Acetone Peroxide Malfunction(?)

[Nope]

Today, I decided to make some AP. I used the method I saw in the "AP Begginer's manual" (pdf). The method says that you can add the acid to the previously cooled acetone and then the HP in small portions because it's easy to control the raction... (I used 95-97% Sulfuric) So, I add the acid to the acetone and in ~5 minutes (in the ice bath) it started to changing color. Finally, it turned to yellow-orange color. After that, I add a small portion of HP (%30); it began fizzing and its color turned to orange - red! (Shit? :p )

All I want to know is wtf was that. :confused:

Also, could it be possible to mix the acids and then add the acetone or it'll screw up the reaction?

Thnx 4 your time

[The_Rsert]

Maybe it was (diiso)propyl ether!?
This would be no problem, because propyl ether will from AP in contact with air and H2O2. And the fizzing is maybe decomposing H2O2 (Because of the partial heat). But I can't explain why the clour changed red.

Have you used oure acetone or nail remover?
Was acid boiled battery acid or a bought one?
Was H2O2 bleach for clothes (contains for example perbromates, percarbonats), a cleaning agent (contains for example tensides) or pure H2O2?
...
When the bleach contains percabonate, the fizzes are only harmless CO2 bubbles.
...

[Nope]

* Acetone was pure.
* Sulfuric acid (>95%) was purchased.
* (Today I bought, ) Perhyrdol (30% H2O2)

After It turned red I threw it away... I thought it'll be useless.. :P

[The_Rsert]

Then, just mix the acid and the H2O2 first together.
This schould work.

But can't explain the changing of the colour.

????

[Nope]

Hm... ok.

About the color.. I'm not a chemist... :P

I think i've noticed this color change when I first make AP. I had mixed acetone and the HP and then I poured the sulfuric... :P A lot of heat produced and I noticed this orange-red color.. Dunno :P

[Nope]

You'd better check this thread "Holy grail organic peroxide! "... it says something about the colour...

[The_Rsert]

Yes, I know the thread by heart.
But usually acetone will not be so decomposed by sulphuric acid when it's cooled. Use lower concentrated/thinned H2SO4 (40%). Maybe it will work better. But why it does fizz?

PS: Next time use the "Edit" function, if you want to add something to your last message.

[Nope]

I wish I was a chemist to give you the answer.. :)

Anyway, thnx.

[trinitride3]

I had the same thing happen to me when I was making HMTD using hydrochloric instead of citric acid. I left garage a few minutes after the last addition of acid only to return 10 minutes later to a violent reaction, to violent for me to get close enough to dump it in water. I got away and let it run its course, when it was safe to return I noticed that the heat caused my brand new mercury thermometer to shatter. What gives?

[Rosco Bodine]

Classic order of addition problems .

For AP chill your acetone and peroxide separately and then pour
the cold acetone into the cold peroxide and stir . Add part of the
acid with stirring and cooling observing for temperature rise between
added portions of acid , only adding more acid each time when the
temperature of the mixture drops down again after each addition .
Usually this will require 3 portions . Keeo the mixture ice cold for two days .

For HMTD , dissolve the hexamine in the cold peroxide and if the solution
warms slightly cool it back down as cold as possible before beginning
the addition of any acid . Add the acid to the cold hexamine and peroxide
solution , in small portions with stirring , allowing to cool between added
portions . Then keep the reaction mixture very cold for 3 days in
the freezer . Patience and correct proportions are essential for good results .

[Nope]

Keeo the mixture ice cold for two days .

Well... Yesterday, I made a batch of AP... After the acid addition, I left my mixture stand for 8 hrs (out of the ice bath)... All the mixture has been converted into a big crystal... Don't you think 2 days are too much?... :p

[Rosco Bodine]

Well it depends on how much acid catalyst you use and how hard you want to drive the reaction . You can do the whole process in one hour if you want to do that . But generally
it is safer and gives a better yield to go cold and slow .

[Chris The Great]

Interesting, I got a deep red colour in a failed attempt at HMTD (then again, I wasn't really trying :p ). I had made hexamine by mixing ammonium hydroxide and formaldehyde together, and since I was to lazy to boil it down and get the pure hexamine, a few months later I dumped in the correct amount of H2O2 and HCl (assuming HCl would work just fine). It didn't work, and I ended up with a beautiful red solution, with a dead bug floating in it after a few days. Was a pretty colour, but no HMTD.

