15% Peracetic Acid - Explosivity?

iodide · Thu Jun 16, 2005 8:29 pm

Chromic's write-up provides what appears to be the most straightforward and OTC method for conversion of isosafrole to MDP2P that exists.

HOWEVER, I am aware of the explosive nature of peracids, and more specifically, the explosivity of highly concentrated peracetic acid.

What I want to know however is the realistc dangers of peracetic acid at the 15% concentration called for in Chromic's write-up, especially since i've read that Chromic's write-up omits to tell of the need to reflux the peracetic acid-isosafrole solution. Perhaps I'm wrong but something tells me the dilute concentration and the presence of water mitigates some of the instability. Therefore:

1. Is 15% peracetic acid to be considered safe for all practical purposes? That is, I can perform a low reflux, not worry about shock-sensitivity and such?

2. Does anyone have familiarity with Chromic's write-up and can chime in on how SWIT handled (or mishandled) the peracetic acid and whether they saw signs of danger, or none at all? Did you reflux? Did you not reflux and instead followed Chromic's write-up verbatim?

Thanks a bunch for your help.

icecool · Insistent Chemist

SWIM did this method with GAA and H2O2 and H2SO4 and it worked fine.
It didn't explode else SWIM wasn't typing this...

iodide · Fri Jun 17, 2005 8:51 pm

Thanks so much for replying IceCool. Nice to finally ask someone in real life as opposed to scouring the Hive archives in hopes of someone having directly responded to my concerns.

Couple questions, if you don't mind:

1. Did SWIY follow the Chromic write-up exactly?
2. If not what did you do different?
3. Did you reflux the peracetic acid/isosafrole mixture at all? I ask because I read some discussion on doing this, and that Chromic's write-up might have negligently omitted this.
4. And if so, what was your procedure with respect to it (temperature you kept it at, how if at all did you cool it?)

Thanks a BUNCH for your help, its appreciated very much!

biobrew · Sat Jun 18, 2005 1:56 am

Hey iodide, SWIM hasn't followed chromics procedure exactly, but have run some peracetics. There is an explosive compund that can be isolated, but don't woory too much. As always, be careful.

SWIM prefers not to reflux a biphasic system with the low BP solvent on the bottom because of possible fountains if not run right. For SWIM, it seems much easier to run small batches(.2-.5M) and just let it stir for 16hrs. Less stress is better.

The formation of the glycol is high yielding, but it's the conversion to the ketone where one really loses product.

SWIM's procedure is to chill the sassy/acetone in the freezer, and put the peracetic in the fridge. When chilled, mix, unless large batches are being attempted. SWIM once tried to run a 2M rxn this way and wound up with an H2O2 volcano......NOT FUN. After they are mixed, let stir for 16hrs. Sometimes SWIM floods post rxn contents with h20 and extracts. When the addition is above .2M, swim does the addition in portions(1/2 first, then 1mL at a time depending on the use of an addition funel or not.) @ .2M, the addition peaks right around 40C.

SWIM is trying a 4M HCl hydrolysis for the first time this weekend. Keep yr fingers crossed for her/him.

Hope this helps, unless you are set on using chromics write-ups. SWIM usually ends up with a 65% yield(SWIM takes a little less yield for ease of use and piece of mind)

edited for lisdexia and additional info----BB

iodide · Sat Jun 18, 2005 11:13 am

Thanks for your input, BioBrew!

However, I am very much afraid to try your variation (in theory as I don't plan on ever doing this) as you introduce acetone into the mix. Peroxyacetone is an incredibly unstable explosive. A kid I know blew his hand off after making some - its most definitely shock-sensitive and from what I've read about peracetic acid, much more dangerous!

Why exactly are you introducing acetone?

Please don't think I'm trying to not your method! Just scared enough to worry about the peracid, and don't want to have to deal with another potential explosive....

good luck!

P.S. I'd love to hear how your HXL hydrolisys goes. It sounds to be superior to an H2SO4 hydrolysis and the acid is easier to obtain!

The_Dude · Sat Jun 18, 2005 3:38 pm

Follow chromics write up exactly as written

Place the reaction flask in a cold water bath, pour in half the peracetic acid, wait 10 minutes, pour in the other half.

It will not get over 25 Celcius this way.

DO NOT reflux (heat up).

I believe the peracetic strength is around 8-9% and not 15%.

icecool · Insistent Chemist

I did not reflux the other information I've got at home in SWIM's computer.
I'll post the info then.