GreenD
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Solid-Liquid Azeotropic Distillation
This paper
http://www.ncbi.nlm.nih.gov/pubmed/18498150
describes a procedure:
"The product was azeotroped with toluene and the resulting solid was used in the next step."
I am wondering what the best apparatus would be for this, as any condensation (incorrect term) of the solid is going to be a mess to clean up from a
regular distillation apparatus. I can't find much with "solid azeotrope distillation" with UTFSE
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S.C. Wack
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Relevant physical properties of this product and resulting "solid" are not described, so I'm unsure why I must assume problems. Assuming the product
is a solid, mechanical stirring is the only extra thing about this in many cases; not even that, if the flask and amount of toluene is large in
comparison or the solid is light/fluffy. And if the product does stick to the RBF, it is presumably dissolved in a solvent in the next step?
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kristofvagyok
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Add some toluene, distill it using a Dean-Stark trap till no more water comes over and distill it till all solvent comes over and be happy with the
remaining dry solid.
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Nicodem
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Quote: Originally posted by kristofvagyok  | | Add some toluene, distill it using a Dean-Stark trap till no more water comes over and distill it till all solvent comes over and be happy with the
remaining dry solid. |
The procedure does not call for such a treatment. It only says that the residue after rotavaping was "azeotroped with toluene" which does not involve
any refluxing or Dean-Stark traps. Besides, this question was already raised in a recent thread.
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