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Author: Subject: NMP - Purification - Ideas?
Dr.Bob
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[*] posted on 27-9-2018 at 12:22


Quote: Originally posted by MrG  
I want to remove NMP from GBL. Could I do this by freezing nmp to its melting point?


Not likely. People need to remember that mps are defined for PURE compounds, once a compound is mixed, the mp is depressed, often completely eliminated. It is one thing to crystallize tBuOH from the liquid to purify it, but trying to freeze out one solvent from another only works in a few cases, almost impossible in many cases. The more similar two solvents are, the harder it would be to freeze one out. Also, in general crystallizations work best with nearly pure material to get it really pure, not so well with 50:50 mixtures.

If the NMP bp was much different than GBL's, so you might be able to distill away the GBL away from the NMP, then once the NMP is mostly pure, you could try to vacuum distill it a second time to purify it. But they are much closer in bp than I would have guessed, only 4 degree F apart. Distillations are affected by mixtures as well, but they work pretty well when the bps are more than 10-20 C apart. But with only 2 C between them, they will be very hard to separate that way.
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Metacelsus
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[*] posted on 28-9-2018 at 04:55


If you don't have a good enough column, you might be able to selectively hydrolyze the GBL, distill off the NMP, and then do an esterification to recover the lactone. However, this probably wouldn't be very economical.

(Of course, if you're just after the lactone hydrolysis product, then this method would be more attractive. But be careful to not do anything you'll regret.)




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