gravityzero - 19-7-2013 at 10:35
In preparation of an Ether Synth I am planning for the weekend, I have a few items I would like to discuss.
The procedure I am familar with involves using 96% ethanol or everclear, other grain alcohol in a reaction with H2SO4 to create Ether. While I am
certain the process works, I understand that the product is still contaminated with excess ethanol. I believe that the two form an azeotrope.
The azeotrope is fine for the initial production and most vendors even add ethanol to ether for stability. I think there is a breakdown in ether that
can form unwanted gas byproducts.
So how should one proceed with this information?
Should I just fractionaly distill the inital product and be content.
Can I use a method, such as dean stark, to break the azeotrope, in an attempt to cleanup the ether?
I'm just not sure, but my intial thought is not to go through the trouble if ethanol should remain as a stabilizer. My only problem is adding ethanol
is only done to a percentage of fairly pure ether. Unless I know my starting point, how would I know if that percentage is already in excess?
I am open to discussion on how others handle the situation.
Please be kind, I am still a newbie.
Magpie - 19-7-2013 at 10:54
Have you read through Len1's procedure in the Prepublication forum?
gravityzero - 19-7-2013 at 11:07
No, I have not. Thanks for the suggestion. I figured it had already been covered. I attempt to keep from being spoonfed. 
ParadoxChem126 - 19-7-2013 at 15:28
If you wash your ether with calcium chloride solution, the CaCl2 will complex with any ethanol. Then dry it and redistill to ensure purity.
vmelkon - 22-7-2013 at 19:07
I though that NaOH is added to stabilize the ether, not ethanol (to prevent peroxide formation).