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Natural Science Forum / Chemistry / Organic Synthesis / September 2003



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Re: drying alcohol

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CJ - 11 Aug 2003 20:54 GMT
Hi,

what do you need this for? If it is for lab scale reactions then just buy some dry Ethanol
from your normal lab chemical supplier. It can't be done as easy as you think. A
commercial process uses beds of molecular sieve at temperature to remove the water. Other
methods are pressure swing distillations to break the azeotrope etc.

CJ

"Michael Carpenter" <mikecarpenter2000@hotmail.com> wrote in message
news:bh302t$as9@panther.Gsu.EDU...
> Hello,

> I am interested in drying etahnol. Would adding anhydrous magnesium
> sulfate do the trick?

> Also, after I add it, do I just filter it out and end up with 'dry'
> alcohol? or does it take more than that?
>
> thanks,
>
> Mike

Signature

Paul J. Franklin(moderator - sci.chem.organic.synthesis)
http://organicworldwide.net/sci.chem.organic.synthesis
Georgia State University <chepjf@panther.gsu.edu>
Atlanta, GA

Dave Muzuno - 11 Aug 2003 20:55 GMT
> Hello,
>
[quoted text clipped - 3 lines]
> Also, after I add it, do I just filter it out and end up with 'dry'
> alcohol? or does it take more than that?

Magnesium sulfate won't work cause it will partially dissolve in the alcohol
AND it also reacts with alcohol.

The easiest way to dry ethanol:

1.  Take 1 L of 95% ethanol and add 20 g of magnesium turnings.
2.  Start heating.  The alcohol starts to react with the magnesium,
producing hydrogen and magnesium ethoxide.  If it doesn't start, shoot in a
0.5 mL of chloroform, then keeping heating.
3.  Gently reflux the mixture until all the magnesium has been consumed
(1 -2 hours).
4.  Distill the mixture, discarding the fore and after run.

Dave

Signature

Paul J. Franklin(moderator - sci.chem.organic.synthesis)
http://organicworldwide.net/sci.chem.organic.synthesis
Georgia State University <chepjf@panther.gsu.edu>
Atlanta, GA

donald j haarmann - 21 Aug 2003 20:39 GMT
"Dave Muzuno" <nobody@nowhere.com

> The easiest way to dry ethanol:
>
[quoted text clipped - 7 lines]
>
> Dave

--------
Organic Synthesis, Collective  Volume 1 pg. 249.

Suggests (if  the presence of methyl alcohol is permissible):-

"by dissolving 24g of magnesium turning in 200 cc. of absolute methyl alcohol (the
reaction is vigorous) and then adding 3 l of the ordinary grade of absolute
alcohol (about 99.5 per cent). The mixture is refluxed for about 5 hours
and distilled into a flask in which the absolute alcohol is to be used."

Preparation using sodium and chlorform can be found on page 259 (same volume).

--
donald j haarmann - independently dubious

Signature

Paul J. Franklin(moderator - sci.chem.organic.synthesis)
http://organicworldwide.net/sci.chem.organic.synthesis
Georgia State University <chepjf@panther.gsu.edu>
Atlanta, GA

maison.mousse - 21 Aug 2003 20:41 GMT
Dave Muzuno a écrit dans le message ...
>> Hello,

>> I am interested in drying etahnol. Would adding anhydrous magnesium
>> sulfate do the trick?

>> Also, after I add it, do I just filter it out and end up with 'dry'
>> alcohol? or does it take more than that?

>Magnesium sulfate won't work cause it will partially dissolve in the
alcohol
>AND it also reacts with alcohol.

>The easiest way to dry ethanol:

>1.  Take 1 L of 95% ethanol and add 20 g of magnesium turnings.
>2.  Start heating.  The alcohol starts to react with the magnesium,
[quoted text clipped - 3 lines]
>(1 -2 hours).
>4.  Distill the mixture, discarding the fore and after run.