I love how AP crystals fill up the jar afterwards. Nothing says success like a huge mound of AP where there once was a small amount of liquid :D

[Rosco Bodine]

HCl will work just fine for HMTD , and so will probably many other
acids , but the amount of acid used must not be in excess of just
that amount needed to neutralize the hexamine and possibly a
little more to make the pH just slightly acidic , maybe to pH 6 ,
I never actually checked it with paper . The acid in the HMTD
synthesis is not a catalyst as is the acid in AP synthesis , so
its quantity is critical because it is an actual reactant in the
process . Get too much acid there and it destroys by hydrolysis
the hexamine before it can peroxidize , or it destroys the HMTD as
fast as it forms and either way you get zip for the effort while
being sloppy about the quantities .

[Chris The Great]

Opps, I dumped maybe 250mL of HCl into it, for a yeild of maybe 65g hexamine (the formaldehyde and ammonia where dilute, 25% and 10% respectivly, so there was alot of water).

That certainly explains it. Maybe I should learn a bit about the synthesis before trying it next time :p I always thought that the process was the same as that for AP and the acid was only a catalyst.

[The_Rsert]

Why you're not using citric acid as catalyst for HMTD? It's cheaper than HCL. The temperature does not rise extremly. The final product has a grater stability. Citric acid is better avaible than HCL.
...

[kingspaz]

Thank you rosco.

The original issue seems to be resolved. Conc. H2SO4 clearly reacts with acetone!

Rosco, just out of curiosity, do you know what the reaction is? I'll be honest, I'm a bit drunk, but I'd be inclined to think its some sort of dehydration producing propylene...but I'm not sure at all!

[Chris The Great]

Where can I get citric acid? I used HCl since I picked up 4 litres at the hardware store of $8 Cdn (32%). They had maybe 10 or so jugs. It's extremely available for me. I've seen citric acid in the pharmacy for a couple of bucks for a very small vial, I can't remember the size but I think it was around 100g. Is there an easier place to get it for cheap?

[IPN]

Chris The Great, if it is too expensive to buy you could always purify it from lemon juice.. but I don't see any trouble using the HCl instead, just make sure the temp stays below 0C. Has always worked for me. :)

BTW.
Kingspaz, in the reaction the sulfuric acid dehydrates the acetone into mesitylene, not propylene. :)

http://koti.mbnet.fi/otto2000/acetone_to_mesitylene.gif

[kingspaz]

Cheers IPN. I'll work out why it does that later :)

[kingspaz]

A slightly off topic thought, but would it not be possible to nitrate that dehydration product? The methyl groups direct ortho/para and due to their arrangement should reinforce each other which should make it *very* easy to nitrate. The only problem I can see with this would be steric hinderence from the methyl groups but I'm not entirely sure how much hinderence a relatively small methyl group would give...

If possible this compound would make an excellent sensitising agent for AN, cheddite type explosives and possibly for making castable charges depending on its melting point.

[Chris The Great]

A, lemons. Yes, that is accessable :D

I've never had problems with heat and 32% HCl making AP, I mix the acetone and H2O2 (35%) then pour in the HCl and stir it for a few minutes, then leave it for 48 hours. Heats up to about 40C on a warm day (maybe 25C at the current temperaturs here right now), but I have no problems.
Then, I filter, wash, and dissolve in acetone. When I need some, I pour some of the acetone solution into water to get a super fine precipitate which after being filtered and dried is very stable and packs extremely well. Never had a problem, although the stuff still worries me.

[Silentnite]

I used H2SO4 in my AP production and it worked fine. No violent reaction, nothing. I kept it chilled in an ice bath, and slowly added. And it was pretty strong conc. of H2SO4. I'm away from my house, so I'll get back to you. Coincidently, I just found HCl so I'm going to start using that instead. Good luck.

[IPN]

would it not be possible to nitrate that dehydration product?

Possible, yes. Easy, no. :(
And the yeild of mesitylene from the reaction is usually very low (13-15 pr cent according to orgsyn)..

http://orgsyn.org/orgsyn/prep.asp?prep=cv2p0449 http://orgsyn.org/orgsyn/prep.asp?prep=cv1p0341

[knowledgehungry]

Not only that I doubt nitromesitylene would be an explosive.