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Author: Subject: Hexamine Diperchlorate
Madog
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[*] posted on 7-3-2003 at 12:31


hm, well, what i meant is that the acid would(or at least should) connect to the hexamine makeing hexamine disulphate, etc. but that brings up a cool idea, i dunno. it does make NH4Cl, i saw it, i filtered it off. the reaction only depens on the H.

of course, if you have HClO4 that would be a hell of alot better than a mix of NH4ClO4 and HCl.

edit: o yes, also, i dont really know anything about the compatability with acids of NH4Cl or NH4SO4, etc

[Edited on 3/7/03 by Madog]
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smile.gif posted on 23-3-2003 at 16:05


Most perchlorates amines are:
*more brisant
*denser
*have higher VODs
*display higher lead block test expansion
*much more impact and heat sensitive

than their nitrate sisters!

Sole possible partial exception to this is hydrazine perchlorate!

hexamine diperchlorate makes large diamond like cristals when you evaporate in the air at ambiant T a saturated solution of hexamine neutralised with diluted HClO4... the stuff contains a lot of hydratation water (like hydrazine perchlorate); thus when you heat it it melts fast, and while water evaporates it already decompose a bit; then when it reaches dryness it burns fiercely with cracks and a blueish flame!
When confined with Al foil those hydrated cristals explode when trown in a fire!

The diperchlorate suffers from hydrolitic unstability more than the dinitrate does!

During melting of the dinitrate and of the diperchlorate of hexamine; there is formation of methylamine salts!

CH3-NH2.HNO3
CH3-NH2.HClO4

Both salts are prompt to start an explosive detonation in the molten mass of the hexamine salt; the second one being critical!

Beware of transition metal contact copper, iron, nickel, ...because danger is even bigger than with ammonium salts to make corrosion and formation of nitrate or perchlorate of those metals and subsequent complexation into sensitisers inside a much more sensitive matrix!
:):):D:D;);):P:P:cool::cool:




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[*] posted on 15-8-2005 at 10:02


Sorry for digging out a such old topic but ive a few questions. Philou, you said, that the HDP contains water. What are the effects of this crystallwater on the explosive strength and on stability as well as the sensivity? Well..... i made HDP. I disolved the Hexamethylenetetramine in destilled water (hot). Then I added HClO4 (70%) dropwise. The solution warmed up again. Ive to say that i worked in the scale of a few grams. I then prepared an icebath (crushed ice with ethyl alcohol). I put the beaker in this icebath. The solution turned milkey. After 2 mins it was a thick slurry. I filtered and poured a few ml of acetone ovr it. Then i took the HDP and put it in 20ml of acetone. I stirred well and filtered again. The product was dry within 2 hours. It burns really fast. Much faster than the nitrate salt does. The flame uppon burning is extreamly bright! So thats what i made. Now Ive a few questions. As i already said before the think with the crystallwater. Then is there a possibility to get out that water (exept of heating it)? Is it possible to detonate it with the water in it or must this be out? All data about this stuff is welcome. thx in advance! :cool:



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[*] posted on 15-8-2005 at 12:24


I should think if you soak the diperchlorate salt in acetone or dry ethanol, you'd remove most of the H2O providing the crystals are small. I can't imagine H2O binding is so strong (as with anorganic salts) that the water-greedy (as it were) ethanol/acetone wouldnt remove it (it's an equilibrium, that's what I am trying to say, and the crystals contain water that is not contained in the EtOH/acetone, thus it shifts to the right and water is lost)

Anyway, the fact that yours burned means probably it's mostly waterfree anyhow.




