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Author: Subject: One-Pot Synthesis of Hexamine Diperchlorate
VSEPR_VOID
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[*] posted on 7-8-2018 at 09:48
One-Pot Synthesis of Hexamine Diperchlorate


Hexamine Diperchlorate is a very stable energetic compound that burns when melted violently. It has been produced in the past by the neutralization of a solution of hexamine with perchloric acid. A simpler method has been devised and tested which involves the production of perchloric acid in situ. This requires less time and no previously prepared solutions of perchloric acid.

40 Grams of ammonium perchlorate (99% Ebay) was added to a 150 ml round bottom flask (rbf) and then partially dissolved in 60 mL of water. Some of this water was used to wash the neck of the flask. To it 17 grams of concentrated sulfuric acid (Drain opener, clearish pink) was added slowly. This caused caustic vapors to be evolved. Do not inhale.

To the mixture 23.8 grams of hexamine (99.9%) was added. No attempt was made to add it slowly and no visible reaction was observed. Once the addition was complete the rbf was heated and the solution reflexed. After ten minutes of reflux the solution was left to cool. Almost immediately crystals began to appear. This is presumed to be the final product.

400 mL of water is used to wash the flask and the mixture was filtered. The product was dried on vacuum for 1 day.

The fluffy white powder, who's structure was thin and needle like, was stable upon heating to 60 C when dry and eventually melted to give a black liquid. This liquid ignited with a great forced and burned intensely within fractions of a second.

In the future yields maybe improved by increase the amount of acid added and reflux times.




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[*] posted on 8-8-2018 at 23:40


Why did you reflux the solution? This is an ionic reaction and once all solid has dissolved it should be OK. The salt will precipitate.

Do you have any idea of purity? Try the following:
- After formation of all crystals and good cooling down (e.g. in fridge), filter and dry the solid mass between coffee filters.
- To the still somewhat humid mass add a small amount of water and heat until boiling. If not all solid dissolves, then add a little more water, until all of it has dissolved.
- Let the liquid cool down and wait for formation of crystals again. Again filter and dry between coffee filters. Next, allow to dry for one day and then do your tests again.

This sounds like an interesting test. This may be a nice little weekend project for me as well. I have some technical pyro-grade NH4ClO4 (from eBay) and as I do not do any pyrotechnics (totally forbidden in NL), this may be a nice use for this otherwise fairly useless chemical.




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[*] posted on 9-8-2018 at 11:14


Ammonium perchlorate is not exceedingly soluble in water, thus I needed to heat the solution to ensure that it all reacted with the sulfuric acid to give perchloric acid. Reflux was used to ensure that none of that perchloric acid was lost.

I wonder if urea would form a similar compound.




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[*] posted on 10-8-2018 at 14:07


What is the melting point of hexamine diperchlorate? Was the compound hygroscopic at all? Could there have been any hydrolysis to form other products as well? Also see this thread here: https://www.sciencemadness.org/whisper/viewthread.php?tid=67...

[Edited on 10-8-2018 by nitro-genes]
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[*] posted on 11-8-2018 at 04:39


What is the VoD for HDP?
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[*] posted on 11-8-2018 at 06:34


Maybe next time you could heat ammonium perchlorate in water to dissolve it before you add the other chemicals. Probably it is not necessary, but I would do it just to be sure there are no decomposition reactions because of the heat.

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[*] posted on 11-8-2018 at 06:42


ammponium perchlorate on ebay?!? I can't find it, and i shop there way more than I do Wal-Mart



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[*] posted on 14-8-2018 at 01:55


Thats strange. I cant find a record of it on ebay. It must have been Amazon then.

Quote: Originally posted by underground  
What is the VoD for HDP?


I have not come across any data on that but I can say for sure I have not observed any samples detonating upon heating or shock.

[Edited on 14-8-2018 by VSEPR_VOID]




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[*] posted on 14-8-2018 at 02:34


So HDP is not detonatable? If it is not then what is its purpose? rocket fuel?
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[*] posted on 16-2-2019 at 14:40
CHP


