GreenD
National Hazard
Posts: 623
Registered: 30-3-2011
Member Is Offline
Mood: Not really high anymore
|
|
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
ʃ Ψ*Ψ
Keepin' it real.
Check out my new collaborated site: MNMLimpact.com
|
|
S.C. Wack
bibliomaster
Posts: 2419
Registered: 7-5-2004
Location: Cornworld, Central USA
Member Is Offline
Mood: Enhanced
|
|
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?
|
|
kristofvagyok
National Hazard
Posts: 659
Registered: 6-4-2012
Location: Europe
Member Is Offline
Mood: No Mood
|
|
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.
I have a blog where I post my pictures from my work: http://labphoto.tumblr.com/
-Pictures from chemistry, check it out(:
"You can’t become a chemist and expect to live forever."
|
|
Nicodem
Super Moderator
Posts: 4230
Registered: 28-12-2004
Member Is Offline
Mood: No Mood
|
|
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.
…there is a human touch of the cultist “believer” in every theorist that he must struggle against as being
unworthy of the scientist. Some of the greatest men of science have publicly repudiated a theory which earlier they hotly defended. In this lies their
scientific temper, not in the scientific defense of the theory. - Weston La Barre (Ghost Dance, 1972)
Read the The ScienceMadness Guidelines!
|
|