how do you make Glacial Acetic Acid

LSDMIKE · Apr 25, 2008

can anyone tell me how to make it?

kalacrow · May 22, 2008

To quote one very busy bee:

Another way to GAA

Admitted, this is not so fast and and easy as the IPA - salting out method or the sodium acetate, but it has some other advantages....

A coppertube of about 70cm length and about 3mm inner diameter is connected to a vessel/flask where acetone is brought into a gaseous state of matter (aka boiling). A batwing propane-burner is installed under the part of the tube at the outlet side which heats the tube to a dull red glow. (The burner is positioned at about 50cm from the tubes inlet). The outlet of the tube leads straight into a big vessel with vinegar. This vessel should be halfway filled with broken glass and be hold at a temperature of about 70Â°C. The vessel has to be closed except for an outlet connected to an smoothly running aspirator.

Operation:
The acetone is brought to an straight boil and the tube is purged by the acetone. The burner is started and soon after the tube reached a dull red heat direct over the burners flame ketene will be formed by thermal decomposition of the acetone. The ketene reacts with the acetic acid in the vinegar to form acetic anhydride which reacts with the water to form acetic acid. It is possible to use straight water from start instead of vinegar but this is unfavorable as the reaction of water and ketene is rather slow and ketene would escape. Ketene is poisonous so the aspirator which must run down the drain - no aspirator-station like design here.
After some time you will have a mixture of GAA and acetic anhydride which can be separated by simple distillation. The GAA will be absolute anhydrous. The ridiculous acetic anhydride may be converted to GAA by the addition of water. This should be done ASAP as acetic anhydride is a scheduled compound and might cause legal trouble.

This is a little bit a piggy-setup as the unreacted acetone is washed down the drain and not recovered. But it spares all these washbottles and scrubbers and condensors and stuff, and acetone is asscheap and not regarded enviromental dangerous. (at least the bottles I buy carry no such warning)

Yields: At least 50% from theory, up to 80% with some finetuning.
Ok, it is some work included. But once the work is done you have a neverending source of GAA....
Click to expand...

Lets emphasize two things here....

Acetone is FLAMMABLE. Make sure the damn thing is totally gas tight before you light a propane burner.

Ketene is POISON. And you don't need much of it to completely mess you up. So have good ventilation. I wold also recommend having a small SCUBA "pony" tank with a regulator so if things get out of hand you can use it to be able to breathe while you prevent the whole thing from boiling over or going out of control.

Please plan out this thing very very carefully, and understand everything involved before you light that burner. If you do it right, it will be perfectly safe.

LSDMIKE · May 26, 2008

Thank You !!!

hippiehillbilly · May 26, 2008

wouldnt it be much safer just to buy it?

http://www.pictureline.com/products/1899/Kodak_Glacial_Acetic_Acid_1_gal./

LSDMIKE · May 26, 2008

FUCK YER

Cheers

dan500 · Feb 1, 2009

buy it
cheap and unwatched--far as I know or evap vinegar as it is nothing but diluted acetic acid

I was cleaning out a warehouse some time ago and threw out gallons of it reagent grade
its no big deal
I dont even know why you would want it?
h prod under vacuum perhaps but that is not very productive
as it is usually made with AA as acetic alone just isnt potent enough

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how do you make Glacial Acetic Acid

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hippiehillbilly the old asshole

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how do you make Glacial Acetic Acid

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hippiehillbilly the old asshole

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