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Topic: Diethyl Ether purification?  (Read 14902 times)

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Offline khemikuhlz

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Diethyl Ether purification?
« on: April 13, 2010, 07:59:30 AM »
I recently learned of a starting fluid from John Deere that contains ~80% diethyl ether by weight. The MSDS I read was from 1990 though so I'm not sure the same product exists anymore but...

I understand that by dripping ethanol into sulfuric acid and controlling the temperature to prevent the unwanted reaction, on can synthesize ether. In the distillation apparatus, what is causing the ether to distill out? I guess the heat of the reaction is enough right? Heck it would probably even do that at room temp. seeing as how ether is well... ether.

Anyways, to the point...
Hydrocarbons such as hexane and heptane are insoluble in sulfuric acid correct?

If so, would I not be feasible to drip the starting fluid consisting of CO2, Heptane, and Ether into the sulfuric acid to separate the two whilst having the ether evaporate out into its own separate container?

I figure one could easily obtain diethyl ether by this method but it seems way too easy...

Could someone bring me some enlightenment on these matters before I waste my money?  ;)
Thanks.
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Offline skyjumper

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Re: Diethyl Ether purification?
« Reply #1 on: April 13, 2010, 07:31:00 PM »
If the fluid contains diethyl ether already, distill it out of the fluid? (Don't store it for to long like this. peroxides explode)

Offline khemikuhlz

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Re: Diethyl Ether purification?
« Reply #2 on: April 13, 2010, 08:17:52 PM »
Had I a nice distillation apparatus I would certainly do just that... I'm working up some money to put towards it. :P

But how effective is the aforementioned method (assuming it works at all)?

Does anyone know anything about such a method?
I have a feeling somebody else would know about it if it was worth trying but... maybe, just maybe, I came up with something.  ::)
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Offline nj_bartel

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Re: Diethyl Ether purification?
« Reply #3 on: April 13, 2010, 09:20:47 PM »
How do you plan on "having the ether evaporate out into its own separate container"

Offline khemikuhlz

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Re: Diethyl Ether purification?
« Reply #4 on: April 13, 2010, 11:28:48 PM »
Ha.
I want answers not questions!   :'(

But in any case..

I plan to take advantage of Diethyl Ether's gloriously low boiling point. (34.6°C?)
It shouldn't take too much heating to coax it out right?
The hydrocarbons could be separated easily due to the formation of a layer, right? This, to prevent the hydrocarbons from evaporating along with the ether and contaminating the end product...
I think it could work...

As for the apparatus... I don't know yet.
Possibly some makeshift less-than-scientific-grade distillation system of sorts made from copper tubing and such...

Copper would be useful in this I believe because it could help to prevent peroxide formation...

Thoughts?
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Offline khemikuhlz

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Re: Diethyl Ether purification?
« Reply #5 on: April 14, 2010, 12:06:15 AM »
Ah a double post... my apologies, guys.
I just noticed that Tetrahydrofuran is also used in Grignard reactions. Is this easier to come by than Diethyl Ether? If so, where may one find it?

I want to prepare as much as possible.. finding all the supplies I need whilst cleaning rooftops and mowing lawns to save up for some decent equipment. Great fun.
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Offline nj_bartel

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Re: Diethyl Ether purification?
« Reply #6 on: April 14, 2010, 01:38:11 AM »
I haven't seen THF on the shelves anywhere.

When you distill the ether, you're going to need a way to cool the vapor so it so that it condenses and doesn't just float away.  You should also chill whatever you're condensing into.

Also, don't heat with fire, use a hot water bath.  Or you will scare the s#*$ out of yourself/possibly hurt yourself when your ether vapor erupts in your face

Offline khemikuhlz

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Re: Diethyl Ether purification?
« Reply #7 on: April 14, 2010, 05:54:23 AM »
Oh definitely on that water bath.

I was going to use copper tubing running through a larger plastic tube. The plastic tube will be the condenser. I'll have my little aquarium pump working to put ice cold water through there.
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Offline cpncoop

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Re: Diethyl Ether purification?
« Reply #8 on: April 23, 2010, 09:27:04 AM »
The Grignard reaction can be complicated since it runs differently in different ethers (Schlenk equilibrea).  Regardless, any type of ether should give you some reaction.  TBME can be used, which is probably easier to get a hold of than THF or diethyl ether.

Starting fluid contains about 50% ether with 50% heptane.  This should also work fine for a Grignard rxn..

Offline khemikuhlz

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Re: Diethyl Ether purification?
« Reply #9 on: April 25, 2010, 06:18:02 PM »
I just think there might be a reason why they aren't using a 50-50 heptane-ether mixture in laboratories. lol
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