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[*] posted on 16-8-2005 at 12:34


Ah..thx for your reply! This is indeet true. I had a similar idea. Now ive a further important question: I read in Federoff (7) that there are 3 forms: The mono-, di- and triperchlorate of hexamethylenetetramine. Now Im a bit confused! Because i always thought that hexamine is a dibasic base. So: can anyone tell me, if this information is wrong or if these forms really exist? And if they do: How is it possible to get the different forms? I hope that someone could give me an answer. Because im really exited about this energetic material. I could test the meltingpoint of my perchlorate. Because the mono and diperchlorate differs up to 100°C in its mp. (mp of the mono is arround 240°C if i remember correct and the one of the di is arround 340°C). My problem: I only have a normal heating plate (like the one in your kitchen). It has 3 levels. I dont know how to test the mp with this plate. It should be said, that the monoperchlorate has about 65% of the power of TNT and the diperchlorate 125% of the power :cool: !! Its nothing written about the triperchlorate....but i think you can imagine how powerfull this must be (if it really exist). I thank you all in andvance and hope for an answer.

[Edited on 16-8-2005 by Kinepak]




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[*] posted on 16-8-2005 at 13:49


Three to four times the stoichiometric amount of HClO4 should do the job (as the acid form). If it is soluble try and precipitate it with EtOH or acetone, it should be insoluble, and then it's likely that you will preciptiate the 3-perchlorate salt.
Stoichiometry ultimately determines which salt you end up with, so I don't think you need to bother with an MP apparatus etc. The reason being, it is highly unlikely that i.e. the diperchlorate precipitates, while one moiety of HClO4 remains in solution...

By the way, how does the your prep so far behave, is it very hygroscopic?
The triperchlorate may be just a little less stable, and leech HClO4. But then, it's a very strong acid. Should be interesting to see!




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[*] posted on 16-8-2005 at 14:21


Thx for your answer. So you mean, if i use the stöchiometric amounts for the diperchlorate, ill get the diperchlorate? And if i use less, ill get the mono, if i use more HClO4 ill get the triperchlorate? That would be great. Is it possible to get tetraperchlorate? And why does the trinitrate not exist? Strange :D
I would produce the diperchlorate because i should be ideal (stability and power). What do you mean with the acetone or ethyl alcohol precipitation? Wich form do you mean? The monoperchlorate should be more watersoluble than the di- or triperchlorate right? My product is absolutely NOT hygroscopic (as far as i can say yet). I left it in a moit room over the night and nevertheless the perchlorate got drieer than yesterday. Its perfectly dry now! Ill make 3 batches tomorrow: one with the stöchiometric amounts for the mono-, one with the amounts for the di- and one with the amounts for the triperchlorate. Thats what you mean. You said that i should use a lot of excess HClO4 for the triperchlorate. Should i use a excess for the diperchlorate too?




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[*] posted on 16-8-2005 at 15:24


Lol, you are confusing yourself!
Yes use 2 mole HClO4 per mole of hexamine for the diperchlorate, and 3 mole of HClO4 for the triperchlorate, I wouldnt use an excess otherwise you'll get a mixture in teh end.
I don't know about the tetraperchlorate, it doesn't always work that way. There are plenty of examples where the theoretical salts do not form, presumably because of the crystal structure precluding addition of further acid.
For making the triperchlorate, I'd rather drip hexamine solution (1/3 in molar quantity) into a pot of dilute HClO4, so as to make sure that the diperchlorate doesn't form first. Then, if it is soluble, precipitate the salt with a large amount of cold acetone or ethanol.

Interesting that it's non-hygroscopic, that's good.




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[*] posted on 16-8-2005 at 17:12


Would there be a danger of ethyl perchlorate forming if there is a little excess acid?
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[*] posted on 16-8-2005 at 17:29


I really doubt ethyl perchlorate could be formed in this reaction.



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[*] posted on 16-8-2005 at 18:35


Sorry, I should have been more clear. I was referring not to the reaction itself, but chemoleo's crash percipitation in EtOH.
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[*] posted on 16-8-2005 at 18:55


Nah, I doubt that once again.
Even if you get a tiny amount (it's an equilibrium after all, although a slow one) it's still massively diluted. Plus, normally these sort of reactions require strong dehydrating conditions (i.e. presence of H2SO4 etc), and often heat.
Anyway, it may be insoluble, so not necessary int he first place.