>Dave

If your alcohol is around 95% distilling through a column filled with corn
meal  will remove most of the water.  NaCl (rock salt )  will remove traces.
CaO can be mixed
with the alcohol and then near absolute alcohol removed by distillation.  Of
interest  is this site.
http://www.journeytoforever.org/biofuel_library/ethanol_manual/manual_ToC.ht
ml

James

Signature

Paul J. Franklin(moderator - sci.chem.organic.synthesis)
http://organicworldwide.net/sci.chem.organic.synthesis
Georgia State University <chepjf@panther.gsu.edu>
Atlanta, GA

Barry Hunt - 23 Aug 2003 17:50 GMT
> Dave Muzuno a écrit dans le message ...
> >> Hello,

> >> I am interested in drying etahnol. Would adding anhydrous magnesium
> >> sulfate do the trick?

> >> Also, after I add it, do I just filter it out and end up with 'dry'
> >> alcohol? or does it take more than that?

> >Magnesium sulfate won't work cause it will partially dissolve in the
> alcohol
> >AND it also reacts with alcohol.

> >The easiest way to dry ethanol:

> >1.  Take 1 L of 95% ethanol and add 20 g of magnesium turnings.
> >2.  Start heating.  The alcohol starts to react with the magnesium,
> >producing hydrogen and magnesium ethoxide.  If it doesn't start, shoot in

> >0.5 mL of chloroform, then keeping heating.
> >3.  Gently reflux the mixture until all the magnesium has been consumed
> >(1 -2 hours).
> >4.  Distill the mixture, discarding the fore and after run.

> >Dave

> If your alcohol is around 95% distilling through a column filled with corn
> meal  will remove most of the water.  NaCl (rock salt )  will remove
traces.
> CaO can be mixed
> with the alcohol and then near absolute alcohol removed by distillation.
Of
> interest  is this site.

http://www.journeytoforever.org/biofuel_library/ethanol_manual/manual_ToC.ht
> ml

> James

I've had a quick look at the web site above (ethanol manual) and there is a
lot of incorrect stuff there (as with most web sites!).
The rock salt thing won't work, (a) you simply can't get enough water out of
the ethanol that way (b) salt is slightly soluble in ethanol (esp wet
ethanol) and I don't think salt in your fuel tank - even traces - is a good
idea. I don't know where the corn meal column is coming from either - it
won't absorb enough water, and you can't distill out the last 5% water so
I'm not sure of the logic behind it.

Barry Hunt

Signature

Paul J. Franklin(moderator - sci.chem.organic.synthesis)
http://organicworldwide.net/sci.chem.organic.synthesis
Georgia State University <chepjf@panther.gsu.edu>
Atlanta, GA

Barry Hunt - 23 Aug 2003 17:51 GMT
> "Dave Muzuno" <nobody@nowhere.com

> > The easiest way to dry ethanol:

> > 1.  Take 1 L of 95% ethanol and add 20 g of magnesium turnings.
> > 2.  Start heating.  The alcohol starts to react with the magnesium,
> > producing hydrogen and magnesium ethoxide.  If it doesn't start, shoot
in a
> > 0.5 mL of chloroform, then keeping heating.
> > 3.  Gently reflux the mixture until all the magnesium has been consumed
> > (1 -2 hours).
> > 4.  Distill the mixture, discarding the fore and after run.

> > Dave

> Organic Synthesis, Collective  Volume 1 pg. 249.

> Suggests (if  the presence of methyl alcohol is permissible):-
>
> "by dissolving 24g of magnesium turning in 200 cc. of absolute methyl
alcohol (the
> reaction is vigorous) and then adding 3 l of the ordinary grade of
absolute
> alcohol (about 99.5 per cent). The mixture is refluxed for about 5 hours
> and distilled into a flask in which the absolute alcohol is to be used."

<snip>
this is cheating, Donald, you're starting with 99.5% ethanol!

Barry Hunt

Signature

Paul J. Franklin(moderator - sci.chem.organic.synthesis)
http://organicworldwide.net/sci.chem.organic.synthesis
Georgia State University <chepjf@panther.gsu.edu>
Atlanta, GA

maison.mousse - 27 Aug 2003 13:55 GMT
Barry Hunt a écrit dans le message ...

>> Dave Muzuno a écrit dans le message ...
>> >> Hello,

>> >> I am interested in drying etahnol. Would adding anhydrous magnesium
>> >> sulfate do the trick?

>> >> Also, after I add it, do I just filter it out and end up with 'dry'
>> >> alcohol? or does it take more than that?

>> >Magnesium sulfate won't work cause it will partially dissolve in the
>> alcohol
>> >AND it also reacts with alcohol.

