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Madog
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Hexamine Diperchlorate
i have always been interested in perchlorates. so today i decided to make hexamine diperchlorate.
i took the method for hexamine dinitrate off of Mr Cools site and subsituted the NH4NO3 for NH4ClO4. i also cut the ratios in half.
i added 5 grams of NH4ClO4 to 17ml of 28% HCl. i swirled it to disolve the HCl. of course it didnt all disolve so i added 15ml of water, most of it
dosolved but there was still NH4ClO4.i poured off the liquid onto 2.5g of hexamine and stirred for a couple seconds as the solution turned white with
precipitate. i quickly filtered it and washed with acetone.
i dried it, i got about 2 grams. i burned some after it dried and sometimes it burns fast, sometimes it pops, and sometimes it crackles. it leaves a
black residue. i also hit some with a hammer on an anvil, it goes off unreliably, but the hammer i was useing is small.
i might detonate it. has anyone else made any other perchlorates?
Most people outgrow their pyro tendencies, we are the ones who\'s tendencies outgrew us.
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DeusExMachina
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do you have any pictures?
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Madog
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nope, i can take some if u want but theres not really much to see, it looks like HDN. a white crystaline powder.
i am probaly gona make more and detonate it
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DeusExMachina
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well, a better idea would be to try to take a few pictures or maybe even a movie clip thing of the detonation since looking at a picture of white
crystals isn't the most exciting thing.
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Madog
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yeah, i will at least take pics of the damage and charge, etc. the standard set of pics for a det
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kingspaz
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don't you just have hexamine dichloride?
ClO4- is a weaker base than Cl- so when you mix a perchlorate salt with HCl you just get a solution of ammonium perchlorate in HCl. you need an acid
stronger than perchloric to make perchloric from it. like HSO4- is a weaker base than NO3- so when you mix a xNO3 with H2SO4 the NO3- accepts H+ in
preference to the HSO4- therefore making xHSO4 and HNO3.
of course you could look at it another way. in the solution you have Cl- and ClO4- aswell as H+ and NH4+.hexamine forms salts by the nitrogen forming
a dative bond to an H+ through its lone pair. ClO4- being a weaker base than Cl- will give up an H+ more easily. therefore it would be more stable to
have an ionic lattice of ClO4- and hexamineH2^2+ than Cl- and the hexamine since there would be a more mid way equilibrium between the reaction as the
Cl- holds onto its H+'s better. so even though no free HClO4 forms the salt can still be made, provided what i said above is correct....can somebody
verify this?
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kingspaz
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scrap my first line of the my original response above.
dam not being able to edit!!!
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Madog
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hmm, it definately seems to have formed. it is definately explosive. i have read about a method for makeing HClO4 with HCl at
http://www.geocities.com/CapeCanaveral/Campus/5361/chlorate/...
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rikkitikkitavi
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mixing NaClO4 with excess of HCl preciptates NaCl almost fully , since it shows little solubility in excess HCl. Left is
HClO4-HCl solution which easily can be separated by distillation since they differ so much in boiling point at their aezotropic points. This is a
method used in the industry today, when more exotic methods of membrane technology -eletrolysis isnt used 
BTW :I could kill for a cation-anion exchange membrane for making f e x sulfuric acid and lye from
sodium sulfate by electrolysis
/rickard
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madscientist
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Wouldn't it be possible to prepare purer hexamine perchlorate by reacting moist ammonium perchlorate with hexamine? It should generate ammonia gas
while preparing hexamine perchlorate - the fact that ammonia is a gas at STP should drive the equilibrium far to the right.
(CH2)6N4 + 2NH4ClO4 ----> (CH2)6N4*2HClO4 +
2NH3
I weep at the sight of flaming acetic anhydride.
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Madog
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that looks cool, maybe i will try that, i am going to make more for the detonation. i would also like to make some good HClO4.
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osamafon
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2NH4CLO4+H2SO4+xH2O
I think your hexamin perchlorat is not dry
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Madog
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its fairly dry, i washed it in acetone, it originaly wasnt burning well before it was dried all the way but now it is. i just made a new batch, 4
times the original one.
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osamafon
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how fast does it detonates? /\
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Madog
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im not sure what the detonation velocity would be but i would say its in the 7000s from waht i have heard about hexamine dinitrate. the hexamine
diperchlorate will kinda melt then crackly with little flames then it all deflagerates fast, like a little explosion, not like AP tho, not nearly that
fast.
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osamafon
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why all n`s are not forming bonds ? Has some one detonated it? sorry obout my english.
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Madog
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aye
what are you talking about? i detonated a little in a .45 with a small amount of HMTD.
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osamafon
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hexamin has 4 amin groups why not hexamin tetraperchlorat? how strong was it?
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Madog
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it was good, i just chucked it into the snow, so i cant really measure that, ill have to try a gram on a piece of plywood. a prpoer test.
i dont know, i have read that its "dibasic" which aparently means that 2 HNO3, HCl, HClO4, H2SO4, etc can bond to it.
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Madog
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today i took a small cardboard tube and put 1 gram of hexamine diperchlorate in it and packed about 1/2 gram of HMTD ontop of it, and chucked it in
the back yard. it was pretty damn loud.
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Haggis
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Would it be possible to replace the ammonium perchlorate with a chlorate? I do not have any perchlorates, but I do have potassium chlorate. Can this
same method be used for all of the nitrates/chlorates/perchlorates by just changing the oxidizer used?
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Madog
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i supose, but it would just be insane. HClO3 is completely unstable explosive. NH4ClO3 is also insanely unstable. chlorates as a group are very
unstable, and more willing to give up their Os than perchlorates are.
so, i highly doubt hexamine dichlorate would exhist, and if it does you dont want it if you enjoy fingers.
edit: ammonia salts are mainly used just for their solubility
[Edited on 2/28/03 by Madog]
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Haggis
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Thanks for the bit of information regarding chlorates. I think that I shall do ammonium nitrate now like suggested instead of a chlorate.
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Madog
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ok, just a warning, yields suck. if you have HNO3 to make hexamine dinitrate use that, yields are far better and its purer. expect about 3 grams from
5g of hexamine for hexamine dinitrate
[Edited on 2/28/03 by Madog]
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Haggis
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Does the acid used matter? I mean, you mention using HCl...I was wondering if the reaction depended on the Cl or is it just using the hydronium ion.
I'm guessing that H2SO4 would work. In the reaction, I believe ammonium chloride is formed. Ammonium chloride, IIRC, is listed as incompatable
with acids. Ammonium Sulfate, IIRC is compatable. Therefore, if it works, I would think that H2SO4 would be a good choice instead of HCl.
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