nasty reaction - Archive File

[megalomania]

shady mutha
Frequent Poster
Posts: 149
From: australia
Registered: SEP 2000
posted March 08, 2001 10:02 PM
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Tried to make acetone peroxide with 50% h2o2 100% acetone and 1835g/litre sulfuric acid.Anyway the second the sulfuric acid touched the cooled peroxide acetone mix it spat the acid out ,made a loud hissing noise and let out a white cloud of stinky shit some stayed in the jar and had to be blown out the jar.What do you think happened?


PYRO500
Moderator
Posts: 1478
From: somewhere in florida
Registered: SEP 2000
posted March 08, 2001 10:12 PM
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I assume this is your first time making
AP with sulfuric acid beacuse that is the nature of that acid, it dosent like being mixed with much of anything. and what you experienced was acid splatter and the fumes were just sulfuric acid fumes. I use a syrnge and a piece of tuning not to get hit by splattering acid. next time ad it more slowly


HMTD Factory
Frequent Poster
Posts: 220
From:
Registered: FEB 2001
posted March 09, 2001 01:21 AM
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Yes, H2SO4 gives out a lot of heat when mixed with water.
You should also know only H2SO4 should be poured into water, not water poured into H2SO4.



shady mutha
Frequent Poster
Posts: 149
From: australia
Registered: SEP 2000
posted March 09, 2001 02:00 AM
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Yes it is my first time with sulfuric.I also tried adding acetone to just sulfuric acid this caused the mixture to boil almost immediately.


Morrigan
Frequent Poster
Posts: 81
From: The Netherlands
Registered: OCT 2000
posted March 09, 2001 04:42 AM
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Sulfuric acid dehydrates everything even if there is no direct H2O present it will break up the molecules in order to steal H2O releasing a lot of heat, what you experienced is this dehydration, it might even break up acetone. It also does this to skin, (resulting in blisters), and lots of other materials. Since you use 50% H2O2 I would advise you to dissolve the H2SO4 to a concentration of about 30%, that bit of water is not going to disturb the reaction. If you use the recipe from Mega’s site you can easily calculate the amount of diluted H2SO4 needed.
If you put the acid into the water and not the water into the acid it will still splatter but the splattering will be mainly water and not the concentrated acid saving you a lot of mess...



PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted March 09, 2001 05:37 AM
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H2SO4 conc. react with water (and what is H2O2 50% but 50% water with 50% oxygenated water????) by releasing heat.
As a matter of facts: peroxydes are unstable at high temp (here in my lab at work we keep the 50% H2O2 in the fridge at 10-4C)....thus no doubt your H2O2 has been destroyed by the heat! Also aceton is a very volatile solvent with a low boiling point... a mix with water heated can boil near 60C, thus increasing the bubbling of your solution.....you lucky bastard that O2 liberated and aceton vapours didn't met a flamme other wise ......BOOOM gas explosion!!!!!
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"Life that deadly disease sexually transmitted".
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nbk2000
Moderator
Posts: 1135
From: Guess
Registered: SEP 2000
posted March 09, 2001 06:23 AM
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You should dilute your peroxide with 1 or 2 times its volume of water because 50% is overkill and just a waste of peroxide.
Once you get over 20 odd percent, any higher just gives decreasing return in yeild.

And add your H2SO4 a drop at a time with stirring in between additions with cooling the whole time.

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"The knowledge that they fear is a weapon to be used against them"

Go here to download the NBK2000 website PDF.



HMTD Factory
Frequent Poster
Posts: 220
From:
Registered: FEB 2001
posted March 10, 2001 01:48 AM
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!!!!!
How do you managed to type the footnotes, nbk?



zaibatsu
Frequent Poster
Posts: 403
From: England
Registered: SEP 2000
posted March 10, 2001 05:51 AM
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By typing H<*sub>2SO<*sub>4 but without the stars, I had to put them there to stop it thinking I meant H2SO4

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[This message has been edited by zaibatsu (edited March 10, 2001).]



nbk2000
Moderator
Posts: 1135
From: Guess
Registered: SEP 2000
posted March 10, 2001 10:53 AM
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Since HTML code is allowed, you could do all sorts of things with your posts. Using < sub > for lowering type or < sup > for raising it.
< pre > allows


You to draw ----- / \ | @ @| Faces \ / & \{}/ other \/ figures
Don't forget that all tags have to be closed using the /. Like < pre > is closed with < /pre >. No spaces in the tags of course.

But there are other things that you could do that won't be tolerated like using frames, blinking, scrolling, or rolling text, etc.

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"The knowledge that they fear is a weapon to be used against them"

Go here to download the NBK2000 website PDF.

[This message has been edited by nbk2000 (edited March 10, 2001).]



HMTD Factory
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Posts: 220
From:
Registered: FEB 2001
posted March 11, 2001 01:37 AM
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Thanks. But, argh, why it has to be such an hassle...anyway.


Teck
Frequent Poster
Posts: 146
From:
Registered: JAN 2001
posted March 15, 2001 04:17 AM
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The only acid I use in making my AP is sulfuric from old car batteries and it never splattered or reacted weird. The concentration on it is like 40% or something and the AP mixture has a faster reaction than using HCL Acid. At least thats what I think.
I had a dream I detonated 1/2 film canister of AP in my back yard and my neighbors car alarm went off even though my nearest neighbor lives about 400ft from me.

[Imperial]

SWIM has tried making some AP with sulfuric acid, as well as hydrochloric acid.

For a newbie, SWIM recommends the latter, for it splatters less, doesn't raise the temperature as much, and generally isn't as dangerous.

The first time SWIM used H₂SO₄ it raised the temperature too much, and SWIM ended up having to cool his acid/acetone mixture (after cleaning up the nasty splatter!) SWIM was more careful next time, and added the acid slowly and cooled the acid and acetone beforehand. SWIM had to cool the actual reaction a lot more, but he ended up with a greater yield than with the HCl. So SWIM suggests that your first few times you use HCl just to ge aquainted with the process, maybe practice the cooling too, and then make it with the sulfuric acid.

[yt2095]

the only problem associated with with AP manufacuring AFAIK are these;

H2SO4: if your AP is not completely neutralised Sulphuric acid will not evaporate in the same way that HCl(aq) will, leaving your product npotentialy unstable.

HNO3: will evaporate in the same way as HCL but risks making acetone nitrate (though I`ve never had a problem with it because of the concs I use and Ammonia to neutralise it)

HCL(aq): is favoured, but I personaly use H2SO4 as it`s cheap/plentifull and I spend A LOT of time neutralising it (a proccess NOT to be skimped on)

these are my OWN findings and are also echoed on certain threads here as well, in fact I beleive it was Kingspaz that told me about the acetone nitrate potential.

H2SO4 (for AP use) is never more than 60%, that avoids all the spattering and lowers the inevitable heat generated.

Enjoy your product :)

[Anthony]

When using H2SO4 in AP synth, I always diluted it to ~30% and cooled before use. It's silly to let it hydrolise during the reaction when you will have to deal with the heat, when you can "remove" that heat before hand.