>> >The easiest way to dry ethanol:

>> >1.  Take 1 L of 95% ethanol and add 20 g of magnesium turnings.
>> >2.  Start heating.  The alcohol starts to react with the magnesium,
>> >producing hydrogen and magnesium ethoxide.  If it doesn't start, shoot
in

>> >0.5 mL of chloroform, then keeping heating.
>> >3.  Gently reflux the mixture until all the magnesium has been consumed
>> >(1 -2 hours).
>> >4.  Distill the mixture, discarding the fore and after run.

>> >Dave

>> If your alcohol is around 95% distilling through a column filled with
corn
>> meal  will remove most of the water.  NaCl (rock salt )  will remove
>traces.
>> CaO can be mixed
>> with the alcohol and then near absolute alcohol removed by distillation.
>Of
>> interest  is this site.

>http://www.journeytoforever.org/biofuel_library/ethanol_manual/manual_ToC.h
t
>> ml

>> James

>I've had a quick look at the web site above (ethanol manual) and there is a
>lot of incorrect stuff there (as with most web sites!).
>The rock salt thing won't work, (a) you simply can't get enough water out
of
>the ethanol that way (b) salt is slightly soluble in ethanol (esp wet
>ethanol) and I don't think salt in your fuel tank - even traces - is a good
>idea. I don't know where the corn meal column is coming from either - it
>won't absorb enough water, and you can't distill out the last 5% water so
>I'm not sure of the logic behind it.

>Barry Hunt

If one starts with 95% EtOH distilling through a dry corn meal
column will remove almost all of the water
NaCl is not soluble in near absolute alcohol and will remove the traces just
fine.
Would you like to point out the errors you found in the link I gave?

James

Signature

Paul J. Franklin(moderator - sci.chem.organic.synthesis)
http://organicworldwide.net/sci.chem.organic.synthesis
Georgia State University <chepjf@panther.gsu.edu>
Atlanta, GA

FirmAbs6pk - 27 Aug 2003 13:56 GMT
wouldnt it be possible to add anhydrous copper sulfate, then filter
then distill.  I dont believe the copper sulfate reacts with ethanol
and if there were any dissolved in the alcohol after this it could be
tested for either visually or with a spectrometer (the blue tint
rather than no tint present from the magnesium sulfate).
Signature

Paul J. Franklin(moderator - sci.chem.organic.synthesis)
http://organicworldwide.net/sci.chem.organic.synthesis
Georgia State University <chepjf@panther.gsu.edu>
Atlanta, GA

Steve Chaffin - 05 Sep 2003 19:53 GMT
I've never had much success drying alcohols (ethanol?) or other polar
solvents with salts, so I don't hold out much hope that you will be
able to do so using CuSO4.

Also, don't rely on a lack of color as an indicator that you have not
contaminated your alcohol with the salt. Remember, the color is due to
the water of hydration. If that water is removed, CuSO4 is colorless.
It is possible to have a minute amt of the salt in the solvent and,
because it is dehydrated, have no color from it.

Steve Chaffin

firmabs6pk@sexmagnet.com (FirmAbs6pk) wrote in message news:<bii9qg$c2d@panther.Gsu.EDU>...
> wouldnt it be possible to add anhydrous copper sulfate, then filter
> then distill.  I dont believe the copper sulfate reacts with ethanol
> and if there were any dissolved in the alcohol after this it could be
> tested for either visually or with a spectrometer (the blue tint
> rather than no tint present from the magnesium sulfate).
Signature

Paul J. Franklin(moderator - sci.chem.organic.synthesis)
http://organicworldwide.net/sci.chem.organic.synthesis
Georgia State University <chepjf@panther.gsu.edu>
Atlanta, GA

Albert Ruggi - 08 Sep 2003 17:45 GMT
A symple method from 95° EtOH is destil with CaO

--
"La sintesi organica è la chimica che fa Dio quando ha voglia di divertirsi
un po'. Se Dio è un chimico" (A.R.)

______________
Albert Ruggi
a.ruggi@inwind.it
www.chimicavita.cjb.net
"Michael Carpenter"

Signature

Paul J. Franklin(moderator - sci.chem.organic.synthesis)
http://organicworldwide.net/sci.chem.organic.synthesis
Georgia State University <chepjf@panther.gsu.edu>
Atlanta, GA

 
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