Ok so I am building a Frankenstein for the purpose of drying ethanol dry but I mean DRY
Need it for a rxn to make a reagent
So the idea is
Dry etho with molsieves 3a 48/72 hours
Then place etho in reactor and ad magnesium turnings reflux. For 8 hours
But I also want the vapors to pass treu molsieves and then condense the etho and let get back into the solution treu a diptube
So the vapors can only go treu on one way to the condensor
What do you think
@downtheterphole @cyclopath
Ive used rock salt with A3 beads in the past to proof up alcohol, it requires double distillation but it does work, with alcohol being less polar than water the ions in the salt attract the water and can be filtered out.
2¢
how much pressure can this handle?
store your condensed liquid with molsieve and dry gas blanketed.
you’re going to gain moisture from your hoses/connections
It s a 12” triclamp pot and max operating pressure will be 45 psi
The main question I have is do you think the
Distilled /refluxed etho will go back in to the pot yust by gravity ? I see no reason why it should not if it arrives treu the dip tube that’s inside the solution
All hoses will be solid pipe if proof of concept works
I read the other day that you can use vacuum distillation to break the ethanol/water azeotrope
Its called pressure swing distillation
And its not wirth the effort
Why are you stuck on ethanol for anhydrous process solvent?
Work smarter
Yes that’s treu and I might use that tech to get rid of the 4 % instead of molsieves but I think RO is the better option either way it s not DRY
At the end of the run
So still need to add magnesium turnings and some iodine
But the main issue is once dry and taken to the main rxn water is formed during the reaction Wich I need to get out ASAP
Reason I am looking at this method
Quick lime is used most of the times but that gives a massive waste stream that I want to avoid
No other solvent is allowed
Was thinking about the cyclohexane entrainer method but that is not allowed
Are you doing anhydrous chemistry? It seems like you are open to chemical drying agents, so you can start with molecular sieves, which get you pretty dry even from 95%. Then add a chemical desiccant that actually destroys water (sodium metal, phosphorous pentoxide, mg turnings work, powder is better.). Then you just distill. You want to get the bulk with sieves to minimize your chemical drying agent since they are expensive/reactive. Distilling through sieves seems like overkill, but that may be the name of the game
If you are doing chemistry where you have precious reagents (exotic organometallics), yes, overkill dryness. If it’s just a reagent (super acids like SnCL4 or super bases like n butyl lithium) add a bit extra and that will destroy your water, taking you to dryness.
What reaction is it, depending on your solvent and reagents, you may be able to use chemicals that chemically destroy the water, but your starting materials may be too sensitive
Google ethanol pressure swing distillation
Lots of available media and studies, could get lost in it easily
If I remember correctly the azeotrope of ethanol is pretty much non existent at pressures above about 100 psi. I bet if you pumped ethanol into a tank containing 3Ă… beads and cranked up the pressure you could probably break the azeotrope and lock up the water at the same time.
Edit: I did not remember correctly, the degree of azeotrope formation actually trends in the opposite direction. Less pressure = less formation of the azeotrope of wthanol/water, not more pressure. 
As far as I remember, the azetrope is broken somewhere around 80 Torr. One problem is that boiling point is now close to ambient temperature. Apparently getting to 200 proof this way is not the most energy efficient way but quite a bit of studies have been done since 200 proof ethanol is a common fuel additive.
Eureka phosphorus pentoxide I have in abundance so that’s a great idea I ll Have ortho phosforic for the neutralizing step as well
You see you folks are gold !! Thank you
You’re welcome! Happy to help. I’m assuming the reaction tek is still on a need to know basis, I’m very curious what reaction you’re doing.
