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Author: Subject: NH4 / K Perchlorate
AngelEyes
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[*] posted on 13-9-2018 at 07:23
NH4 / K Perchlorate


So...in the UK it's a pain to get hold of certain materials - conc sulphuric being the latest victim of the state's efforts to keep us all safe.

However, I can still get Ammonium Perchlorate (eBay)...it's not cheap but it's legally purchasable by individuals. It's also not the most useful perchlorate, but it is a perchlorate nonetheless.

I was thinking I could turn it into K Perc quite easily by treating it with KOH. This'd free up Ammonia and water (the NH3 would slowly evaporate off) leaving a solution of K Perc (which itself has poor solubility so should just crash out of soln)

I'd prefer not to have any stray KOH in it though so I figured to add enough KOH to react with 98% of the NH4 perc then add K2CO3 in slight excess to deal with the rest. That'd mean there was a little K2CO3 contamination in the final K Perc, but that's got to be better than KOH contamination.

Thoughts? I'm pretty sure the reactions would work and I can't see any issue with a little K2CO3 contamination.
The resulting K Perc would be used for pyro purposes...so many formulas call for it and, even though K Nitrate is useful, sometimes you just need perc.

...unless anyone knows where I can get K Perc easily in the UK and without an EPP license?

Cheers


Angel




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[*] posted on 13-9-2018 at 08:40


Quote: Originally posted by AngelEyes  
However, I can still get Ammonium Perchlorate (eBay)...it's not cheap but it's legally purchasable by individuals. It's also not the most useful perchlorate, but it is a perchlorate nonetheless.
Didnt you say it's legal? Just go get some from ebay.



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greenlight
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[*] posted on 13-9-2018 at 10:02


You also have the option of these reactions and probably many others considering potassium perchlorates extremely low solubility in water:

2NH4ClO4 + K2SO4 = (NH4)2SO4 + 2KClO4

The ammonium sulfate is very soluble in water and the perc can be filtered off

NH4ClO4 + KNO3 = KClO4 + NH4NO3

Same as above, ammonium nitrate extremely soluble in water and is useful, can be precipitated by boiling down.

NH4ClO4 + KCl = KClO4 + NH4Cl

Once again ammonium chloride is highly soluble.





[Edited on 13-9-2018 by greenlight]




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Laboratory of Liptakov
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[*] posted on 14-9-2018 at 12:44


Ammonium perchlorate is free available in UK...?....NH4ClO4 is holy grail of energetics materials. If you have it, you have all what you need for almost any purposes. He is universal oxidizer for any color flames. Best specific impulse with some fuel for rocket engines. And next great properties on HE field.



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AngelEyes
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[*] posted on 16-9-2018 at 09:30


Thanks for replies.

Fusso - I am looking to get K Perc as that's better for flash and lift charges...cannot see that on eBay and suppliers want an EPP.
Greenlight - hadn't considered K sulphate, thanks for the suggestion.
Liptakov - yes NH4 Perc is good for lances, stars and coloured flames (I don't really do rockets, got nowhere to test them) but it's also quite slow burning - hence it's not great for everything.

I want the K Perc to make some lift charges for some Ghost Mines I will be attempting for Nov 5th. My BP is just not good enough...I guess I really ought to invest in a good ball mill.

Cheers


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greenlight
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[*] posted on 16-9-2018 at 09:52


Definitely get a ball mill :D

I have a dual and single drum Chicago mill filled with lead spherical sinkers.
About 8 hours milling with willow charcoal, then granulated through a 6 mesh screen (or strainer for small items) and works excellent.
About 14% of shell weight for 3 and 4 inch cylinders shoots em perfect for me.

[Edited on 16-9-2018 by greenlight]




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[*] posted on 17-9-2018 at 10:07


Quote: Originally posted by Laboratory of Liptakov  
.NH4ClO4 is holy grail of energetics materials. If you have it, you have all what you need for almost any purposes. He is universal oxidizer for any color flames. Best specific impulse with some fuel for rocket engines. And next great properties on HE field.