[Edited on 17-8-2005 by chemoleo]




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[*] posted on 17-8-2005 at 01:05


Youre right! It was late and i wasnt fit enough. Thx for your advice. I can say, that its not hygoscopic. Great if you keep in mind that the urea salt is extremely hygroscopic. I made this one time.....i couldnt even reach precipitation. But i know someone who had real crystals. These became liquid again after a short time. I dont like this excess procedures. The HClO4 that i use is so precious. I dont want to waste it that way. But if i want the perchlorates of hexamine there probably is no other way. You earlier said that the triperchlorate could be less stable and release HClO4 right? Hmm.....that would be bad. Badly i dont understand that mechanism (of the forming of the different forms) really good :(. The real problem is to say under wich conditions the diffrent salts are forming. How much excess. To make it concrete: If I add 1mol of HClO4 to one mol of hexamin.....wich salt would be formed? Is the hexamine converted to the monoperchlorate (in theorie all should be..but there would be still unreacted hexamin and HClO4 left)? Or is the half of the hexamine converted to the diperchlorate? This is my biggest problem. Sorry if this sound stipid and if you explained it one or two times. But ill try it as you said and post the news as fast as possible. Ill make it that way: I take one g of hexamine and dissolve it in 2-3g of destil. water. This solution is then dropwise added to 8g of 70% HClO4. In this case ill have a great excess of HClO4. Ill precipitate it out with acetone. Is there any dangerous reaction between the HClO4 and the acetone? The HClO4 should be dilutet. But i know: perchloric acid + organic things = BAD. If there is something i could dilute the 70% HClO4 down a bit.
The stuff i get out of this reaction is then compared with the one i got out of the stöchiometric reaction for the diperchlorate.
Thx again to all who posted and helped me!




[Edited on 17-8-2005 by Kinepak]




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[*] posted on 18-8-2005 at 06:55


Here are the results of my little test (double post....sorry...but thats worth a new reply):
1g of Hexamine was dissolved in 3g of hot destil. water. This solution was dropwise added to 8g of 70% HClO4. The thing turned milkey as soon as the addition was started. After all of the Hexamine solution was added the whole thing was cooled in an icebath. Then this sludge was dropwise added to about 20g of acetone. The white precipitate settled on the bottom. The mix was stirred well and then filtered. Then the white mass was put in another beaker with 20g of acetone. Again the mix was stirred well an then again filtered. Then the precipate was dried at roomtemp. . Now its perfectly dry. It is very very very!!! fine!! Finer than flour....finer than everything that ive see until yet :o . Upon ignition the Hexamineperchlorate burs very quickly and much uniformer that the previous perchlorate does. The flame is very bright too. Thers less residude (black) than from the previous perchlorate. Now to the experts: what is the mainproduct i got? for shure not the monoperchlorate. Ill try a comparison between the two products in a burning-test, hammer-test, solubility-test and a meltingpoint-test. Further advices and/or incitation? Please post!

[Edited on 18-8-2005 by Kinepak]




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[*] posted on 18-8-2005 at 12:27


Well that's interesting news.
I suspect it's the diperchlorate as the OB is almost perfect only with the triperchlorate, while C is left over with the diperchlorate (explaining your black residue).
Hmm. I wonder then why the triperchlorate didnt form, it should have formed since you dripped the hexamine (7 mmoles) into such a large excess of HClO4 (56 mmoles). Well. It probably isn't possible by this route. Maybe by metathesis? Might be worth checking out if hexamine forms tri-salts with some other acids, maybe it can then be used for a metathesis reaction.
By the way, it is possible to determine the type of salt (mono/di/tri) by measuring the gas volume that is produced, at RT (allowing it to cool down. That'd need careful design though.

Anyway... do tell us of the follow up tests.

There are plenty other amine substrates that can be potentially tried!




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[*] posted on 18-8-2005 at 23:19


Quote:
Originally posted by Kinepak
Now to the experts: what is the mainproduct i got? for shure not the monoperchlorate.

