Finkelstein Reaction - A Mess... How to Recover Iodide?
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Short version:
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DId finkelstein with
-Sodium Iodide with Naoh impuritites
-DCM
-Acetone
mixed 24 hour at low reflux.
distilled off acetone, little bit of liquid (actone?) was left over, maybe water.
white sludge at bottom , reddish liquid was left over.
should be a white liquid with fluffy NaCl precipitate.
red liquid with white sludge cant be filtered,
how can I recover Iodine from this without forming peroxides by accident?
tried crashing out iodine with potassium peroxymonosulfate but
that only formed a red 'oil' layer on top of a white water layer below.
maybe iodoacetone got produced?
defiantly some diacetone alcohol since it smells like 'funk' !
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LONG VERSION
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tried the finkelstein reaction with
-homemade sodium iodide with some NaOh impurities
-acetone drived over calcium sulfate
-DCM dried over molecular sieves 3A
all were added together into a flask with a reflux condenser and high
magnetic stirring for 24 hours.
solution turned red after a very short time, this should not happen....
then after 24 hours mix was filtered.
a white sludge clogged the vacuum filtration up completely.
added all solids back into the flask and distilled off all the acetone.
a little bit did not distill over at ~100+C hotplate temperature.
some red sludge was left in the flask.
flask was flooded with water.
nothing much changed...
now I got a orange colored liquid with
-maybe acetone residue
-some NaOh
-NaCl
-Iodine in some form?
-NaI unreacted
-diacetone alcohol , that was aldol formed between acetone and the NaOh impurity
(smells funky)
-maybe some diiodomethane...
I just want to get the iodine back and start again clean.
I took a small sample from the mess and added
some potassium peroxymonosulfate...
solution turned red but no solid iodine precipitated out,
only a thin reddish oil layer appeared on top of a white water layer.
some pot peroxy was also accumulated at the bottom...
the last thing I want is to make some acetone peroxide by accident..
this can not be dangerous if its in an aqueous solution? (its insoluble in water)
any way to recover the iodine from this mess?
[Edited on 1-12-2020 by LuckyWinner]
[Edited on 2-12-2020 by LuckyWinner]
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