@ VSEPR_VOID

I've tested your NH4ClO4 + H2SO4 + hexamine method. Yes, a white fluffy powder is actually created. Which becomes dark after warming, is a smell of formaldehyde. It burns violently, similary as ETN. The powder is not detonable. It also agrees. I probably did not understand his end use. However, if you have NH4ClO4 and hexamine, you can more easily synthesize CHP. More precisely, Tetraamine copper - hexamine diperchlorate. Abbreviated = Copper Hexamine Perchlorate = CHP.
The basic ratios are almost same according to your description. I recommend testing the synthesis of only a small amount, that is, only 10% of your description. Thus: 4 g NH4 ClO4 + 2.38 g hexamine. As a copper source, 1.06g CuO should be used. And as the solvent NH4OH 20-25% in aq. of 12 grams.
All components are mixed together in a sealed chemical tube. The rubber plug is enough.
This mixture is heated to 70 degrees Celsius. For example, in a water bath. The mixture is shaken at this temperature for about 10-15 minutes. Be careful, about 1 bar will be pressurized in the tube. If all CuO disappears from the bottom of the tube, the reaction is complete. And all crystals should be dissolved. In tube now will dark blue solution. It require (maybe) increase temperaure on 80 Celsius on short time, (30 seconnds) for dissolving all agglomerates.
After cooling in ice bath you can separe crystalls from mother liquor.
Do not use paper filter. Solution is powerful Schweizer reagent, which dissolve any organic material. Drying process can run on any inert surface. Glass, ceramic, tephlone, stainless steel. Temperature of surface can be 40 - 50 Celsius. Drying takes about 10 minute. Is incredible fast, thanks to evaporate NH3 + Water together. Storage can be CHP in close jar. Thats all.
You obtain energetic material that you never dreamed about. At testing on the Anvil you use ears the plugs......:cool:...LL
Yield should be 3,2g CHP

[Edited on 16-2-2019 by Laboratory of Liptakov]




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[*] posted on 16-2-2019 at 22:33


HDP can be detonated and it is 125% equivalent to TVT
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[*] posted on 17-2-2019 at 13:00


Yes. A eutetic mixture of hexamine and AP is quite powerful and even mouldable.

LL. I have tried this with CuO. It’s a f***ing nightmare. It hardly dissolves the CuO and then I have to figure out how to separate it from the TACP... and since water tends to destroy TACP it’s REALLY difficult. My CuO is dust too. I use 10percent ammonia... but I would think this would be fine, it works with Cu just fine. But. Yah. CuO is a nightmare, it sucks to use 2 gallons of water to dissolve the TACP from the CuO, boil it down to 300ml and then add ammonia.
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[*] posted on 17-2-2019 at 13:56


MineMan, you need 24% ammonia water, or higher. After all will works according description. In one flask you can boil 10% NH4OH (cca 300ml) and NH3 gas insert bubble throught your TACP solution, which must be cooled on - 10 C. TACP will precipitated and solution will look as light blue color. This is maximal yield.



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[*] posted on 18-2-2019 at 03:04


Quote: Originally posted by MineMan  
Yes. A eutetic mixture of hexamine and AP is quite powerful and even mouldable.


HDP is not an eutetic mixture of hexamine and AP but a Perclorate salt of Hexamine. It is produced by neutalization of hCLO4 with Hexamine
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[*] posted on 18-2-2019 at 08:24


Is possible melting process Hexamine + NH4Cl04 1:1. For example 0,2g Hex + 0,2g AP on the spoon. Melting point I estimate about 200 C. Arises plastic material, which look as the Honey. Color and behavior are very similar, at 20 C. Process require very carefull heating. Because the higher temperature decompose this material on formaldehyde. (smell) Or explosion, of course. Material is hygroscopic. At strong heating over 300 C follow decomposition on black color. After follows long high flame, without residuums. Very similar behavior as at heating ETN.....:cool:....LL



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[*] posted on 19-2-2019 at 16:38


Correct LL... but 15 percent hexamine is better. It works well in a toaster oven. I know underground that it’s different, but still similar.

LL, the issue is separating the copper oxide from the TACP... as much water is needed to dissolve the TACP...
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[*] posted on 19-2-2019 at 22:14


@Mineman
Is possible casting process 15% hexamine + 85 NH4ClO4? Nothing detonation during preparation? It is maybe miracle.

I dont understad, what you do it with TACP. How separation CuO? Ratio for reaction AP 1g + 0,266g CuO is exact. Reaction must be complete without CuO on bottom. Nothing CuO in TACP shlould by to be. And if yes, your CuO is dirty, contaminated. Crystals TACP are much bigger than residuum CuO. Filtering on fine sieve (not filter paper) is question of a few seconds. For separation crystals of TACP you not need some external water.




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[*] posted on 23-2-2019 at 02:08


Not castable LL.

[Edited on 23-2-2019 by MineMan]
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