There is russian patent publication 999122472 (http://www.fips.ru) about synthesis of (CH2NH)4*2HClO4 (!) by the reaction of (CH2)6N4 with HClO4 and next cooling of the mix. Probably, hypothetic (CH2)6N4*3HClO4 just is (CH2NH)4*2HClO4?
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[*] posted on 18-8-2005 at 23:26


Quote:
Originally posted by chemoleo
Might be worth checking out if hexamine forms tri-salts with some other acids, maybe it can then be used for a metathesis reaction.


Well, the only hexamine tri-salts I know of is hexamine trichloride. I dont think there are any other hexamine tri-salts, least say hexamine triperchlorate.
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cool.gif posted on 20-8-2005 at 07:26


Thx for all your replies. So...here are the news for all who are interested:
I made another batch. This time the diperchlorate was the aim and thus the stöchiometric amounts where taken, except of a little excess of HClO4. So 7g hexamine were dissolved in 10-12g of hot water. This solution was added to 16g of cooled HClO4. When almost all of the hexamine solution was added precipitation occured. The whole mix turned into a solid mass :o. Uppon stirring it turned to a sludge again. I know this from the hexamine dinitrate procedure. There was a fast precipitation, too. 10g acetone was added to the sludge. Then i cooled the thing down to almost 0°C. It was filtered. Then the precipitate was added to 25g of acetone (with good stirring). After it was filtered again it was dry within 3h. I got out 11g. This is a only little yield. But say later why. Today i decided to do a few tests with the 3 batches i have. At first i did a solubility-test. The 3 batches were tested with water, acetone and isopropyl alcohol. The results: (sample 1 is the first batch, sample 2 the second [eventually the triperchlorate] and sample 3 is the third batch [hopefully the diperchlorate]. This order applies to all tests). Sample 1: good soluble in water and acetone, not soluble in isopropyl alcohol. Sample 2: soluble in water (not as good as sample 1), bad soluble in acetone and not soluble in isopropyl alcohol. Sample 3: soluble in water (like sample 2), bad soluble in acetone and also insoluble in isopropyl alcohol.
Now the burn-test: Sample 1: burned fast and left little residude (black). Sample 2: burned fast (almost as fast as sample 1) and left a little less residude than sample 1. Sample 3: burned not as fast as sample 1/2 but also acceptable. It left also little residude.
Additional info: All samples could be initiated with a hammerblow!! They went of with a sharp bang. After the detonation there was an unpleasant smell in the air. Also all batches have a similar meltingpoint. When they are dropped on a hot heatplate, all samples flashed with a slightly lilac flamecolour. The last test i did was an initiation test with AP. About 300mg of the 3. batch was pressed in a drinkingstraw. Then 300mg of AP was pressed on top. Uppon detonation the was white smoke. The detonation was complete.
My conclusion: The mainproduct in all 3 batches should be the diperchlorate. But i dont know the percentage of the different forms. I hope this report is useful for some people. :D
And because of the yield: It seems that the perchlorates are little soluble in acetone.... and thus my yield isnt that good. Next time ill try to wash it with isopropyl alcohol.




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[*] posted on 17-9-2005 at 00:56


GB 168,333 should be of interest to you, KinePak.
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[*] posted on 12-3-2008 at 10:36


I am sorry for diggin out this old thread. Im new and don’t want to start a new one with my first post. Recently I had a closer look at hexamine diperchlorate (HDPC) and another perchlorate-salt. This one is not really worth a new thread: aminoacetic acid perchlorate (glycine perchlorate; GP). I spent a bit of time and here are the results:

HDPC:

I once prepared this stuff by carefully adding hexamethylenetetramine to perchloric acid. The HDPC formed immediately. But the HDPC I describe now was made slightly different:

14g (0,1mole) hexamine are dissolved in 30ml of destilled water. This solution is stirred with a magnetic stirrer. Now 28,8g of 70% perchloric acid (0,2 mole) are added dropwise. The temperature rises a bit because of the dilution of the perchloric acid. At the end of the addition the mixture turns milkey because of the precipitation of HDPC. The beaker is cooled to near 0°C. 25ml of also pre cooled ethyl alcohol is added at once and the crystals are filtered off. They are rinsed with additional 10ml of ethanol (as cold as possible). If spread out the crystals are dry within a few hours. ! Keep ethanol ! It will evaporate and leave an additional amount of HDPC crystals.

