Peracetic Acid Oxidation

[Rhodium]

This nice article has been referenced earlier in

Post 245000

(Greensnake: "preparation of peracid solutions", Chemistry Discourse)

Preparation of Aliphatic Peroxyacids
Benjamin Phillips, Paul S. Starcher, Bertrand D. Ash

J. Org. Chem. 23(12), 1823-1826 (1958)

(https://www.thevespiary.org/rhodium/Rhodium/pdf/aliphatic.peroxyacid.preparation.pdf)

Abstract

Convenient procedures are described for preparing peracetic and perpropionic acids as anhydrous solutions in solvents of negligible acidity. The method is based on the reaction of carboxylic acids with hydrogen peroxide and employs azeotropic removal of water to drive the reaction to completion. Conditions for safe operation are chosen on the basis of measurements of the detonability of peracid solutions.

[Chromic]

There's other ways to get the peracetic to form faster--you can raise the temperature and reduce the time as in the document that Rhodium mentions. Azeotropic removal of water with ethyl acetate (or whatever) doesn't look promising to increase the concentration of peracetic acid much--perhaps I'm mistaken on that, I only briefly reviewed the journal. There should not be much oxygen coming from the peracetic... an occassional tiny bubble can be seen, but it's very intermittent.

Yes, running the peracetic with a cold water bath, and just letting it to come to room temperature is the way that I did it. The references I read recommended keeping it cool--I found it important at the beginning if I didn't want the flask to hit a reflux.