All that salt is used for now is rocketry ─ during WW1, it IIRC was used in mortar rounds and grenades as it was cheap and close to TNT in strength.

Its singular lack of green credentials has led to a rush for less polluting oxidisers, of which ADN looks a suitable candidate...

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[*] posted on 19-9-2018 at 01:33


Ebay sometimes has NH4ClO4 in the UK, I also purchased some of that some time ago.

It is very easy to make KClO4 of high purity by means of recrystallization.

I would proceed as follows:
- Dissolve NH4ClO4 in as little as possible of hot water. You need quite some water to dissolve all of it. Use hot water, otherwise you will make really dilute solutions.
- Take a stoichiometric amount of KOH (1 mole of KOH for 1 mole of NH4ClO4) as precisely as you can. Dissolve this in as little as possible of water (careful: a lot of heat is produced). If you have a little excess NH4ClO4, no problem. If you have a little excess of KOH, also no problem, but the work-up in later stages is somewhat unpleasant, due to the corrosive and nasty properties of hydroxide. So, try to avoid excess KOH.
- Mix the solutions slowly, while stirring. Do this outside, you get a lot of NH3. You also get a white precipitate of impure KClO4.
- Still outside, heat the solution to (near) boiling in order to drive off all ammonia and to get all of the solid dissolved. If you cannot manage to get all solid material dissolved, then add water in 10% volume increments and heat to boiling again. I, however, expect that addition of water is not necessary. Continue boiling until you just get some crystalline stuff at the surface. Then add water, 10% of the volume of that liquid and heat until you have a clear liquid again.
- Allow to cool down at room temperature. You get a lot of crystals.
- Put the cooled down solution in a refirgerator and allow to cool down further (cold, but not freezing). You get a little more crystals.
- Decant the cold liquid from the solid and pour/scrape the solid on a coffee filter, which in turn is put on a pile of paper tissue or toilet paper. Nearly all water is absorbed by the paper tissue. You can replace the paper tissue under the coffee filter a few times. Finally, fold the coffee filter with the fairly dry KClO4 between the two sides of the folded filter and press this between fresh tissue paper to squeeze out the last amount of water.
- Open the folded filter again and carefully scrape off the solid into a small porcelain or glass dish and allow to dry on a warm place free of dust.

Using the above procedure you get very pure KClO4. I think it is much better than 99% purity if you use distilled water in the process. If you want really really pure KClO4 you can redissolve all of the solid in as little as possible of clean distilled boiling hot water and repeat the cooling/crystallizing/filter/dry cycle. Then I expect you get better than 99.9% purity.

I have done this work-up of KClO4 quite a few times and each time it works like a charm. I also do this with any perchlorate waste from experiments with solutions of HClO4 or NH4ClO4. I collect such waste and once I have a few 100's of ml I boil it down and collect KClO4 from it. It's a pity to throw away valuable perchlorate, I recycle it this way and give it a second life as KClO4.

KClO4 is a fantastic chemical for recrystallization, because it dissolves quite well in boiling hot water, while it is only very sparingly soluble in ice cold water and forms crystals very easily.

Unfortunately, making pure and dry NaClO4 is not easy. NaClO4 is VERY hygroscopic and even in a well-sealed bottle it becomes a wet slurry in a year or so. Only an all glass container, perfectly sealed, can keep the NaClO4 good for use. In any other container it becomes a wet sticky mass. I recently converted my last small stock of NaClO4 by making KClO4 from it. The NaClO4 had become a really unpleasant wet and sticky mud, and I decided to get rid of that. I made some pure and perfectly dry CsClO4 from that, which works equally well as making KClO4.

[Edited on 19-9-18 by woelen]




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[*] posted on 21-9-2018 at 09:30


Hi!

I have got a lot of NH4ClO4 and KClO4, i can sell it. I could send it mainly in middle Europe. If you interested in feel free to contact with me.
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