The HDPC forms a very fine powder. When exposed to flame it first melts (partially) and then deflagrates violently. It is easily detonated by a hammer blow.
The white powder/colorless crystals are slingtly soluble in water and ethyl alcohol. The solubility in acetone is little. It is not soluble in non polar solvents such as naphta. I noticed absolutely no hygroscopicity. The HDPC dried perfectly. It seemed more stable than the dinitrate which easily releases fomaldehyde. Even when stored there was no smell of formaldehyde. HDPC is acidic and corrodes metals and other material (especially when wet). The effects are not as dramatic as that of HDN.

Maybe HDPC could also be made via HCl and XClO4. But yield will never be that good.

Now to the new stuff: Glycine perchlorate

I found absolutely no information about it. PATR 2700 only mentions the nitrate salt and the nitramine (nitroglycine). But the nitrate salt is said to be as powerful as picric acid.
I started as for HDPC. Dissolved the glycine in a bit of destilled water and adding perchloric acid slowly. Afer addition of acid was complete there was no trace of crystalisation. So the beaker was put in the fridge and cooled to 0°C. Still there was no single crystal. I remembered that urea perchlorate has similar properties (in 100ml water over 900g of urea perchlorate can be dissolved). It is also very hygroscopic and crystals are very hard to obtain. But anyway I gave GP another try. This time with success:

14,4g of perchloric acid (70%; 0,1 mole) was cooled to 5°C and stirred electrically. 7,5g of aminoacetic acid (0,1 mole) was added slowly. The slow addition and stirring is important because there could form hot spots (you know…..perchloric acid and organics aren’t that good). The temeprature of the mix rose a bit. After addition was complete all of the glycine dissolved. The mixture was a viscous and clear liquid. Next step was a bit crazy. The beaker was put in a water-bath and heated to 80°C and held there for 20min. Still it was a liquid. This was crazy because boiling down a solution of an unknown organic perchlorate isn’t harmless. The beaker was put into the fridge. Crystalisation occurred. The crystals were scraped out of the beaker and instantly packed airtight. Tests were performed with the following results:

Hygroscopicity: GP is definitive hygroscopic. If exposed to the air it “melts”.
Solubility: GP is very soluble in water, soluble in ethyl alcohol and acetone. It . is however insoluble in non polar solvents such as naphta.

It builds colorless crystals which melts easy without decomposition. If stored airtight there was no trace of decomposition. When crystals of GP get in contact with flame they first melt (fast and easy) and then burn down with a hissing noise. It looks quite energetic. GP can also be detonated by a hammer blow.
I thought about the existence of salts of GP. So I made a solution of GP in water/ethanol (1:1) and slowly added potassium carbonate. Carbon dioxide was evolved and the solution turned milkey. I put it in a waterbath and evaporated as much water/ethanol as possible. Put in in fridge and got a white powder. Upon ignition it melts and then flashes like potassium picrate or calcium nitronate. I don’t know whether this is a real salt of GP or simply a mixture of glycine and potassium perchlorate (the proton in the reaction could also be from the protonated amine group). Just out of curiosity the lead (or other heavymetal salts should be tested).

I’ll do further tests with both substances and would love to try other perchlorate salts such as methylamine perchlorate (which is said to be a very powerful explosive), guanidine perchlorate (also very powerful), ethylendiamine diperchlorate, hydrazine perchlorate, diaminobenzene diperchlorate, hexamethylenediamine diperchlorate and others.
Maybe someone else is interested in energetic perchlorates (especially the salts; the esters are insane!) and can support my tests.

