soma
Hazard to Others
Posts: 297
Registered: 31-7-2010
Member Is Offline
Mood: No Mood
|
|
molecular sieve capacity
I've read that molecular sieve can adsorb up to 22% it's weight in water. Would the number of molecules of ethanol adsorbed be the same as for water?
Meaning that it would adsorb about 56% of it's weight in ethanol? I want to remove ethanol from ether using 4A sieve.
Thanks.
|
|
|
Burner
Hazard to Others
Posts: 100
Registered: 28-3-2014
Member Is Offline
Mood: No Mood
|
|
Don't have an answer for your question, but I do have a question. Why not distill it?
|
|
|
EdMeese
Harmless
Posts: 16
Registered: 25-1-2013
Member Is Offline
Mood: No Mood
|
|
probably not ... ethanol is much larger than water so far fewer will fit inside the pores where all the action is. But I've never seen any data,
either.
|
|
|
sparkgap
International Hazard
Posts: 1234
Registered: 16-1-2005
Location: not where you think
Member Is Offline
Mood: chaotropic
|
|
Also, you're assuming that ethanol is the only thing contaminating your ether; if it's also wet, then you'll need to add some more 4A just to fit in
all the water, ethanol, and other possible gunk in your ether. Should you need to get the ethanol from the sieves afterward, you'll need to do a good
amount of heating.
And thus, we go back to Burner's suggestion.
sparky (~_~)
"What's UTFSE? I keep hearing about it, but I can't be arsed to search for the answer..."
|
|
|
soma
Hazard to Others
Posts: 297
Registered: 31-7-2010
Member Is Offline
Mood: No Mood
|
|
Actually, it's "anhydrous" ether with 2% ethanol stabilizer. I was going to add sieve to dry it more and then distill it from LAH to complete. I'd
rather not have to distill it twice (once to remove ethanol, 2nd time from LAH).
|
|
|
kristofvagyok
National Hazard
Posts: 659
Registered: 6-4-2012
Location: Europe
Member Is Offline
Mood: No Mood
|
|
Quote: Originally posted by soma  | | Actually, it's "anhydrous" ether with 2% ethanol stabilizer. I was going to add sieve to dry it more and then distill it from LAH to complete. I'd
rather not have to distill it twice (once to remove ethanol, 2nd time from LAH). |
Why not add some sodium or activated magnesium, stir a few days and distill it from that? Much cheaper and easier to handle, than LAH.
P.S.: someone in our lab blown up a flask while distilling dioxane from LAH. Some peroxides formed during the past 20 years and when the distillate
was concentrated enough on the LAH it blown up.
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." |
|
|
Dan Vizine
National Hazard
Posts: 628
Registered: 4-4-2014
Location: Tonawanda, New York
Member Is Offline
Mood: High Resistance
|
|
[/rquote]
Why not add some sodium or activated magnesium, stir a few days and distill it from that? Much cheaper and easier to handle, than LAH.
P.S.: someone in our lab blown up a flask while distilling dioxane from LAH. Some peroxides formed during the past 20 years
and when the distillate was concentrated enough on the LAH it blown up.[/rquote]
C'mon, really? Distilling 20 yo dioxane w/o testing for peroxides and destroying them? It's hard to understand how someone gets to the point of even
needing anhydrous dioxane without having learned that THF and p-dioxane (I assume) are quite prone to peroxide formation. I'm assuming he knew better
but was in a hurry? Bad lapse of judgement.
Anyway, molecular sieves, zeolites, can remove whatever the cavities are optimized to hold to an astonishing degree. All sieves are not the same, they
vary principally in the above mentioned feature. If you get a 3A sieve it will have 3 angstom holes. Choose accordingly, consult the manufacturers
charts. Molecular sieves, for instance, can dry solvents to a much smaller residual water level than any perchlorate or pentoxide ever could. That
being said....
Sieves are most effective in scavenging roles and not as good for bulk removals (I'd call 2% a bulk removal, it's certainly not considered trace).
Just as kristofvagyok said, it's easier to just "react" the ethanol out.
Once dry, molecular sieves will maintain it that way. Remember, peroxides are most easily formed in very dry, pure ether and especially in
light-transmitting bottles.
|
|
|
leu
Hazard to Others
Posts: 368
Registered: 13-10-2005
Member Is Offline
Mood: No Mood
|
|
Some documents related to the safe handling of solvents prone to peroxide formation are in the attached archive 
Attachment: steere+.zip (1.1MB)
This file has been downloaded 362 times
Chemistry is our Covalent Bond
|
|
|
soma
Hazard to Others
Posts: 297
Registered: 31-7-2010
Member Is Offline
Mood: No Mood
|
|
I've wondered why someone would want to reflux (or distill) dioxane from LAH since dioxane boils at 101C and the flash point of LAH is 125. But,
wouldn't the LAH get rid of the peroxides? Or maybe the explosion happened immediately upon adding the LAH?
[Edited on 9-6-2014 by soma]
|
|
|
chemrox
International Hazard
Posts: 2961
Registered: 18-1-2007
Location: UTM
Member Is Offline
Mood: LaGrangian
|
|
So far the best thing to come out of this was the link posted by Leu. Someone should also post the table of sieve sizes vs. cmpds captured. (I'm
traveling and don't have it). I still think the best idea was to stir over sodium or magnesium, check for peroxides and distill. If peroxides are
present you'd want to grab those before any distillation is run.
"When you let the dumbasses vote you end up with populism followed by autocracy and getting back is a bitch." Plato (sort of)
|
|
|
ziqquratu
Hazard to Others
Posts: 385
Registered: 15-11-2002
Member Is Offline
Mood: No Mood
|
|
| Quote: |
I've wondered why someone would want to reflux (or distill) dioxane from LAH since dioxane boils at 101C and the flash point of LAH is 125. But,
wouldn't the LAH get rid of the peroxides? Or maybe the explosion happened immediately upon adding the LAH? |
Remember that the flash point (lowest temperature at which the vapour pressure can sustain a flame) is NOT the same thing as the autoignition temperature (the lowest temperature at which a material will spontaneously ignite - without any external ignition source).
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
