breaks down in H2SO4, try a bit and see I suppose?

all the best :)