Btw.: Is it possible to get methylamine perchlorate out of a solution of methylamine hydrochloride (which is easy made out of hexamine and HCl) and perchloric acid? HCl is a stronger acid. But maybe the perchlorate has a lower solubility and thus can be precipitated?

[Edited on 12-3-2008 by enthalpy]
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[*] posted on 12-3-2008 at 16:21


I've made some triperchlorate using perchloric acid solution some long time ago, yes it flashes, it crackles and it can expode, but power is weak compared to conventional explosives, and storage stability is bad. I prefer not waste HClO4 for such useless subject.



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[*] posted on 13-3-2008 at 11:00


Hi Enthalpy,
Good job :)

I also like perchlorates.
CH3-NH2.HCl + HOClO3 will give the desired perchlorate because despite HCl is stronger acid than HClO4, HClO4 is less volatile...but it will release a lot of HCl fumes; so better first allow neutralisation of the amine chloride with NaOH, and bubbling of the gaseous CH3-NH2 into the diluted perchloric acid.

About the triperchlorates of hexamine, it is possible that only strong acids are able of mutiple binding to the third stage...same is seen with hydrazine, of wich disalts are not always possible and occurs only with very strong acids (HCl, HBr, HI, HClO4 and maybe with HNO3). Those are very easily hydrolysable into a mix of the monosalt with the free acid...




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[*] posted on 13-3-2008 at 13:15


Thanks philou.
Do you really think the triperchlorate exist? if yes, it should be possible to prepare it by interaction of excess perchloric acid on hexamine. The water content in the reaction should kept low and precipitation should not be induced by adding ethyl alcohol!! (ethyl perchlorate is insane! I wouldn’t deal with it, even traces of it; someone here did it) the existance could be confirmed by yield and comparison of properties (especially the melting point). This must be done.

To engager: what are you talking about if I’m allowed to ask? Conventional explosives like TNT? Now, the diperchlorate of hexamine is stated to have 125% of the power of TNT. Can you please tell us how you prepared the triperchlorate? besides: the triperchlorate should be even more powerful (because of OB is nearly zero) than the diperchlorate is. In my experience the diperchlorate is a strong explosive. Of course this stuff has no importance in civil/military/industrial explosives but it is still a very energetic one! I would say NH4ClO4 is waste of perchloric acid but other perchlorates of organic bases are interesting compounds.

Switching to the new compound: glycine perchlorate
Do you think that salts of it exist? As I mentioned in the previous post the proton of the reaction could (I think so) be from the protonated amine group. This should leave plain glycine and a corresponding perchlorate salt (eg the neutralisation of a glycine perchlorate solution with potassium carbonate would form glycine, potassium perchlorate, CO2 and H2O). Anyway has someone else prepared this stuff?

The methylamine perchlorate could be made by refluxing hexamine/HCl wich will form ammonium chloride and CH2O. Then methyleneimine is formed which is hydrolised to methylamine respectively its hydrochloride. The HCl evolved upon the interaction of HClO4 should be no problem.

Finally: sorry for shifting this thread a bit off topic but I think other amineperchlorates could also discussed here.
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[*] posted on 18-3-2008 at 10:17


Engager cannot judge it's power, he probably put it in a cardboard tube with a sparkler fuse..... :P

And don't worry enthalpy, there can't be a thread about every energetic amine salt, discussing them and comparing is interesting, even for me who had to dispose off his energetics precursors.

I can see people from a certain forum foam around the mouth at the thought of wasting methylamine.HCl for explosives - that's like an Iranian using Ac2O for camp fuel! ;)
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carbonfeind
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[*] posted on 5-11-2009 at 06:41


Sorry for digging up a thread as old as this, I have some information that might be useful. I use the same synthesis as Madog, though I scaled it up about three times and used less ammonium perchlorate. I also add the hexamine dissolved in water as well as cooling the reactants down to 10 or 5 degrees C before adding the hexamine. HDP is very easy to initiate and I have used it successfully in several shaped charges. Here are a few vids I took. link link

[Edited on 5-11-2009 by carbonfeind]
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