CwisGons
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Purifying TCCA
Hello y’all. I have some TCCA I received from a pool supply company. I think I need to purify it by recrystallization. However the only procedure I
found needs concentrated sulfuric acid, which I’m worried to even mess with.
http://www.google.com.br/patents/US2828308
I’m wondering if I could use isopropyl chloride, or even ethyl acetate to dissolve and then recrystallize the TCCA. Will any of these Solvents react
with the TCCA? DCM is hard to come by.
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woelen
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Do not mix TCCA with easy to oxidize organic solvents (most flammable liquids are easy to oxidize). Such mixes may spontaneously ignite and give rise
to intense fires. I have read multiple accounts on accidents with TCCA, runaway reactions with organic solvents, charring and production of lots of
nasty fumes, and even explosions. TCCA is quite a dangerous chemical if handled in the wrong way!
I think that only highly chlorinated solvents can be safely used with TCCA, or compounds which are themselves in high oxidation states.
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CwisGons
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Solvents?
Would you consider isopropyl chloride to be highly chlorinated? Also ethyl acetate is already fairly oxidized, could that work? If not, what would you
recommend I use to purify my TCCA?
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RustyShackleford
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purifying TCCA is not even close to worth the effort, save it for generating chlorine and buy some better stuff for whatever you need decent purity to
do.
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woelen
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Quote: Originally posted by CwisGons  | | Would you consider isopropyl chloride to be highly chlorinated? Also ethyl acetate is already fairly oxidized, could that work? If not, what would you
recommend I use to purify my TCCA? |
Ethylacetate is quite flammable, so I expect that it could react in a very nasty way with TCCA, especially if the solution is heated somewhat.
Some holds for isopropyl chloride. It may be somewhat less reactive than ethyl acetate towards TCCA, but still, I would not dare mixing a bag of TCCA
with this solvent.
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unionised
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| Quote: Originally posted by CwisGons | | Would you consider isopropyl chloride to be highly chlorinated? Also ethyl acetate is already fairly oxidized, could that work? If not, what would you
recommend I use to purify my TCCA? |
No
Also ethyl acetate is already fairly oxidized, could that work?
No
If not, what would you recommend I use to purify my TCCA?
Something that will not burn.
CCl4, CHCl3, C2H6.
Maybe C2H4
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clearly_not_atara
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Someone should warn these authors apparently:
https://www.sciencedirect.com/science/article/pii/S004040391...
And them:
https://onlinelibrary.wiley.com/doi/abs/10.1002/adsc.2003032...
And these authors too:
https://pubs.acs.org/doi/full/10.1021/acs.jchemed.7b00809
And apparently this one uses refluxing EtOAc:
https://www.ingentaconnect.com/content/ben/loc/2020/00000017...
And for some reason multiple review papers about TCCA:
https://chemistry-europe.onlinelibrary.wiley.com/doi/pdfdire...
mention its solubility in EtOAc:
https://pubs.acs.org/doi/full/10.1021/op010103h
I am not aware of TCCA "spontaneously" igniting; I only know that it should not be allowed to get hot. In other papers it's even used in acetone,
which sounds way more reactive than EtOAc. However, I would not recommend using TCCA in any high-temperature process, and solvents ideally should be
removed under vacuum.
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unionised
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So, you wouldn't recommend recrystallisation then.
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clearly_not_atara
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Not the ordinary hot-cold method. But evaporative recrystallization without heating would probably be fine. There are not many solvents you can let
evaporate without environmental hazard, but ethyl acetate is as mild as it comes.
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